Metrohm 828IC User Manual

828 IC Dual Suppressor
Instructions for Use
8.828.1003
828 IC Dual Suppressor
Instructions for Use
8.828.1003 09.2002 / pkl
Teachware Metrohm AG Oberdorfstrasse 68 CH-9101 Herisau
teachware@metrohm.com
1st Edition 2002
These instructions are protected by copyright. All rights reserved.
Although all the information given in these instructions has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please inform the author at the address given above.
Contents
Table of contents
1 Introduction.................................................... 1
1.1 Instrument description ............................................................. 1
1.2 How it works.............................................................................. 2
1.3 Parts and controls .................................................................... 4
1.4 Information about the Instructions for Use ............................. 7
1.4.1 Organization ..................................................................................7
1.4.2 Notation and pictograms ..............................................................8
1.5 Safety notes ..............................................................................9
1.5.1 Electrical safety..............................................................................9
1.5.2 General safety measures ..............................................................9
2 Installation ................................................... 10
2.1 Instrument setup..................................................................... 10
2.1.1 Packaging.................................................................................... 10
2.1.2 Checks.........................................................................................10
2.1.3 Location ....................................................................................... 10
2.2 Connecting the accessories................................................... 11
2.2.1 Attaching the CO2 absorber cartridge ........................................11
2.3 Mains connection.................................................................... 12
2.3.1 Mains voltage ..............................................................................12
2.3.2 Fuse.............................................................................................12
2.3.3 Mains cable and mains connection ............................................13
2.3.4 Switching the instrument on/off...................................................13
2.4 Connecting to a modular gradient IC system ....................... 14
2.4.1 Electrical connections .................................................................14
2.4.2 Connecting the IC Dual Suppressor ...........................................15
2.4.3 Settings in IC Net 2.1...................................................................17
2.5 Connecting to the 761 Compact IC........................................ 19
2.5.1 Electrical connection ...................................................................19
2.5.2 Connecting the IC Dual Suppressor ...........................................19
2.5.3 Settings for control by the 761 PC Software 1.1 ......................... 20
3 Operation...................................................... 22
3.1 General information................................................................ 22
3.2 Eluent....................................................................................... 23
3.3 Capacity................................................................................... 23
3.4 Degassing unit and CO2 absorber cartridge ......................... 23
3.5 Flow rate ratio ......................................................................... 24
3.5.1 Setting the flow rates ................................................................... 24
3.6 Routine operation ................................................................... 26
3.6.1 Manual operation ........................................................................26
3.6.2 Software control...........................................................................27
4 Troubleshooting - Problems......................... 30
4.1 Remedying faults and problems ............................................ 30
4.2 Chromatography problems .................................................... 30
4.3 Instrument problems ..............................................................32
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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Contents
5 Care and maintenance ................................33
5.1 Instrument care ....................................................................... 33
5.2 Maintenance by Metrohm Service ......................................... 33
5.3 Shutdown ................................................................................ 33
5.4 Regular maintenance.............................................................. 33
5.4.1 Replacing the CO2 absorber cartridge .......................................34
5.5 Unplanned maintenance work................................................ 34
5.5.1 Regenerating the cation exchanger............................................ 34
5.5.2 Replacing the suppressor cell .................................................... 35
6 Appendix ....................................................... 39
6.1 Technical data......................................................................... 39
6.1.1 Suppressor cell ...........................................................................39
6.1.2 RS 232 interface.......................................................................... 39
6.1.3 Remote interface ......................................................................... 39
6.1.4 Fault switch, ready output........................................................... 40
6.1.5 Mains connection........................................................................ 40
6.1.6 Safety specifications ...................................................................40
6.1.7 Electromagnetic compatibility (EMC) ......................................... 41
6.1.8 Ambient temperature ..................................................................41
6.1.9 Housing ....................................................................................... 41
6.2 Standard equipment ............................................................... 42
6.3 Optional accessories .............................................................. 44
6.4 Validation / GLP ...................................................................... 45
6.5 Warranty and conformity ........................................................ 46
6.5.1 Warranty ......................................................................................46
6.5.2 EU Declaration of Conformity .....................................................47
6.5.3 Certificate of conformity and system validation.......................... 48
6.6 Index ........................................................................................ 49
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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Contents
List of illustrations
Figure 1: Dual suppressor flow diagram............................................. 2
Figure 2: Front panel of the 828 IC Dual Suppressor ......................... 4
Figure 3: Rear panel of the 828 IC Dual Suppressor .......................... 6
Figure 4: Attaching the CO2 absorber cartridge................................ 11
Figure 5: Electrical connections in the MIC 10 system ..................... 14
Figure 6: Flow diagram of the MIC 10............................................... 15
Figure 7: Connecting the 828 IC Dual Suppressor to
the 761 Compact IC ........................................................... 19
Figure 8: Opening the instrument ..................................................... 36
Figure 9: Opened IC Dual Suppressor.............................................. 37
Figure 10: Suppressor cell position, front view ................................... 38
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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Contents
List of numbered
parts and controls
LEDs
1 Ready ..................................................................................................... 4
2 RS 232.................................................................................................... 4
3 Voltage ................................................................................................... 4
4 Current................................................................................................... 4
5 Vacuum .................................................................................................. 4
6 Power ..................................................................................................... 4
7 Connection To Detector ........................................................................ 5
8 Connection From Column..................................................................... 5
9 Flow anode............................................................................................ 5
10 Flow cathode......................................................................................... 5
11 Detector flow setting screw .................................................................. 5
12 Connection for Waste............................................................................. 5
13 RS-232 interface..................................................................................... 6
14 Holder for CO
15 Remote switch ...................................................................................... 6
16 Fuse holder, mains switch, mains connection ................................ 6
17 Vacuum pump inlet .............................................................................. 6
18 Ready Output interface ......................................................................... 6
19 Type and serial number....................................................................... 6
20 Drain....................................................................................................... 6
21 Remote interface.................................................................................... 6
22 Vacuum pump exhaust ........................................................................ 6
23 Front housing screws........................................................................ 36
24 Rear housing screws......................................................................... 36
25 Housing cover .................................................................................... 36
26 Suppressor cell ..............................................................................36,37
Trap Cartridge ............................................................. 6
2
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
IV
1.1 Instrument description
1 Introduction
1.1 Instrument description
The 828 IC Dual Suppressor is a continuous, regeneration-free solid phase suppressor which is used to increase the sensitivity of the detection of anions in ion chromatography.
As well as the usual chemical suppression of the carbonate/bicarbonate background, in a second suppression step the suppressor also removes dissolved CO background conductivity of the mobile phase even further. This results in an improved signal-to-noise ratio; peak areas in the ppm-range and above are increased by approx. 30%. At the same time the areas of the injection peak (water dip) and the system peak are reduced to a minimum. The reduction of the injection peak means that the detection of early-eluting anions is improved; the reduction of the system peak allows the detection of anions which coelute with the system peak. The baseline drift is also minimized when carbonate/bicarbonate gradients are used.
in order to reduce the
2
In Metrohm IC systems the 828 IC Dual Suppressor can be remotely controlled via a remote interface. It can also be combined with all other commercially available HPLC systems.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1 Introduction
X
X
1.2 How it works
The 828 IC Dual Suppressor is used to increase the sensitivity of the
detection of anions in conductivity measurements. It is installed between the separation column and the conductivity detector. The IC Dual Suppressor consists of a suppressor cell, a direct current source and a degassing unit. After it enters the suppressor cell the eluent containing the sample ions is split proportionally toward the detector, anode and cathode as shown in Figure 1.
NaHCO
/Na2CO3 + MX
3
+ O2+ H
2 H
2CO3
Anode
+
+
H+
Na+ form Resin
IN
Cathode
NaOH + MOH + H2+ NaX
2 H2O  4 H++ O2+ 4 e
H+
H+
H+
OUT
2 H2O + 2 e
-
H2CO3+ HX
+2 OH
H
2
-
Degassing Unit
 CO2 + H2O
H
2CO3
-
M = Cations (Na+, K+, Mg2+, etc.)
= Anions
H
O + HX
2
To Detector
Figure 1: Dual suppressor flow diagram
Three processes take place simultaneously in the 828 IC Dual Suppressor:
1. As the eluent and the sample ions emerge from the separation
column an acid/base reaction converts them to their protonated forms. The cell is packed with a strong cation exchanger which is present in protonated form. The following exchange reactions occur in the suppressor:
Eluent:
NaOH + Resin-SO
-H+
Resin-SO
3
-Na+
3
+ H2O
or
NaHCO
/Na2CO3 + Resin-SO
3
-H+
Resin-SO
3
-Na+
3
+ H2CO3
Sample:
MX + Resin-SO
-H+
Resin-SO
3
-M+
3
+ HX
-
-
, NO
X = Cl
, Br-, etc.
3
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1.2 How it works
The counter ions (Na+) of the eluent are exchanged for the hydrogen
+
ions (H water will be formed; if NaHCO
) of the resin in the cell. If NaOH is used as the eluent then
/Na2CO3 is used as the eluent then
3
carbon dioxide is produced. At the same time the counter ions of the sample (M
+
= metal cation) are exchanged for protons from the resin. Together with the sample anions these form acids which have an increased conductivity, e.g. hydrochloric acid, nitric acid, etc. This provides an improved signal-to-noise ratio and an improved detection sensitivity.
2. During the operation of the 828 IC Dual Suppressor a direct current
is constantly applied to the suppressor cell electrodes.
Water in the cell is electrolyzed and the following electrode reactions take place:
Anode: 2 H
O 4 H+ + O2(g) + 4 e-
2
Cathode: 2 H
O + 2 e- 2 OH- + H2(g)
2
At the anode hydrogen ions and gaseous oxygen are produced; at the cathode hydroxide ions and gaseous hydrogen. In this way the hydrogen ions produced at the anode continuously regenerate the cation exchanger. The sodium cations of the eluent and the cations of the sample wander toward the cathode in the direct current field. The eluate that leaves the suppressor cell on the cathode side contains the hydroxide salts of these cations, gaseous hydrogen and some sample anions (in the form of their sodium salts). The eluate at the anode side contains carbonic acid or water together with gaseous oxygen and some sample ions (protonated form). The protonated sample anions are eluted toward the detector with carbonic acid or water.
3. After leaving the suppressor cell all eluates pass through a
degassing unit. Oxygen and hydrogen are removed from the eluate flows at the anode and cathode sides respectively before they reach the waste container. The eluate at the OUT connection (see Figure 1, Figure 10) contains the sample anions and carbonic acid (if a carbonate/bicarbonate eluent is used) and passes the degassing unit before reaching the conductivity detector. In the degassing unit the carbonic acid dissociates to form carbon dioxide and water. Carbon dioxide is removed and water remains.
This further reduces the background conductivity of the eluate to provide improved sensitivity and a more stable baseline. This means that it is possible to use carbonate/bicarbonate gradients. The injection peak (water dip), which is often overlapped by quickly eluting anions, and the system peak, which interferes with the detection of anions which coelute with it, are eliminated.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1 Introduction
1.3 Parts and controls
12 34 56
78 9 10 11 12
LEDs The color of the LED indicates the instrument status.
Ready
1
Green: the suppressor is ready for an analysis.
Red: an error has occurred.
RS-232
2
Green: data transfer via RS 232 connection 13, only for service purposes.
Figure 2: Front panel of the 828 IC Dual Suppressor
4
5
Current Green: current is flowing across the
suppressor cell.
Vacuum Green: the vacuum has operating
pressure. Red: insufficient vacuum. A leak is present or the set value has not been reached within 30 minutes of the instrument being switched on.
Voltage
3
Green: the voltage applied to the suppressor cell is within the limits for normal operation. Red: the voltage is outside the operating limits.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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6
Power Green: the Dual Suppressor is
switched on, mains voltage is applied.
1.3 Parts and controls
To Detector
7
Inlet connection to detector, connection for 6.1831.010 PEEK Capillary with 6.2744.010 PEEK Pressure screw
From Column
8
Outlet connection from column, connection for 6.1831.010 PEEK Capillary with 6.2744.010 PEEK Pressure screw
9 Flow Anode
For a visual check of the anode eluate. The liquid from the anode passes through the FEP tubing before entering the degassing unit. In normal operation oxygen bubbles should be seen regularly.
10
Flow Cathode For a visual check of the cathode eluate. The liquid from the cathode passes through the FEP tubing before entering the degassing unit. In normal operation hydrogen bubbles should be seen regularly.
11
Detector Flow
The flow to the detector can be regulated with a screwdriver.
12 Waste
Outlet to waste container, connection for 6.1803.020 PTFE Tubing with
6.2744.010 PEEK Pressure screw
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1 Introduction
13 14 15 16
17
18 19 20 21 22
Figure 3: Rear panel of the 828 IC Dual Suppressor
RS 232
13
Interface for service purposes
18
Ready Output
6-pin connector, used as fault switch, carries status signals (ready/not ready) to external instruments.
CO
14
Trap Cartridge
2
Holder for CO
absorber-cartridge for
2
19 Type and serial number
cleaning the incoming air
Remote switch
15
Activates the remote control of the
20
Drain Drain port outlet for liquids
Dual Suppressor via the Remote connector:
I = ON 0 = OFF
Fuse holder
16
For slow blow fuse 1.0 AT, U.600.0016
Mains switch
21
Remote Remote interface for remote control by external instruments.
For switching instrument on/off:
I = ON 0 = OFF Mains connector
For mains connection see Section 2.3
Vacuum pump inlet
17
Connected to 6.2837.000,
22
Vacuum pump exhaust
see Section 2.2.1
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1.4 Information about the Instructions for Use
1.4 Information about the Instructions for Use
Please study these Instructions for Use carefully before you start to use the 828 IC Dual Suppressor. The instructions contain information and warnings that must be observed by the user in order to guarantee the safe use of the instrument. Please keep these instructions near the instrument so that they are always to hand when required.
1.4.1 Organization
These 8.828.1003 Instructions for Use for the 828 IC Dual Suppressor provide you with a comprehensive overview of the installation, startup, troubleshooting and technical specifications of the instrument. The installation instructions are arranged as follows:
Sect. 1 Introduction
General description of the instrument, operating parts and controls, and safety notes
Sect. 2 Installation
Installation of the instrument, mains connection, connection of the accessories, connection to IC system
Sect. 3 Operation
Information about the operation of the 828 IC Dual Suppressor
Sect. 4 Troubleshooting - Problems
Possible faults and their remedies
Sect. 5 Care and maintenance
Care and maintenance of the instrument
Sect. 6 Appendix
Technical data, standard equipment, optional accessories, warranty and declaration of conformity, index
In order to find the information you require about the 828 Dual Suppressor you should either use the Contents or the Index.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1 Introduction
1.4.2 Notation and pictograms
The following notation and pictograms (symbols) are used in these Instructions:
15 828 parts and controls
Danger/Warning
This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components by electricity.
Danger/Warning This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components.
Attention This symbol indicates important information that you should read before continuing.
Information This symbol indicates additional information and tips which may be of particular use to you.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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1.5 Safety notes
1.5 Safety notes
Warning! This instrument should only be used in accordance with the information given in these Instructions for Use.
1.5.1 Electrical safety
Electrical safety when handling the 828 IC Dual Suppressor is guaranteed within the scope of Standard IEC 61010. However, please observe the following points:
Mains connection
The mains connection and checking the mains fuse must be carried out according to the information given in Section 2.3.
Opening the 828 IC Dual Suppressor
If the 828 IC Dual Suppressor is connected to the mains supply then it must neither be opened nor should any parts be removed from it, as otherwise the risk of contact with current-carrying assemblies exists. This is why the instrument should be separated from all voltage sources before being opened. Please make sure that the mains cable is pulled out from mains connector 16!
Protection against electrostatic charges
Electronic components are sensitive to electrostatic charges and can be destroyed by a discharge. Before touching any assembly within the 828 IC Dual Suppressor you should ground yourself and any tool you are using by grasping a grounded object (e.g. the instrument housing or a radiator) in order to eliminate any electrostatic charge which may be present.
1.5.2 General safety measures
Liquid handling
Check all inlet and outlet tubing for leaks at regular intervals. Observe the appropriate regulations concerning the handling of flammable and/or toxic solutions and their disposal.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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2 Installation
2 Installation
2.1 Instrument setup
2.1.1 Packaging
The 828 IC Dual Suppressor and its specially packed accessories are supplied in very protective special packaging which contains a shock­absorbing plastic foam lining. The instrument itself is contained in an dustproof evacuated polyethylene bag. Please store this packaging in a safe place; it is the only way in which the safe transport of the instrument can be guaranteed.
2.1.2 Checks
Please check that the delivery is complete and undamaged immediately on receipt (compare with delivery note and list of accessories given in Section 6.2). If transport damage is evident please refer to the information given in Section 6.4 “Warranty”.
2.1.3 Location
Place the instrument on a suitable vibration-free laboratory bench, protected as much as possible from corrosive atmospheres and contact with chemicals.
Choose a location where the temperature is usually between +5 °C and +45 °C. The instrument should be protected against excessive variations in temperature and direct sunlight.
828 IC Dual Suppressor/ 8.828.1003 Instructions for Use
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