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Man IC ICS5000 Operators Dec2011 DOC065342 06

ICS 5000 Ionic Chromatography Operating Manual

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Stephane Gouin
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0% found this document useful (0 votes)
15 views

Man IC ICS5000 Operators Dec2011 DOC065342 06

ICS 5000 Ionic Chromatography Operating Manual

Uploaded by

Stephane Gouin
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Dionex ICS-5000 Ion Chromatography

System Operator's Manual

Document No. 065342


Revision 06
December 2011
© 2011 Thermo Fisher Scientific. All rights reserved.
AES, Atlas, Chromeleon, IonPac, OnGuard, and SRS are registered
trademarks of Thermo Fisher Scientific, Inc. in the United States.
Adobe, Acrobat, and Adobe Reader are registered trademarks of Adobe
Systems, Incorporated in the United States and other countries. Windows is a
registered trademark of Microsoft Corporation in the United states and other
countries.
The following are registered trademarks in the United States and possibly
other countries: Kel-F is a registered trademark of 3M Company, Inc.
KIMWIPES is a registered trademark of Kimberly-Clark Corporation.
PharMed and Tygon are registered trademarks of Saint-Gobain Performance
Plastics. Ultrajet is a registered trademark of ITW Chemtronics.
PEEK is a trademark of Victrex PLC. TitanHP is a trademark of Rheodyne
L.L.C.
All other trademarks are the property of Thermo Fisher Scientific and its
subsidiaries.
Thermo Fisher Scientific Inc. provides this document to its customers with a
product purchase to use in the product operation. This document is copyright
protected and any reproduction of the whole or any part of this document is
strictly prohibited, except with the written authorization of Thermo Fisher
Scientific Inc.
The contents of this document are subject to change without notice. All
technical information in this document is for reference purposes only. System
configurations and specifications in this document supersede all previous
information received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this
document is complete, accurate or error-free and assumes no
responsibility and will not be liable for any errors, omissions, damage or
loss that might result from any use of this document, even if the
information in the document is followed properly.
Revision history: Revision 01 released May 2010
Revision 02 released June 2010 Revision 03 released February 2011
Revision 04 released June 2011 Revision 05 released September 2011
Revision 06 released December 2011

For research use only. Not for use in diagnostic procedures.


Contents

1 • Introduction
1.1 Thermo Scientific Dionex ICS-5000 System Overview . . . . . . . . . . . 1
1.1.1 Dionex ICS-5000 System Components . . . . . . . . . . . . . . . . . 2
1.1.2 Dionex ICS-5000 System Control . . . . . . . . . . . . . . . . . . . . 11
1.2 Dionex ICS-5000 System Documentation . . . . . . . . . . . . . . . . . . . . . 14
1.3 The Dionex ICS-5000 System Operator’s Manual . . . . . . . . . . . . . . 15
1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . 16
1.4.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . 16
1.4.2 Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
1.4.3 Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . 19
1.5 Deionized Water Requirements for IC . . . . . . . . . . . . . . . . . . . . . . . . 20

2 • Description
DP/SP Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.1 DP/SP Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.2 DP/SP Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
2.2.1 Pump Heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
2.2.2 Pressure Transducer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.2.3 Proportioning Valves (Gradient pump only) . . . . . . . . . . . . 25
2.2.4 Vacuum Degassing Module . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.2.5 Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

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2.2.6 Static Mixer (Analytical IC only) . . . . . . . . . . . . . . . . . . . . . 27


2.2.7 Pulse Damper (Capillary IC only) . . . . . . . . . . . . . . . . . . . . 27
2.3 DP/SP Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
2.3.1 Isocratic Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . 28
2.3.2 Gradient Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . 29
2.4 DP/SP Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
2.5 Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
2.5.1 EO (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
2.5.2 Pressurizing Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . 34
2.5.3 Filtering Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

EG Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
2.6 EG Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
2.7 EG Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
2.8 EG Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
2.9 EG Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

DC Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
2.10 DC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
2.11 DC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
2.11.1 DC Interior Components for Capillary IC . . . . . . . . . . . . . . 54
2.11.2 IC Cube for Capillary IC . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
2.11.3 DC Interior Components for Analytical IC . . . . . . . . . . . . . 61
2.12 DC Temperature Control Zones . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
2.13 High-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
2.13.1 4-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66

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Contents

2.13.2 6-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67


2.13.3 10-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
2.14 CD Conductivity Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
2.14.1 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
2.14.2 Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
2.14.3 System Flow Schematics for Conductivity Detection . . . . . 72
2.15 ED Electrochemical Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
2.15.1 Electrochemical Detector Cell . . . . . . . . . . . . . . . . . . . . . . . 75
2.15.2 Combination pH–Ag/AgCl Reference Electrode . . . . . . . . . 77
2.15.3 Palladium Hydrogen (PdH) Reference Electrode . . . . . . . . . 79
2.16 DC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
2.17 I/O Option . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
2.17.1 I/O Option Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
2.17.2 Analog Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
2.17.3 Power, Relay, and TTL Outputs . . . . . . . . . . . . . . . . . . . . . . 87
2.17.4 TTL Inputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
2.18 Automation Manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
2.18.1 AM High-Pressure Switching Valves . . . . . . . . . . . . . . . . . . 96
2.18.2 AM Low-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
2.18.3 AM High- and Low-Pressure Valve Control . . . . . . . . . . . . 98
2.18.4 RCH-1 Reaction Coil Heater . . . . . . . . . . . . . . . . . . . . . . . 101
2.19 Electrochemical Detection Modes . . . . . . . . . . . . . . . . . . . . . . . . . . 102
2.19.1 DC Amperometric Detection . . . . . . . . . . . . . . . . . . . . . . . 102
2.19.2 Integrated and Pulsed Amperometric Detection . . . . . . . . 103
2.19.3 Cyclic Voltammetry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105

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Dionex ICS-5000 Operator’s Manual

2.19.4 Waveforms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105


2.19.5 Storing and Reprocessing Amperometry Data . . . . . . . . . . 109

TC Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
2.20 TC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
2.21 TC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
2.22 TC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
2.23 Injection Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
2.23.1 Injection Valve Operation . . . . . . . . . . . . . . . . . . . . . . . . . . 122
2.23.2 Injection Valve Plumbing . . . . . . . . . . . . . . . . . . . . . . . . . . 124
2.24 Column Identification (ID) System . . . . . . . . . . . . . . . . . . . . . . . . . 125
2.25 Gas and Humidity Sensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
2.26 TC Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127
2.26.1 Predictive Performance . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

3 • Configurations
3.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129

4 • Startup
4.1 Operating Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141
4.1.1 EG Operating Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . 141
4.1.2 ED Cell Operating Precautions . . . . . . . . . . . . . . . . . . . . . . 143
4.2 System Startup Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146
4.3 Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147
4.3.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . 147

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4.3.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147


4.3.3 Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148
4.3.4 Filling the Autosampler Vials and Loading the Sample
Tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
4.4 Starting Chromeleon 7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
4.4.1 Starting the Chromeleon 7 Instrument Controller Service . 149
4.4.2 Starting the Chromeleon 7 Client . . . . . . . . . . . . . . . . . . . . 149
4.5 Starting Chromeleon 6.8 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
4.5.1 Starting the Chromeleon 6.8 Server . . . . . . . . . . . . . . . . . . 150
4.5.2 Starting the Chromeleon 6.8 Client . . . . . . . . . . . . . . . . . . 151

DP/SP Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153


4.6 Setting Up the Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
4.7 Setting Up the Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . 154
4.8 Starting the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157

EG Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161
4.9 Entering the Eluent Concentration . . . . . . . . . . . . . . . . . . . . . . . . . . 161
4.10 Selecting an Eluent Concentration . . . . . . . . . . . . . . . . . . . . . . . . . . 162

DC Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
4.11 Starting the DC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
4.12 Equilibrating the System and Verifying Operational Readiness . . . 166

TC Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.13 Starting the TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.14 Equilibrating the System and Verifying Operational Readiness . . . 170

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Dionex ICS-5000 Operator’s Manual

5 • Operation
5.1 Controlling Modules Directly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
5.2 Analyzing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
5.2.1 Creating a New Sequence in Chromeleon 7 . . . . . . . . . . . . 173
5.2.2 Creating a New Sequence in Chromeleon 6.8 . . . . . . . . . . 174
5.2.3 Starting a Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 176
5.3 Loading Samples Into the Sample Loop or Concentrator . . . . . . . . 178
5.3.1 Loading Samples with an Autosampler . . . . . . . . . . . . . . . 178
5.3.2 Loading Samples with a Syringe . . . . . . . . . . . . . . . . . . . . 178
5.3.3 Loading Samples with a Vacuum Syringe (Pull Method) . 179
5.4 Autosampler Commands for Loading and Injecting Samples . . . . . 180

6 • Shutdown
DP/SP Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183

EG Shutdown. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
6.1 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185
6.2 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185

DC Shutdown. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
6.3 Consumables Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
6.4 ED Cell Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
6.4.1 Short-term Storage of the ED Cell . . . . . . . . . . . . . . . . . . . 187
6.4.2 Long-term Storage of the pH-Ag/AgCl Reference
Electrode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187

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TC Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.5 Consumables Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.6 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.7 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189

7 • Maintenance
7.1 System Maintenance Checklists . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.2 Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.3 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
7.1.4 Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192

DP/SP Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195


7.2 DP/SP Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
7.3 DP/SP Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
7.4 DP/SP Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 196
7.5 DP/SP Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 196

EG Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197


7.6 EG Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197
7.7 EG Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197
7.8 EG Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 197

DC Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199


7.9 DC Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199
7.10 DC Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199

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Dionex ICS-5000 Operator’s Manual

7.11 DC Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 199


7.12 DC Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 200

TC Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201


7.13 TC Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201
7.14 TC Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201
7.15 TC Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 201
7.16 TC Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 202

8 • Troubleshooting
8.1 Audit Trail Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 203
8.1.1 DP/SP Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . 204
8.1.2 EG Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 205
8.1.3 DC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 207
8.1.4 TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 209
8.2 Noisy Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 214
8.3 Poor Retention Time Reproducibility . . . . . . . . . . . . . . . . . . . . . . . 218
8.4 Peak Retention Times Are Too Early . . . . . . . . . . . . . . . . . . . . . . . 220
8.5 Peak Retention Times Are Too Late . . . . . . . . . . . . . . . . . . . . . . . . 220
8.6 No Peaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 220
8.7 Tailing Peaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 222
8.8 Low System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 223
8.9 High System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 223
8.10 Low Detector Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 224
8.11 High Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 225

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Contents

DP/SP Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 227


8.12 Troubleshooting DP/SP Error Messages . . . . . . . . . . . . . . . . . . . . . 227
8.13 DP/SP Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 235
8.14 DP/SP Stops . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 236
8.15 DP/SP Liquid Leaks/Leak Alarm . . . . . . . . . . . . . . . . . . . . . . . . . . 237
8.16 Vacuum Degassing Module Low Vacuum . . . . . . . . . . . . . . . . . . . 238
8.17 Vacuum Degassing Module Does Not Run . . . . . . . . . . . . . . . . . . . 238
8.18 DP/SP Digital I/O Port Inoperative . . . . . . . . . . . . . . . . . . . . . . . . . 239

EG Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 241
8.19 Troubleshooting EG Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 241
8.20 EG ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 253
8.21 EG POWER LED Fails to Light . . . . . . . . . . . . . . . . . . . . . . . . . . . 254
8.22 Liquid Leaks in the EG . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254
8.23 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255
8.24 EG Stops Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

DC Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259
8.25 Troubleshooting DC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 259
8.26 Liquid Leaks from DC Components . . . . . . . . . . . . . . . . . . . . . . . . 270
8.27 VALVE Button Not Working . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 271
8.28 ED Cell Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 271
8.28.1 ED Cell pH Readout Always 7.0 . . . . . . . . . . . . . . . . . . . . 271
8.28.2 Cannot Set ED Cell pH Readout to 7.0 . . . . . . . . . . . . . . . . 272
8.28.3 Shift in ED Cell pH Readout . . . . . . . . . . . . . . . . . . . . . . . 272
8.28.4 No ED Cell pH Readout or Intermittent Readout . . . . . . . . 273

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8.28.5 Leak in pH-Ag/AgCl Reference Electrode Compartment . 274


8.28.6 Shift in Ag/AgCl Reference Potential . . . . . . . . . . . . . . . . . 274

TC Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275
8.29 Troubleshooting TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 275
8.30 TC ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 299
8.31 Liquid Leaks from TC Components . . . . . . . . . . . . . . . . . . . . . . . . 300
8.32 TC Temperature Does Not Increase . . . . . . . . . . . . . . . . . . . . . . . . . 301
8.33 TC Temperature Stabilizer Not Operating Properly . . . . . . . . . . . . 301

9 • Service
9.1 Connecting Capillary Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
9.2 Tightening Guidelines for High-Pressure Fittings . . . . . . . . . . . . . . 305

DP/SP Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 306


9.3 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 306
9.4 Cleaning Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 308
9.5 Priming the DP/SP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 308
9.5.1 Priming with the PUMP PRIME Button . . . . . . . . . . . . . . . 309
9.5.2 Priming from the Chromeleon Panel . . . . . . . . . . . . . . . . . 310
9.6 Replacing the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 312
9.6.1 Removing the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . 313
9.6.2 Installing the New Check Valves . . . . . . . . . . . . . . . . . . . . 314
9.7 Replacing Piston Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316
9.7.1 Removing the Pump Head and Piston . . . . . . . . . . . . . . . . 317
9.7.2 Cleaning the Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 320

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9.7.3 Removing the Main Piston Seal . . . . . . . . . . . . . . . . . . . . . 320


9.7.4 Removing the Piston Seal Wash Seal . . . . . . . . . . . . . . . . . 321
9.7.5 Installing the Piston Seals and O-Ring . . . . . . . . . . . . . . . . 321
9.7.6 Reinstalling the Piston and Pump Head . . . . . . . . . . . . . . . 323
9.8 Replacing the Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
9.8.1 Removing the Pump Head and Piston . . . . . . . . . . . . . . . . 324
9.8.2 Reinstalling the New Piston . . . . . . . . . . . . . . . . . . . . . . . . 325
9.8.3 Reinstalling the Pump Head . . . . . . . . . . . . . . . . . . . . . . . . 325
9.9 Replacing the Piston Seal Wash Tubing . . . . . . . . . . . . . . . . . . . . . 326
9.10 Replacing the DP/SP Priming Valve Knob Seal . . . . . . . . . . . . . . . 329
9.11 Changing the DP/SP Main Power Fuses . . . . . . . . . . . . . . . . . . . . . 330

EG Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 333
9.12 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 333
9.12.1 Tubing and Fittings for Capillary IC EG Channels . . . . . . 333
9.12.2 Tubing and Fittings for Analytical IC EG Channels . . . . . 335
9.13 Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . 336
9.14 Replacing the EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 336
9.14.1 Removing the Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . 337
9.14.2 Disposing of the Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . 339
9.14.3 Storing an Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339
9.14.4 Installing and Conditioning a New Capillary EGC . . . . . . 340
9.14.5 Installing and Conditioning a New Analytical EGC . . . . . . 345
9.15 Replacing the CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 349
9.15.1 Removing the Old CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . 350

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9.15.2 Installing and Flushing the New CR-TC . . . . . . . . . . . . . . 350


9.15.3 Completing the New CR-TC Plumbing . . . . . . . . . . . . . . . 353
9.16 Replacing the RFIC Eluent Degasser . . . . . . . . . . . . . . . . . . . . . . . . 355
9.17 Installing a Backpressure Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 355
9.18 Changing the EG Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . 357

DC Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 359
9.19 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 359
9.19.1 Tubing and Fittings for Capillary IC Systems . . . . . . . . . . 359
9.19.2 Tubing and Fittings for Analytical IC Systems . . . . . . . . . 362
9.20 Connecting a Sample Loading Port to the Injection Valve . . . . . . . 363
9.21 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 364
9.22 Rebuilding a High-Pressure (Injection) Valve . . . . . . . . . . . . . . . . . 366
9.23 Replacing a High-Pressure (Injection) Valve Pod . . . . . . . . . . . . . . 367
9.24 Installing or Replacing an I/O Option Board . . . . . . . . . . . . . . . . . . 369
9.25 Changing the DC Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . 371
9.26 IC Cube Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 372
9.26.1 Replacing an IC Cube Cartridge . . . . . . . . . . . . . . . . . . . . . 372
9.26.2 Replacing Capillary Columns . . . . . . . . . . . . . . . . . . . . . . . 374
9.27 CD Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 379
9.27.1 Calibrating the CD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . 379
9.27.2 Replacing an Analytical Suppressor . . . . . . . . . . . . . . . . . . 381
9.27.3 Replacing a CD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 382
9.27.4 Removing Trapped Air from the Conductivity Cell . . . . . . 383
9.28 ED Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 385

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Contents

9.28.1 Disconnecting the ED Cell . . . . . . . . . . . . . . . . . . . . . . . . . 385


9.28.2 Replacing an ED Cell Disposable Working Electrode
Gasket . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 386
9.28.3 Replacing an ED Cell Conventional Working Electrode
Gasket . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 386
9.28.4 Polishing an ED Cell Conventional Working Electrode . . . 389
9.28.5 Replacing a pH-Ag/AgCl Reference Electrode . . . . . . . . . 392
9.28.6 Calibrating the pH-Ag/AgCl Reference Electrode . . . . . . . 394
9.28.7 Replacing the pH-Ag/AgCl Reference Electrode O-Ring . 399
9.28.8 Replacing a PdH Reference Electrode . . . . . . . . . . . . . . . . 400
9.28.9 Replacing an ED Detector . . . . . . . . . . . . . . . . . . . . . . . . . 404

TC Service. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 407
9.29 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 407
9.30 Setting Up the Column ID System . . . . . . . . . . . . . . . . . . . . . . . . . . 408
9.31 Rebuilding an Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 410
9.32 Replacing an Injection Valve Pod . . . . . . . . . . . . . . . . . . . . . . . . . . 411
9.33 Changing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . 413

A • Specifications
DP/SP Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415

EG Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 419

DC Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 423

TC Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 433

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B • Reordering Information
DP/SP Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . 435

EG Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 439

DC Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 441

TC Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445

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1 • Introduction

1.1 Thermo Scientific Dionex ICS-5000 System


Overview

1 Dionex ICS-5000 Dual Pump (DP)


1
Dionex ICS-5000 Eluent Generator
2 (EG)

3 Dionex ICS-5000
Detector/Chromatography Module

3 2

Figure 1-1. Dual Dionex ICS-5000 System with RFIC-EG™

The Thermo Scientific Dionex ICS-5000 Ion Chromatography System offers


a full range of Reagent-Free™ IC (RFIC™) components. RFIC-EG combines
automated eluent generation and self-regenerating suppression to make IC
easier and more powerful than ever before. It is no longer necessary to spend
time preparing eluents and regenerants. All you need is deionized water—the
IC system automatically generates eluent in the exact amount and
concentration needed for your application, ensuring superior analytical

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Dionex ICS-5000 Operator’s Manual

results. In combination with capillary columns at flow rates of 0.010 mL/min,


the Dionex ICS-5000 system can be used for long periods of continuous
operation and minimal eluent consumption.
The dual-analysis capabilities (both simultaneous and sequential) of the
Dionex ICS-5000 system let you maximize efficiency and throughput and
minimize downtime. The modular system design lets you quickly configure
and customize hardware.
The single-channel Dionex ICS-5000 can be configured to run either capillary
IC applications or microbore or standard bore IC applications.
• Capillary IC applications use 0.4 mm diameter columns with flow rates
typically from 0.005 to 0.02 mL/min.
• Microbore IC applications use 2 mm diameter columns and with flow
rates typically from 0.2 to 0.5 mL/min.
• Standard bore IC applications use 4 mm diameter columns with flow rates
typically from 1.0 to 2.0 mL/min.
A dual Dionex ICS-5000 system can be configured with any combination of
the above application types (for example, one capillary IC channel and one
microbore IC channel, or two capillary IC channels, or one microbore IC
channel and one standard bore IC channel).

1.1.1 Dionex ICS-5000 System Components


The table below identifies modules in the Dionex ICS-5000 product line, as
well as additional products that can be added to a Dionex ICS-5000 system.
Refer to the page number indicated here for a brief product overview.

Product Type Product Name Page


Pump Dionex ICS-5000 Dual Pump page 3
Dionex ICS-5000 Single Pump page 3
Eluent Generator Dionex ICS-5000 Eluent Generator page 5
Eluent Organizer Dionex ICS-5000 Eluent Organizer page 6
Detector/Chromatography Dionex ICS-5000 page 7
Compartment Detector/Chromatography Module
IC Cube™ (inside DC) Dionex IC Cube page 7

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1 • Introduction

Product Type Product Name Page


Detector (inside DC) Dionex ICS-5000 Conductivity page 7
Detector
Dionex ICS-5000 Electrochemical page 7
Detector
Accessory (inside DC) Dionex ICS-5000 Automation page 8
Manager
Detector (outside DC) ICS Series Photodiode Array page 9
Detector
ICS Series Variable Wavelength page 10
Detector
Thermal Compartment Dionex ICS-5000 Thermal page 8
Compartment
Autosampler Dionex AS Autosampler page 9
Dionex AS-DV Autosampler page 9
Mass Spectrometer MSQ Plus™ page 10

Dionex ICS-5000 Dual Pump (DP) and Dionex ICS-5000 Single Pump (SP)

Each Dionex ICS-5000 pump can be configured for either capillary IC


applications or analytical (standard bore and microbore) IC applications.
Capillary IC pumps are always isocratic (they deliver one eluent). Analytical
IC pumps can be either isocratic or low pressure proportioned gradient.
Gradient pumps deliver gradient mixtures of up to four eluent components.
The eluent composition selected for a gradient pump can be delivered as
isocratic, isocratic proportioned, linear ramp, step, curved, or any
combination of these.
The SP contains one of the following pump types:
• Isocratic capillary IC pump
• Isocratic analytical IC pump
• Gradient analytical IC pump
The DP contains two pumps in any combination of the three types listed
above (for example, two isocratic capillary IC pumps, or two isocratic
analytical IC pumps, or one isocratic capillary IC pump and one gradient
analytical IC pump).

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Dionex ICS-5000 Operator’s Manual

The second pump in the DP can be operated as a second-channel


chromatography pump, an auxiliary dependent pump, or an auxiliary
independent pump.
Capillary Capillary IC pumps operate at flow rates ranging from 0.001 to 3.0 mL/min
IC and operating pressures up to 41 MPa (6000 psi) (without RFIC) and up to
35 MPa (5000 psi) (with RFIC).

IMPORTANT

Capillary IC pumps shipped before February 17, 2011 were rated for lower
operating pressures than the pumps currently being shipped. The older
pumps can be operated at pressures up to 35 MPa (5000 psi) (without
RFIC) and up to 21 MPa (3000 psi) (with RFIC). Before operating at
pressures above these limits, verify that you have the appropriate pump.
• HPC is stamped on the secondary
pump heads of the older (lower
pressure rated) capillary IC pumps.

• HPC-2 is stamped on the secondary


pump heads of the newer (higher
pressure rated) capillary IC pumps.

A Capillary Pump High-Pressure Upgrade Kit (P/N 075994) is available


for converting a lower pressure rated capillary IC pump to a higher
pressure rated pump. The kit includes the HPC-2 secondary pump head and
high-pressure pump seals.

NOTE A high-pressure EG degas (capillary) cartridge (P/N 074459) is


also required when operating a capillary RFIC system at pressures
up to 35 MPa (5000 psi). For details, see page 5.

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1 • Introduction

Analytical IC pumps operate at flow rates ranging from 0.00 to 10.0 mL/min
and operating pressures up to 35 MPa (5000 psi) without RFIC and up to
21 MPa (3000 psi) with RFIC. Both microbore and standard bore IC
applications are supported.

Dionex ICS-5000 Eluent Generator (EG)

The EG generates high purity acid or base eluents online from deionized
water. The EG can be configured for single- or dual-channel operation. Each
channel includes:
• A high precision programmable current source (power supply)
For each channel, the following options must be ordered separately for
installation inside the EG.
• A disposable eluent generator cartridge (EGC). Each cartridge contains an
electrolyte concentrate solution, appropriate for the eluent being
generated.
• A Continuously Regenerated Trap Column (CR-TC) to remove any
extraneous contaminants from the deionized water source. The CR-TC is
electrolytically-regenerated, which allows it to operate for extended
periods without chemical regeneration.
• A high-pressure gas removal device that removes electrolysis gases
created during eluent generation
Two versions of EGC and CR-TC are available: one for capillary IC systems
and one for analytical IC systems.

Capillary IMPORTANT
IC
If your system includes a capillary pump linked to an
EGC, check the label on the EG degas (capillary)
cartridge in the IC Cube and verify that 5000 psi is
printed on the label (see the figure on the right).
If 5000 psi is not on the label, you must change the high 5000 psi
pressure limit to 21 MPa (3000 psi) (see page 158) or
replace the cartridge with an EG degas (capillary)
cartridge that is rated for 35 MPa (5000 psi)
P/N 074459
(P/N 074459).

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Dionex ICS-5000 Operator’s Manual

Reagent-Free IC with Eluent Regeneration (RFIC-ER™)

RFIC-ER is available as an option for Dionex ICS-5000 systems without an


EG. Eluent regeneration uses the suppressor to reconstitute the starting eluent,
allowing use of a single 4-liter bottle of eluent for up to four weeks. Because
the system is a closed loop, it can run continuously, eliminating the need for
recalibration or re-equilibration during the 28 days of non-stop operation.
RFIC-ER uses carbonate, carbonate/bicarbonate, or MSA eluents for isocratic
separations on standard bore columns.

Dionex ICS-5000 Eluent Organizer (EO)

The EO holds eluent reservoirs in a liner that contains spills and leaks. Up to
two EOs can be installed on top of the DC. Each EO accommodates up to four
1-liter or 2-liter reservoirs or up to two 4-liter reservoirs. The EO is typically
ordered configured with four 2-liter reservoirs (P/N 072058).
All eluent reservoirs available for use with the DP/SP can be pressurized. If
you plan to pressurize the eluent reservoirs, the optional EO Regulator
Accessory and Stand (P/N 074423) is required.
The Regulator Accessory includes a pressure regulator and gauge assembly
with four outputs (for connections to four eluent reservoirs), as well as the
tubing and connection fitting required. If more reservoirs are required, order a
second regulator (P/N 074422).

Reagent-Free IC with Electrolytic Sample Preparation (RFIC-ESP™)

RFIC-ESP systems enable a range of automated sample preparation


techniques which use proprietary electrolytic devices to provide reduced cost
and higher value analyses.
RFIC-ESP devices and techniques can be used for removing cations from an
anion sample before analysis by using a Dionex CR-TC device, or
neutralizing a strongly acidic or basic solution—25% phosphoric acid or
sodium hydroxide solutions, for example—with an AutoNeutralization™
device. An Electrolytic Water Purifier is available which provides water of
extremely high purity (backgrounds below sub ng/L levels are possible) for
use in trace-level analytical work where use of a concentrator column is
necessary.

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1 • Introduction

Dionex ICS-5000 Detector/Chromatography Module (DC)

The DC provides a temperature-controlled environment for Dionex ICS-5000


chromatography components. The DC can accommodate components for two
channels, plumbed either serially or in parallel.
The following components may be installed in the DC:
• Conductivity detectors
• Electrochemical detectors
• Injection valves
• Switching valves
• Guard and separator columns
• Suppressors
• Dionex IC Cubes or Dionex ICS-5000 Automation Manager

Dionex ICS-5000 Conductivity Detector (CD)

The CD is a modular detector with an integrated cell. The CD has a signal


range up to 15,000 S and supports high background, nonsuppressed
applications. The CD is installed in the upper compartment of the DC. For a
dual-system, two CDs can be installed.

Dionex ICS-5000 Electrochemical Detector (ED)

The ED is a modular detector and a modular cell. The ED supports multiple


waveforms, multiple integration times, and post-analysis data manipulation.
With Chromeleon 6.8, the ED is also capable of providing 3D amperometry
data. The ED cell can be configured with gold, silver, platinum, carbon, or
glassy carbon working electrodes. The ED is installed in the upper
compartment of the DC. For a dual-system, two EDs can be installed.

Capillary Dionex IC Cube (IC Cube)


IC
The IC Cube houses components for running capillary IC applications. Each
IC Cube includes an injection valve, a column heater, and removable
cartridges containing capillary IC components. Cartridges for the following
components are available: carbonate removal device (CRD), suppressor,
guard and separator columns, and EG degasser. The IC Cube is installed in the

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Dionex ICS-5000 Operator’s Manual

upper compartment of the DC. For a dual-system, two IC Cubes can be


installed.

Dionex ICS-5000 Automation Manager (AM)

The AM consists of a component mounting panel on a base tray. The AM


provides mounting sites for sample preparation and post-column application
components: high-pressure (switching) valves, low-pressure (solenoid)
valves, reaction coils, etc. The AM is installed in the upper compartment of
the DC, above the detector.

Dionex ICS-5000 Thermal Compartment (TC)

The TC provides a temperature-controlled environment for Dionex ICS-5000


chromatography components. The TC is intended for applications that do not
require conductivity or electrochemical detection.
The TC is available in four configurations:
• With one 2-position, 6-port high-pressure injection valve
• With two 2-position, 6-port high-pressure injection valves
• With one 2-position, 6-port high-pressure injection valve and one 2-
position, 10-port high-pressure injection valve
• With no injection valves
An optional temperature stabilizer (standard bore, P/N 064548; microbore,
P/N 064650) can be installed inside the TC, if necessary. The temperature
stabilizer brings the eluent to the column temperature before it enters the
column.

Dionex AS-AP Autosampler (AS-AP)

The AS-AP provides high-performance, automated sample processing for ion


chromatography applications. Key features of the AS-AP include:
• Excellent reproducibility with RSDs less than 0.3% for full-loop
injections
• All-PEEK™ flow paths, compatible with aqueous and reversed-phase
eluents, safe from metal contamination

8 Doc. 065342-06 12/11


1 • Introduction

• Carousel and moving-needle design to guarantee reliable sampling from a


variety of vial sizes and well plates
• 10 mL polystyrene sample vials with wide openings for large-volume
injections and trace analysis
• High sample capacity, from 81 (10 mL vials) to 1152 (three 384-position
well plates)
• Sample preparation function to automate sample and standard
preparations, saving time and labor
Optional features of the AS-AP include sample tray temperature control,
simultaneous injections, sequential injections, sample preparation, or fraction
collection and reinjection, and 6-port or 10-port valves.

Dionex AS-DV Autosampler

The AS-DV is a basic autosampler that is capable of delivering between 0.1


and 5.0 mL of sample (in 0.1 mL increments) to the sample loop or
concentrator column in an ion chromatography system.
The Dionex ICS-5000 holds 50 vials (either 0.5 mL or 5.0 mL, or a
combination of the two sizes). Vials can be sampled in any order and multiple
samples can be taken from each vial. The Dionex AS-DV remembers the vial
size and volume delivered for each vial position, allowing multiple samples to
be taken from a vial non-sequentially.

Dionex AS Autosampler (AS)

The AS is a powerful, full-featured autosampler that precisely delivers from


1.0 to 100 µL (in 0.1 µL increments) or 100 to 8000 µL (in 1 µL increments)
of sample to an injection valve. In addition to the normal mode, the
autosampler can operate in several other modes, including concentrate,
simultaneous, and sequential injections.

Dionex ICS Series Photodiode Array Detector (PDA)

The PDA optical detector is capable of measuring the absorbance spectrum


from 190 to 800 nm. A deuterium lamp optimizes the UV range (190 to
380 nm) and a tungsten lamp optimizes the visible range (380 to 800 nm).
The PDA enables you to collect up to five single wavelengths (2D
chromatograms) without being required to collect 3D data. Collecting

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Dionex ICS-5000 Operator’s Manual

chromatograms at individual wavelengths instead of from spectra offers two


advantages: it eliminates the need to perform extractions for chromatograms
that do not require spectral data and it conserves disk space.

Dionex ICS Series Variable Wavelength Detector (VWD)

The VWD is a dual-beam, variable wavelength photometer with one


measurement and one internal reference beam. Spectral capability from 190 to
900 nm is provided by two light sources: a deuterium lamp for ultraviolet
detection and a tungsten lamp for visible wavelength operation. The four-
channel detector measures at up to four wavelengths simultaneously. The
VWD contains a built-in holmium oxide filter for wavelength verification. To
suppress higher-order radiation, two optical filters can be inserted
(automatically) into the light path.

MSQ Plus Mass Spectrometer

The MSQ Plus is an advanced analytical instrument that includes an MS


detector, vacuum pumps, and data system. When integrated with an IC
system, the MSQ Plus provides the separation capability of an IC and the
detection capability of a single-quadrupole MS detector. This provides a
strong starting point for sample analysis by offering a quick and clear mass
identification for chromatographic peaks.
The MS detector contains an atmospheric pressure ionization (API) source,
advanced high efficiency transmission ion optics of a square quadrupole RF
lens and dual RF generators, a mass analyzer, and an ion detection system. An
optional cone wash pump is available for improved performance when
dealing with dirty matrices.
The MS detector is equipped with FastLock™ probes for two complementary
ionization techniques: atmospheric pressure chemical ionization (APCI) and
electrospray ionization (ESI).
During a scan, ions of selected mass-to-charge ratios are sequentially
transmitted through a quadrupole mass filter analyzer. The MS detector can
perform both full-range scans and selected ion monitoring (SIM) scans.

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1 • Introduction

1.1.2 Dionex ICS-5000 System Control


The Dionex ICS-5000 system is controlled by a PC configured with Thermo
Scientific Dionex Chromeleon™ 7 Chromatography Data System (release 7.0
SR1 or later) or Thermo Scientific Dionex Chromeleon 6.8 Chromatography
Data System (release 6.8 SR9a or later). Chromeleon 7 and Chromeleon 6.8
provide complete instrument control, data acquisition, and data management.
Optionally, the Dionex ICS-5000 system can be controlled by a PC
configured with Chromeleon Xpress. Chromeleon Xpress provides real-time
control and monitoring of Dionex chromatography instruments, but does not
include data management capabilities.
In Chromeleon 7, an ePanel Set provides centralized system control. You can
use the ePanel Set to view system status information and issue commands for
controlling each module. In Chromeleon 6.8, these functions are available on
a panel tabset. In both the ePanel Set and the panel tabset, a convenient Home
panel shows the overall system status and provides basic module control
functions. Individual tabs provide quick access to additional functions for
each module and detailed status and diagnostics functions. Figure 1-2 shows

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Dionex ICS-5000 Operator’s Manual

the Home panel in Chromeleon 7 and Figure 1-3 shows the Home panel in
Chromeleon 6.8

Figure 1-2. Chromeleon 7 ePanel Set


(Dionex ICS-5000 Home Panel Shown)

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1 • Introduction

Figure 1-3. Chromeleon 6.8 Panel Tabset


(Dionex ICS-5000 Home Panel Shown)

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Dionex ICS-5000 Operator’s Manual

1.2 Dionex ICS-5000 System Documentation


Every effort has been made to provide complete and accurate user
documentation for the Dionex ICS-5000 system. The table below lists the
primary sources of product information and the formats in which information
is available.

Source Part PDF Printed


Number File Manual
Thermo Scientific Dionex ICS-5000 Ion 065342 Yes No
Chromatography System Operator’s
Manual
Installing the Thermo Scientific Dionex 065343 Yes Yes
ICS-5000 Ion Chromatography System
Dionex AS Autosampler Operator’s 065051 Yes No
Manual
Dionex ICS Series Photodiode Array 065147 Yes No
Detector Operator’s Manual
Dionex ICS Series Variable Wavelength 065141 Yes No
Detector Operator’s Manual
Chromeleon 7 Installation Guide 071686 Yes Yes
Chromeleon 7 Quick Start Guide 071679 Yes Yes
Chromeleon 7 online Help N/A N/A N/A
Chromeleon 6.8 Software User’s Guide 4829.5060 Yes No
Installing the Chromeleon 6.8 031883 Yes No
Chromatography Management System
with a Dionex Ion Chromatograph (IC)
Chromeleon 6.8 online Help N/A N/A N/A

All Adobe® PDF files listed above are shipped on the Thermo Scientific
Reference Library DVD (P/N 053891), which is included in the ship kit of
each Dionex ICS-5000 system module. In addition, the software manuals are
provided as PDF files on the Chromeleon DVD. A printed copy of the
software installation instructions is provided in the software ship kit.

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1 • Introduction

Consumables documentation: For complete information about columns,


suppressors, eluent generator cartridges, etc., refer to the appropriate product
manual. These manuals are provided on the Reference Library DVD.

1.3 The Dionex ICS-5000 System Operator’s Manual


The electronic version (i.e., PDF file) of the Dionex ICS-5000 system
operator’s manual contains numerous links that you can click to go to other
locations within the manual. These links include:
• Table of contents entries
• Index entries
• Cross-references (underlined in blue) to sections, figures, tables, etc.
If you are not familiar with how to navigate PDF files, refer to the Help
system for Adobe® Acrobat® or Adobe Reader® for assistance.

Chapter 1 An overview of the Dionex ICS-5000 system;


Introduction includes a brief description of the Dionex ICS-5000
modules, the software required for Dionex ICS-5000
operation, and the Dionex ICS-5000 user manuals.
Chapter 2 Detailed descriptions of Dionex ICS-5000 system
Description components and important operating features;
includes an introduction to Chromeleon software.
Chapter 3 Detailed illustrations of component plumbing for
System several Dionex ICS-5000 system configurations.
Configurations
Chapter 4 Tasks to be performed before beginning operation of
Getting Started the Dionex ICS-5000 system.
Chapter 5 Instructions for routine operation of the Dionex ICS-
Operation 5000 system.
Chapter 6 Short-term and long-term shutdown procedures for
Shutdown the Dionex ICS-5000 system.
Chapter 7 Routine preventive maintenance procedures for the
Maintenance Dionex ICS-5000 system.

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Dionex ICS-5000 Operator’s Manual

Chapter 8 List of Chromeleon Audit Trail error messages and a


Troubleshooting list of minor problems that may occur during
operation of the Dionex ICS-5000 system. The
possible cause of each message or problem and the
corrective action to take is included.
Chapter 9 Instructions for routine service and parts
Service replacement procedures the user can perform for the
Dionex ICS-5000 system.
Appendix A Specifications and installation site requirements for
Specifications the Dionex ICS-5000 modules.
Appendix B Spare parts for the Dionex ICS-5000 modules.
Reordering
Information

1.4 Safety and Regulatory Information


The Thermo Scientific Dionex ICS-5000 Ion Chromatography System was
manufactured by Thermo Fisher Scientific Corporation at the following
location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The Dionex
ICS-5000 system is designed for IC (ion chromatography) and HPLC (high-
performance liquid chromatography) applications and should not be used for
any other purpose. Operation of a Dionex ICS-5000 module in a manner not
specified by Thermo Fisher Scientific may result in personal injury.
If there is a question regarding appropriate usage, contact Technical Support
for Dionex products. In the U.S. and Canada, call 1-800-346-6390. Outside
the U.S. and Canada, call the nearest Thermo Fisher Scientific office.

1.4.1 Safety Messages and Notes


This manual contains warnings and precautionary statements that can prevent
personal injury and/or damage to the Dionex ICS-5000 system when properly
followed. Safety messages appear in bold type and are accompanied by icons,
as shown below.

Indicates an imminently hazardous situation which, if not avoided, will


result in death or serious injury.

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1 • Introduction

Indicates a potentially hazardous situation which, if not avoided, could


result in death or serious injury.

Indicates a potentially hazardous situation which, if not avoided, may


result in minor or moderate injury. Also used to identify a situation or
practice that may seriously damage the instrument, but will not cause
injury.
Indicates that the function or process of the instrument may be
impaired. Operation does not constitute a hazard.

Messages d'avertissement en français

Signale une situation de danger immédiat qui, si elle n'est pas évitée,
entraînera des blessures graves à mortelles.

Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures graves à mortelles.

Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures mineures à modérées. Également
utilisé pour signaler une situation ou une pratique qui pourrait
gravement endommager l'instrument mais qui n'entraînera pas de
blessures.

Warnhinweise in Deutsch

Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder


schwerwiegenden Verletzungen führen.

Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder


schwerwiegenden Verletzungen führen.

Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren


oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn
eine Situation zu schweren Schäden am Gerät führen kann, jedoch
keine Verletzungsgefahr besteht.

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Dionex ICS-5000 Operator’s Manual

Notes

Informational messages also appear throughout this manual. These are labeled
NOTE and are in bold type:

NOTE NOTES call attention to certain information. They alert you


to an unexpected result of an action, suggest how to optimize
instrument performance, etc.

Capillary Sections preceded with the Capillary IC flag indicate that the information in
IC the section applies to capillary IC systems only.
Sections preceded with the Analytical IC flag indicate that the information in
the section applies to analytical IC systems only.
If a section is not flagged, the information in the section applies to both
capillary IC and analytical IC systems.

1.4.2 Safety Symbols


These symbols appear on the Dionex ICS-5000 modules or on labels affixed
to the modules:

Alternating current

Primary protective conductor terminal

Secondary protective conductor terminal

Power supply is on

Power supply is off

Indicates a potential hazard. Refer to this operator’s


manual for an explanation of the hazard and how to
proceed.

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1 • Introduction

1.4.3 Declaration of Conformity


The cETLus or cTUVus and CE marks on the model/data labels on each
Dionex ICS-5000 module indicate that the modules are in compliance with
the following standards.

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Dionex ICS-5000 Operator’s Manual

1.5 Deionized Water Requirements for IC


For eluent generation or when manually preparing eluent and regenerant, use
ASTM Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Table 1-1.

Contaminant Specification
Ions–Resistivity >18.0 (megohm-cm)
Organics–TOC <10 ppb
Iron/Transition Metals* <1 ppb
Pyrogens <0.03 (Eu/mL)
Particulates > 0.2 µm <1 (units/mL)
Colloids–Silica <10 ppb
Bacteria <1 (cfu/mL)
* Iron/transition metal content not specified for ASTM
Type I Water

Table 1-1. ASTM Filtered, Type I Deionized Water


Specifications for Ion Chromatography

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2 • Description

ICS-5000
DP/SP DP/SP Description

2.1 DP/SP Front Features


A status bar on the front of the Dionex ICS-5000 Dual Pump (DP) and Dionex
ICS-5000 Single Pump (SP) includes buttons for controlling certain pump
functions, as well as LEDs (light emitting diodes) that indicate the status of
several pump functions (see Figure 2-1 and Figure 2-2).

FLOW PRIME FLOW PRIME

CONNECTED ALARM PUMP 1 PUMP 2

Figure 2-1. DP Status Bar

FLOW PRIME

CONNECTED ALARM PUMP 1

Figure 2-2. SP Status Bar

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Dionex ICS-5000 Operator’s Manual

Button/LED If the LED Is On If the LED Is Flashing


Label
CONNECTED The DP/SP is connected to Does not flash.
a Chromeleon 7 instrument
or Chromeleon 6.8
timebase.
ALARM A DP/SP-related problem Does not flash.
has occurred (for example,
a pressure limit was
activated). Check the
Chromeleon Audit Trail for
the cause.
PUMP 1 FLOW* Use the FLOW button to Does not flash.
PUMP 2 FLOW** start and stop the pump
flow. The LED indicates
when the flow is on.
PUMP 1 PRIME* Use the PRIME button to The pump is being primed.
PUMP 2 PRIME** prime the pump (see
Section 9.5).
The LED indicates whether
the pump is being primed.
POWER Use this POWER button for Does not flash.
routine on/off control of the
DP/SP. When the power is
on, this LED is lighted. To
turn off the DP/SP, press
and hold this POWER
button for 2 seconds.
Note: The main power
switch is on the rear panel.
* Pump 1 is always installed in the lower half of the DP/SP enclosure.
** This button is not present on the SP.

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2 • Description

2.2 DP/SP Interior Components


The pump’s mechanical components are located directly behind the front door
of the module. Figure 2-3 shows the mechanical components of a DP that
contains a gradient analytical pump (pump 1) and an isocratic capillary pump
(pump 2). Figure 2-4 identifies the pump components that are unique to a
gradient analytical pump.

1 1 Status Bar

2 Priming Valve

2 8 3 Secondary Pump Head


3 4 7
4 Primary Pump Head
5
9 5 Pressure Transducer
6 9
10
6 Priming Waste Line

11 Peristaltic Pump (for


7 seal wash system)
12
Vacuum Degas Chamber
8
(one channel)
13
9 Eluent Supply On/Off Valve
(isocratic pumps only)

9
10 Tubing Chase (2)

Pulse Damper Outlet


9
10 11 (capillary pumps only)

12 Handle (2)

14 13 Piston Seal Wash Reservoir


12
14 Leak Sensor

Figure 2-3. Example DP Interior Components:


Pump 1: Analytical Gradient Pump
Pump 2: Capillary Isocratic Pump

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Dionex ICS-5000 Operator’s Manual

1 Vacuum Degas
1 Chambers (four
channels)

Proportioning
2 Valve Fittings

Proportioning
Valve Outlet to
3 2 3
Primary Pump
Head

4 4 Static Mixer
5
Pump Outlet to
5 EG or Injection
Valve

Figure 2-4. Analytical Gradient Pump Components

NOTE For easier access to pump components when performing ser-


vice procedures, the pump panel can be pulled forward to the
front of the pump compartment. First, make sure that the five
red Phillips screws are removed from the component panel.
Then, use the handles to pull the panel forward. The upper
and lower component panels slide forward together.

2.2.1 Pump Heads


The DP/SP is a low-pulsation, serial dual-piston pump with electronic
compressibility compensation. Two pump heads—a primary head and a
secondary head—are connected in series. Eluent passes through both pump
heads in succession.
The primary pump head delivers eluent at the selected flow rate, while
simultaneously filling the secondary pump head. The latter serves as a
reservoir and delivers eluent while the primary head carries out the refill
stroke.
The characteristic feature of the patented isokinetic pre-compression phase is
the programmed overlapping of the delivery strokes of the two pump heads.
When delivering compressible liquids without controlled pre-compression,

24 Doc. 065342-06 12/11


2 • Description

the pulsation increases as the operating pressure increases, because part of the
delivery stroke is required to compress eluent in the pump head.
During the pre-compression phase, pulsation is minimized. A patented
secondary control system (automatic compressibility compensation) ensures
highly constant eluent delivery. The flow rate remains constant in relation to
the pressure.

2.2.2 Pressure Transducer


The secondary pump head contains a built-in pressure transducer to measure
the system pressure. The DP/SP instrument control firmware installed in the
pump precisely controls the pump motor speed to ensure flow rate accuracy
and to maintain constant flow and constant pressure.

2.2.3 Proportioning Valves (Gradient pump only)


In the gradient pump, which is available for analytical IC applications only,
eluent flows from the eluent reservoirs, through the vacuum degas chambers,
and into a four-way proportioning valve assembly (see Figure 2-4).
Programmed percentages of each eluent are proportioned by the four valves.

2.2.4 Vacuum Degassing Module


The DP/SP vacuum degassing module provides continuous, online eluent
degassing. Eluent quality significantly affects DP/SP performance, and
vacuum degassing eluents is one way to ensure high eluent quality.
Degassing helps prevent bubbles (caused by eluent outgassing) from forming
in the eluent proportioning valves (gradient pump only), pump heads, and
detector cell. Degassing eluents is especially important when combining
aqueous and nonaqueous components (for example, water and acetonitrile).
The vacuum degassing module is either single-channel (in an isocratic pump)
or quad-channel (in a gradient pump). The module consists of:
• A degas chamber (with degassing membranes) with internal capacity of
670 L per channel
• A dual-stage diaphragm vacuum pump
• An on-board vacuum sensor

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Dionex ICS-5000 Operator’s Manual

• The electronics required to operate the vacuum pump


• Tubing, fittings, and other accessories
The vacuum degassing module is automatically activated when the DP/SP
power is turned on. Allow about 10 minutes for the module to equilibrate.

NOTE Make sure the run time is long enough to ensure that the vac-
uum degassing module delivers the optimal degassing perfor-
mance.

Manual Control of the Vacuum Degassing Module

The vacuum degassing module normally remains on continuously. To turn it


off (for example, to investigate a leak), follow these steps:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the pump name.
4. Select the Degasser property and select Off.
5. For Chromeleon 6.8, click Execute.
6. To turn on the degasser again, select On.

2.2.5 Piston Seal Wash System


The piston seal wash system consists of a peristaltic pump, a reservoir
containing wash solution, and the connecting tubing. The wash solution is
usually ASTM Type I (18 megohm-cm) filtered and deionized water that
meets the specifications listed in Section 1.5.
When seal washing is activated, the back of the main piston seal is rinsed with
wash solution; this prolongs seal lifetime by preventing eluent crystallization
on the piston surfaces.

Notes About the DP Piston Seal Wash System

The piston seal wash system is designed for use with only one of the two
pumps in a DP module. When the DP is shipped from Thermo Fisher
Scientific, the seal wash system is connected to pump 1 (the bottom pump). If

26 Doc. 065342-06 12/11


2 • Description

necessary, connect the seal wash system to pump 2 (the top pump), instead.
For instructions on how to replumb the system, refer to Section 4.7.

NOTE For users who need to operate a piston seal wash system for
both pumps in the DP, Thermo Fisher Scientific offers an
External Seal Wash Kit (P/N 063518) or a second seal wash
system (P/N 068661).

2.2.6 Static Mixer (Analytical IC only)


For an analytical pump, a GM-3 or GM-4 static mixer is installed after the
secondary pump head (see Figure 2-3). In the gradient pump, the mixer helps
to ensure that proportioned eluents are mixed thoroughly. In the isocratic
pump, the mixer is optional, but can function as a pulse damper.
The DP/SP gradient delay volume is 600 L when a GM-3 is installed and
380 L when a GM-4 is installed. The gradient delay volume (or dwell
volume) is the volume of liquid in the system between the point where the
gradient is formed and the point where it enters the column. This includes the
mixer, transfer tubing, and swept volume in the injector or autosampler.

Capillary 2.2.7 Pulse Damper (Capillary IC only)


IC
For a capillary pump, flow output from the pressure transducer continues to
the pulse damper, which smooths minor pressure variations. From there, flow
is directed to the injection valve and then to the remainder of the
chromatography system.

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Dionex ICS-5000 Operator’s Manual

2.3 DP/SP Flow Schematics

2.3.1 Isocratic Pump Flow Schematic


Figure 2-5 illustrates the liquid flow path through an isocratic pump.

OUTLET
CHECK VALVE DI WATER
OR
ELUENT
SECONDARY PRIMARY
PUMP PUMP
HEAD HEAD

INLET
VACUUM
CHECK VALVE DEGAS

PULSE
DAMPER*

TO ELUENT GENERATOR ELUENT SUPPLY


OR INJECTION VALVE ON/OFF VALVE
*Capillary IC pumps only

Figure 2-5. Isocratic Pump Flow Schematic

• Eluent flows from the reservoir, through the vacuum degas chamber,
through the eluent supply on/off valve, and into the inlet check valve on
the primary pump head.
• The inlet check valve opens, drawing eluent into the primary pump head.
At the same time, the secondary piston pushes forward, pushing eluent
into the system. After completing the intake, the primary piston pushes
eluent through the outlet check valve and into the secondary pump head.
• Flow exits the secondary pump head and is directed to the eluent
generator (if installed) or injection valve and then to the remainder of the
chromatography system.

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2 • Description

2.3.2 Gradient Pump Flow Schematic


Figure 2-6 illustrates the liquid flow path through a gradient pump.

OUTLET ELUENT ELUENT ELUENT ELUENT


CHECK VALVE A B C D

SECONDARY PRIMARY
PUMP PUMP
HEAD HEAD

INLET
CHECK VALVE
VACUUM
DEGAS
STATIC
MIXER

A B

PROPORTIONING
VALVE D C

TO ELUENT GENERATOR
OR INJECTION VALVE

Figure 2-6. Gradient Pump Flow Schematic

• Eluent flows from the reservoirs and through the vacuum degas
chambers. The selected proportions of eluent flow out of the
proportioning valve assembly and into the inlet check valve on the
primary pump head.
• The inlet check valve opens, drawing eluent into the primary pump head.
At the same time, the secondary piston pushes forward, pushing eluent
into the system. After completing the intake, the primary piston pushes
eluent through the outlet check valve and into the secondary pump head.
• Flow exits the secondary pump head, continues through the static mixer,
and is then directed to the eluent generator (if installed) or injection valve
and then to the remainder of the chromatography system.

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Dionex ICS-5000 Operator’s Manual

2.4 DP/SP Rear Panel


Figure 2-1 illustrates the rear panel of the DP/SP.

1 Tubing Chase (2)

Main Power Switch, Fuse


2 Holder, and Power Receptacle

3 Digital I/O Port


1 4

3 5 4 Analog Pressure Output

2 6 USB Receptacle
5 (“B” Connectors)

USB Ports (3) (“A”


6
Connectors)

Exhaust Port from


7 Vacuum Degas Module
1
8 Drain Port

Figure 2-7. DP/SP Rear Panel

Tubing Chases

The tubing chases route tubing from the front of the DP/SP, through the
interior of the module, and to the rear panel.

Main Power Switch, Fuse Holder, and Power Receptacle

The rear panel power switch is the main power switch for the DP/SP. Turn on
the main power switch before initial operation and leave it on unless
instructed to turn it off (for example, before performing a service procedure).

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2 • Description

NOTE For routine on/off control, use the POWER button on the front
of the DP/SP (see Figure 2-1 and Figure 2-2). To turn off the
pump, press and hold the POWER button for 2 seconds.

The fuse cartridge contains two 2-amp IEC 60127-2 slow-blow fuses
(P/N 954773). For instructions on how to change the fuses, see Section 9.11.
The power cord plugs into the IEC 320 three-prong receptacle.

The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the DC and is easily accessible.

Le cordon d'alimentation principal est utilisé comme dispositif principal


de débranchement. Veillez à ce que la prise de base soit située/installée
près du module et facilement accessible.

Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen


Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht
zugänglich ist.

Digital I/O Port

The digital I/O port provides a connection to auxiliary devices. The connector
includes three TTL inputs and four relay outputs. Table 2-1 indicates the
functions assigned to the connector pins.
The maximum switching voltage of the relays is 24 V. The switching
current must not exceed 100 mA.

Pin Number Signal Name Signal Level Description


1 ----- ----- Not used
2 ----- ----- Not used
3 Relay 3 Out Potential-free Normally open
4 Relay 1 Out Potential-free Normally closed
5 Relay 2 Out Potential-free Normally closed
6 Relay 3 Out Potential-free Normally closed
7 Relay 1 Out Potential-free Common

Table 2-1. 25-Pin D-Sub I/O Port (Female)

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Dionex ICS-5000 Operator’s Manual

Pin Number Signal Name Signal Level Description


8 Relay 2 Out Potential-free Common
9 Gnd Ground Ground
10 Gnd Ground Ground
11 Gnd Ground Ground
12 Gnd Ground Ground
13 ----- ----- Not used
14 Relay 4 Out Potential-free Normally open
15 Relay 4 Out Potential-free Common
16 Relay 4 Out Potential-free Normally closed
17 ----- ----- Not used
18 Relay 3 Out Potential-free Common
19 Relay 1 Out Potential-free Normally open
20 Relay 2 Out Potential-free Normally open
21 Vcc Out +5V +5V, 500 mA
22 TTL Input 1 TTL Hold/Run
23 TTL Input 2 TTL Stop
24 TTL Input 3 TTL Start
25 ----- ----- Not used

Table 2-1. 25-Pin D-Sub I/O Port (Female) (Continued)

Analog Pressure Output

The analog pressure output indicates the operating pressure of the pump. The
pressure output is set to 50 mV/MPa (5 mV/14.51 psi). To monitor the
pressure, connect the pressure output to a recorder or an A/D converter. These
are the pin assignments for the 2-pin Cinch connector (P/N 8005.9001A):

Signal Level Function


Inner ring: Signal (pressure)
Outer ring: Ground

32 Doc. 065342-06 12/11


2 • Description

The analog pressure output defaults to the pump 1 (bottom pump) output
signal. To redirect the output to pump 2 (the top pump), follow these steps:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the pump name.
4. Select the AnalogOut property and select PumpTop. For Chromeleon
6.8, click Execute.

USB Connections

• One USB receptacle (“B” type connector) allows a connection from the
PC on which Chromeleon is installed.
• Three USB (Universal Serial Bus) ports (“A” type connectors) are
provided for connections to other Dionex ICS-5000 modules.
One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the pump ship kit:

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

Waste and Drain Lines

• One waste line is connected to the secondary pump head on each pump
and is routed through the tubing chace to the rear of the DP/SP.
• The drain port removes any liquid that collects in the drip tray in the
bottom of the DP/SP. A clear corrugated drain hose (P/N 055075) is
connected to this port during installation.
Place the free ends of the waste lines and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
pump.
For correct drainage, make sure the waste lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.

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Dionex ICS-5000 Operator’s Manual

2.5 Eluent Reservoirs


The following reservoirs are available for use with the DP/SP:
• 1-liter plastic reservoir (P/N 063291)
• 2-liter plastic reservoir (P/N 062510)
• 4-liter plastic reservoir (P/N 063292)
Do not use the plastic reservoirs for offline vacuum degassing of
eluents. The reservoirs were not designed for this purpose.

N'utilisez pas le réservoir en plastique pour le dégazage à vide hors


ligne d'éluants. Le réservoir n'a pas été conçu à cette fin.

Verwenden Sie keine Plastikbehälter zum Offline Vakkum-Entgasen von


Eluenten. Die Behälter sind dafür nicht ausgelegt.

2.5.1 EO (Optional)
The Dionex ICS-5000 Eluent Organizer (EO) holds eluent reservoirs in a liner
that contains spills and leaks. Up to two EOs can be installed on top of the
DC. Each EO accommodates up to four 1-liter or 2-liter reservoirs or up to
two 4-liter reservoirs. The EO is typically ordered configured with four 2-liter
reservoirs (P/N 072058).

2.5.2 Pressurizing Eluent Reservoirs


All eluent reservoirs available for use with the DP/SP can be pressurized.
Although the DP/SP does not require pressurized reservoirs, Thermo Fisher
Scientific recommends pressurizing reservoirs with helium or nitrogen under
the following circumstances:
• When using eluents that are sensitive to contamination.

34 Doc. 065342-06 12/11


2 • Description

• When combining aqueous and nonaqueous components (for example,


water and acetonitrile). Pressurizable reservoirs allow eluents to be stored
under a specific atmosphere.
Never pressurize eluent reservoirs above 0.07 MPa (10 psi).
Pressurizing reservoirs above this limit can cause the reservoir to
explode.

Ne mettez jamais les réservoirs d'éluants sous une pression supérieure


à 0,07 MPa (10 psi).

Setzen Sie den Eluentbehälter auf keinen Fall einem Druck über
0,07 MPa aus.

If you plan to pressurize the eluent reservoirs, an optional regulator kit is


required. The kit is available in two versions:
• When the DC is installed as the topmost module in the system, the EO
Regulator Kit (P/N 074422) is required. The kit includes a pressure
regulator and gauge assembly with four outputs (for connections to four
eluent reservoirs), as well as the tubing and connection fitting required.
• When the TC, VWD, or PDA is installed as the topmost module in the
system, the TC/VWD/PDA Regulator Bracket Kit (P/N 074424) is
required. The kit includes the EO Regulator Kit described above, as well
as a right-angle regulator bracket and mounting hardware. After attaching
the bracket to the TC or detector, you will mount the gas regulator
assembly on the bracket.
If more reservoirs are required, order a second regulator (P/N 074423).
For instructions on installing the regulator kits, refer to Thermo Scientific
Dionex ICS-5000 Ion Chromatography System Installation Instructions
(Document No. 065343). The manual is included on the Thermo Scientific
Reference Library DVD (P/N 053891).

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Dionex ICS-5000 Operator’s Manual

2.5.3 Filtering Eluent


• Install an end-line filter (P/N 045987) on the end of each reservoir’s
eluent line. End-line filters are provided in the pump ship kit.
• A Dionex High-Pressure Inline Filter (P/N 044105) can be used to
remove particulates down to 0.45 micron from eluent. Connect the inline
filter between the pump outlet and the eluent inlet port on the injection
valve. For details, see the instructions provided with the inline filter.

36 Doc. 065342-06 12/11


ICS-5000
EG EG Description

2.6 EG Front Features


The status bar on the front of the Dionex ICS-5000 Eluent Generator (EG)
includes buttons that provide control of certain EG functions, as well as LEDs
that indicate the status of several EG functions (see Figure 2-8).

1 2 1 2

CONNECTED ALARM EGC CR-TC

Figure 2-8. EG Status Bar

Button/LED If the LED Is On Comment


Label
CONNECTED The EG is connected to a -----
Chromeleon 7 instrument or
a Chromeleon 6.8 timebase.
ALARM An EG-related problem has Check the Chromeleon Audit
occurred (for example, the Trail for the cause.
eluent generator cartridge
(EGC) was disconnected).
EGC 1 The EGC is on and is EGC 1 is always installed in
EGC 2 generating eluent. the left section of the
component compartment.
EGC 2, if present, is installed
in the right section of the
compartment.
CR-TC 1 The CR-TC is on. CR-TC 1 is always installed in
CR-TC 2 the left section of the
component compartment.
CR-TC 2, if present, is
installed in the right section of
the compartment.

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Dionex ICS-5000 Operator’s Manual

Button/LED If the LED Is On Comment


Label
POWER Use this POWER button for The main power switch is on
routine on/off control of the the EG rear panel.
EG. When the power is on,
this LED is lighted. To turn off
the EG, press and hold this
POWER button for
2 seconds.
NOTE: The EG status bar LEDs do not flash.

2.7 EG Interior Components


The EG component compartment, which is located directly behind the front
door, accommodates the components required for generating eluent in a single
system or in both channels of a dual system. A component mounting panel
divides the compartment into two sections.
• The left section is for a single-channel EG or for system 1 of a dual-
channel EG.
• The right section is for system 2 of a dual-channel EG.
Each section holds the components for either a capillary IC or an analytical IC
system. A dual-channel EG can hold components for two capillary IC
systems, two analytical IC systems, or one system of each type.
Figure 2-9 shows the component panel for a capillary IC system. Figure 2-10
shows the component panel for an analytical IC system

38 Doc. 065342-06 12/11


2 • EG Description

To access components for maintenance or service procedures, push down on


the slide release latch and pull the tray forward until it reaches the stop.

1 EGC (Capillary)

Chase for Electrical


2
Cables

3 CR-TC (Capillary)

4 Leak Sensor
1
5 Drip Tray

6 Slide Release Latch


2

Note:
For a capillary IC
3 system, the eluent
4 degasser is installed in
the IC Cube.

5 6

Figure 2-9. Example EG Interior Components for a Capillary IC System


(System 1 Shown)

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Dionex ICS-5000 Operator’s Manual

1 EGC III (Analytical)

RFIC Eluent Degasser


2
1 (for Analytical IC only)
2
3 Electrical Cables

4 CR-TC (Analytical)

5 Drip Tray

3 6 Slide Release Latch

6 5

Figure 2-10. Example EG Interior Components for an Analytical IC System


(System 2 of a Dual-Channel EG Shown)

40 Doc. 065342-06 12/11


2 • EG Description

Eluent Generator Cartridge (EGC)

Table 2-2 lists the versions of eluent generator cartridges available for use
with the EG. Each EGC contains an electrolyte concentrate solution
appropriate for the particular eluent generation. Each EGC is designed to be
used in either a capillary IC system or an analytical IC system. An EGC
designed for a capillary IC system cannot be used in an analytical IC system,
and vice versa.
Analytical IC systems require EGC III cartridges and (if used) the EPM III
Electrolytic pH Modifier. Previous versions of EGC or EPM are not
compatible with the Dionex ICS-5000 Eluent Generator.

EGC Version Part Function


Number
Eluent Generator Cartridges for Capillary IC Systems
EGC KOH (Capillary) 072076 Generates potassium hydroxide eluent
for anion exchange separations.
EGC MSA (Capillary) 072077 Generates methanesulfonic acid eluent
for cation exchange separations.
Eluent Generator Cartridges and Accessories for Analytical IC Systems
EGC III K2CO3 074536 Generates potassium carbonate eluent
for anion exchange separations.
EPM III Electrolytic 080135 Produces a carbonate/ bicarbonate
pH Modifier mixture when installed with the EGC III
K2CO3. Requires a carbonate mixer:
P/N 061686 (4 mm); P/N 063443
(2 mm).
EGC III KOH 074532 Generates potassium hydroxide eluent
for anion exchange separations.
EGC III LiOH 074534 Generates lithium hydroxide eluent for
anion exchange separations.
EGC III MSA 074535 Generates methanesulfonic acid eluent
for cation exchange separations.
EGC III NaOH 074533 Generates sodium hydroxide eluent for
anion exchange separations.

Table 2-2. Capillary and Analytical EGCs

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Dionex ICS-5000 Operator’s Manual

For more information, refer to the EGC manual. The manual is included on
the Thermo Scientific Reference Library DVD (P/N 053891).

Continuously Regenerated Trap Column (CR-TC)

The CR-TC is a high pressure, electrolytically-


regenerated trap column. The CR-TC is designed to
remove anionic or cationic contaminants in the eluent or
deionized water and to reduce drift during gradient
separations. The following versions of the CR-TC can be
used with the EG:

CR-TC Version IC System Part


Type Number
Continuously Regenerated Anion Trap Column Capillary 072078
(Capillary); CR-ATC (Capillary)
Continuously Regenerated Cation Trap Column Capillary 072079
(Capillary); CR-CTC (Capillary)
Continuously Regenerated Anion Trap Column; Analytical 060477
CR-ATC
Continuously Regenerated Cation Trap Column; Analytical 060478
CR-CTC II

Figure 2-11. Capillary and Analytical CR-TCs

For more information, refer to the CR-TC manual. The manual is included on
the Thermo Scientific Reference Library DVD (P/N 053891).

NOTE Do not install a CR-TC in the same channel as an EGC


K2CO3 or an EPM III Electrolytic pH Modifier.

NOTE The Thermo Scientific Dionex IonPac™ ATC-HC Trap Col-


umn (P/N 059604) or Thermo Scientific Dionex IonPac
CTC-1 Trap Column (P/N 040192) may be used with the EG.
However, both Dionex IonPac trap columns require off-line
chemical regeneration. Contact Thermo Fisher Scientific for
more information.

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2 • EG Description

RFIC Eluent Degasser

For analytical IC systems, an RFIC Eluent Degasser (P/N 062137) is installed


on the EG component mounting panel. The degasser contains a tubing
assembly that purges the electrolysis gas from the freshly-generated eluent
before it is directed to the separator column.
Capillary For capillary IC systems, the degasser is installed in the IC Cube (see
IC Section 2.11.2).

Backpressure Coil (Optional)

For analytical IC systems, the EGC requires at least 14 MPa (2000 psi) of
system backpressure for removal of electrolysis gas from the eluent produced
by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal.
If necessary, increase the system backpressure by installing a backpressure
coil between the injection valve and the EGC OUTLET port. For details, refer
to Section 9.17.

EPM III Electrolytic pH Modifier and Carbonate Mixer

The EGC III K2CO3 can be used with an EPM III Electrolytic pH Modifier
(P/N 080135) and a carbonate mixer (P/N 061686, 4 mm; P/N 063443, 2 mm)
to produce a carbonate/bicarbonate mixture for use with anion exchange
separations on carbonate-based Dionex IonPac columns.
After the cartridge generates potassium carbonate eluent, the EPM adjusts the
eluent concentration to produce the carbonate/bicarbonate mixture. The
carbonate mixer provides mixing necessary to produce a homogenous
solution of electrolytically-generated K2CO3 and KHCO3 eluent.
For more information about these products, refer to the EGC manual. EGC
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).

Leak Sensor

If liquid collects in the drip tray in the bottom of the EG, a leak sensor reports
the leak to Chromeleon, and an error message is displayed in the Audit Trail.
In addition, the Alarm LED on the EG front panel lights.

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Dionex ICS-5000 Operator’s Manual

Electrical Connections

Electrical connectors provide a connection from the components installed in


the EG to the EG power supplies. There are two sets of electrical connectors
(one per channel). Connections for the following components are provided:
• Two EGCs or one EGC and one EPM
and
• Two CR-TCs
When operating with an EGC III K2CO3 and the EPM III, the EGC is
connected to the EGC power supply for one channel and the EPM is
connected to the EGC power supply for the second channel. Thus, the EG can
accommodate only one such configuration.

44 Doc. 065342-06 12/11


2 • EG Description

2.8 EG Rear Panel


Figure 2-12 illustrates the rear panel of the Dionex ICS-5000 Eluent
Generator (EG).

1 1 Exhaust Fan

2 Gas Vent Lines

2
USB Receptacle
3 (“B” Connector)

USB Ports (2)


4
(“A” Connectors)

3 Fuse Holder, Main Power


5 Switch, and Power
4 Receptacle

Tubing for Connecting to


6 Suppressors
6
5 7 Tubing Chase

8 Drain Port
7

Figure 2-12. EG Rear Panel

Exhaust Fan

The exhaust fan cools the interior of the EG and exhausts any hydrogen and
oxygen gases that escape during operation.

USB Connections

• One USB receptacle (“B” type connector) allows a connection from the
PC on which Chromeleon is installed.
• Two USB (Universal Serial Bus) ports (“A” type connectors) are
provided for connections to other Dionex ICS-5000 modules.

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Dionex ICS-5000 Operator’s Manual

One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the EG Ship Kit
(P/N 072047).

Fuse Holder, Main Power Switch, and Power Receptacle

The fuse cartridge contains two 2-amp slow-blow fuses (P/N 954773). For
instructions on how to change the fuses, see Section 9.18.
The rear panel power switch is the main power switch for the EG. Turn on the
main power switch before initial operation and leave it on unless instructed to
turn it off (for example, before performing a service procedure).

NOTE For routine on/off control, use the POWER button on the front
of the EG (see Figure 2-8). To turn off the EG, press and hold
the POWER button for 2 seconds.

The power cord plugs into the IEC 320 three-prong receptacle.

The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the EG and is easily accessible.

Le cordon d'alimentation principal est utilisé comme dispositif principal


de débranchement. Veillez à ce que la prise de base soit située/installée
près du module et facilement accessible.

Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen


Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht
zugänglich ist.

Tubing Chase

The tubing chase routes tubing from the front of the EG, through the interior
of the module, and to the rear panel.

Suppressor, Vent, and Drain Lines

• The lines exiting the tubing chase (white tubing) are for connecting the
REGEN IN port on the RFIC Eluent Degasser or EPM III Electrolytic pH
Modifier to the REGEN OUT port on the suppressor.
• The gas vent line (clear tubing) discharges the electrolysis gas (H2 or O2)
that is vented from the electrolyte reservoir of the EGC.

46 Doc. 065342-06 12/11


2 • EG Description

• The drain port removes any liquid that collects in the drip tray in the
bottom of the EG. A clear corrugated drain hose (P/N 055075) is
connected to this port during installation.
Place the free ends of the vent lines and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
EG.
For correct drainage, make sure the vent lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.

2.9 EG Flow Schematics


Liquid flows through the EG components in the following order:
• The pump delivers deionized water to the EGC. Direct current is applied
to the EGC to produce eluent.
• The electrolytically-generated eluent flows to the CR-TC (which traps
ionic contaminants) and then into the degasser.
• After exiting the degasser, the eluent flows through the backpressure coil
(if installed), through the injection valve to the separator column, and
finally to the detector cell.
• The detector cell effluent is directed through the suppressor regenerant
chamber, to the degasser regenerant tubing, through the CR-TC
regenerant chamber, and finally to waste.
The flow paths for a capillary IC and an analytical IC system are the same.
However, in a capillary IC system, a degasser cartridge is located in the IC
Cube inside the DC. In an analytical IC system, the degasser is located inside
the EG.
Capillary Figure 2-13 illustrates the liquid flow path through an EG configured for a
IC capillary IC system.
Figure 2-14 illustrates the liquid flow path through an EG configured for an
analytical IC system.

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Dionex ICS-5000 Operator’s Manual

Vent

EGC
(Capillary)

EGC
IN

EGC
OUT
TO PUMP/DAMPER

WASTE, GAS
SEPARATOR
EG To CR-TC
Degas Regen Out
Cartridge (blue label)
(inside DC)

To CR-TC To CR-TC

ELUENT OUT
REGEN IN
REGEN OUT

Eluent In Eluent Out


(red label) (yellow label)
To EG Degas
Regen Out To CR-TC
ELUENT OUT
(blue label) Regen In
(orange label)

To Inject ELUENT IN To EG Degas


Valve Eluent In
(red label)

Figure 2-13. EG Flow Schematic Example for Capillary IC

48 Doc. 065342-06 12/11


2 • EG Description

EGC VENT

EGC
RFIC
Eluent
Degasser

Regen Regen
To Waste Out In

Eluent Eluent
Out In
Inlet Outlet
EGC
IN
EGC
TO PUMP OUT
Coupler
TO INJ VALVE - P

Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Regen In
TO CR -TC (orange label)
WASTE, GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
ELUENT OUT

To CR-TC
REGEN IN

Eluent In
(red label)

CR-TC

Figure 2-14. EG Flow Schematic Example for Analytical IC

NOTE Refer to the EGC-CO3 Mixer manual for a flow schematic


showing the components required to generate a carbon-
ate/bicarbonate mixture. The manual is included on the
Thermo Scientific Reference Library DVD (P/N 053891).

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Dionex ICS-5000 Operator’s Manual

50 Doc. 065342-06 12/11


ICS-5000
DC DC Description

2.10 DC Front Features


The status bar on the front of the Dionex ICS-5000 Detector/Chromatography
Module (DC) (see Figure 2-15) includes buttons for controlling certain DC
functions, as well as LEDs that indicate the status of several DC components
and functions.

1 2 UPPER LOWER LOAD INJECT LOAD INJECT

CONNECTED ALARM SUPPRESSOR OVEN VALVE 1 VALVE 2

Figure 2-15. DC Status Bar

Button/LED If the LED Is On If the LED Is Flashing


Label
CONNECTED The DC is connected to a Does not flash.
Chromeleon 7 instrument or
Chromeleon 6.8 timebase
ALARM The leak sensor is wet or there Does not flash.
was a valve or suppressor
error. Check the Chromeleon
Audit Trail for the cause.
SUPPRESSOR 1 The suppressor is on and Does not flash.
SUPPRESSOR 2 current is being applied.
OVEN UPPER The upper compartment is at The upper compartment
its set temperature. is transitioning to the set
temperature. The
compartment is not
ready for operation.
OVEN LOWER The lower compartment is at its The lower compartment
set temperature. is transitioning to the set
temperature. The
compartment is not
ready for operation.

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Dionex ICS-5000 Operator’s Manual

Button/LED If the LED Is On If the LED Is Flashing


Label
VALVE 1 LOAD Use the VALVE 1 and VALVE 2 Valve error. See
VALVE 2 LOAD buttons to manually switch the Section 8.25 for
VALVE 1 INJECT position of the DC injection troubleshooting.
VALVE 2 INJECT valves. The LEDs indicate
whether the valve is in the
Load or Inject position.
Use this POWER button for Does not flash.
POWER routine on/off control of the
DC. When the power is on, this
LED is lighted. To turn off the
DC, press and hold this
POWER button for 2 seconds.
Note: The main power switch
is on the DC rear panel.

NOTE The VALVE 1 and VALVE 2 buttons can be enabled and dis-
abled in Chromeleon. When disabled, you can control the
valve only from the software. To enable or disable a button,
open the Commands dialog box (press the F8 key), select the
Advanced or Expert user level, and select the Valve1Button
(or Valve2Button) property in the list of properties for the
DC.

The front of the DC has two sample loading ports (see Figure 2-16) that can
be connected to injection valves installed inside the DC. A syringe can then be
used to manually load sample through the ports. For automated sample

52 Doc. 065342-06 12/11


2 • DC Description

injection, the DC can be connected to an autosampler. For more information


about sample injection, see Section 5.2.

Sample
Loading Ports

Figure 2-16. DC Sample Loading Ports

2.11 DC Interior Components


The interior of the DC consists of two temperature controlled compartments
(upper and lower). To access the upper compartment, lift up the top door. To
access the lower compartment, pull down the lower door.
The upper and lower compartments are isolated from each other in separate
temperature zones. There is no common air flow between the two
compartments. For details about DC temperature control, see Section 2.12.
The compartments can accommodate the components necessary for up to two
IC systems. The following configurations are possible:
• Single system: one capillary IC or one analytical IC system
• Dual system: two capillary IC systems or two analytical IC systems; or
one system of each type (a “hybrid”)

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Dionex ICS-5000 Operator’s Manual

Capillary 2.11.1 DC Interior Components for Capillary IC


IC
In capillary ion chromatography systems, the upper compartment of the DC
houses the required components. If the DC is used for capillary IC only, the
lower compartment is unused.
The DC upper compartment consists of two sections:
• The top section houses one or two Dionex IC Cubes (IC Cube). For
details about the IC Cube, see Section 2.11.2. The tray slides forward for
easy access to components.
• The lower section houses either one or two Dionex ICS-5000
Conductivity Detectors (CDs), one or two Dionex ICS-5000
Electrochemical Detectors (EDs), or one detector of each type. For details
about the CD, see Section 2.14. For details about the ED, see
Section 2.15.

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2 • DC Description

Figure 2-17 shows the upper compartments of a DC that is configured for two
capillary IC systems. Both systems are configured for conductivity detection.

1 3

2 4

1 IC Cube (System #1) 3 IC Cube (System #2)

Conductivity Detector Conductivity Detector


2 (Capillary) (System #1) 4 (Capillary) (System #2)

Figure 2-17. Example DC Interior View


(Upper Compartment of a Dual IC System Shown)

Capillary 2.11.2 IC Cube for Capillary IC


IC
The IC Cube houses components for running capillary IC applications. The IC
Cube is installed in the upper compartment of the DC. For a dual-system, two
IC Cubes can be installed.

NOTE When an IC Cube is installed, a Dionex ICS-5000 Automa-


tion Manager cannot be included in the DC.

Each IC Cube includes an injection valve, a column heater, and four


component cartridges that slide into the housing. Each cartridge holds a
capillary IC component and includes the plumbing required to connect the
component to other IC Cube and system components.

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Dionex ICS-5000 Operator’s Manual

Cartridges for the following components are available: carbonate removal


device (CRD); suppressor, guard and separator columns; and EG degasser.

NOTE If the IC Cube does not include a CRD or suppressor, bypass


cartridges must be installed. Bypass cartridges provide the
internal plumbing connections required for eluent and regen-
erant flow between IC Cube components.

Figure 2-18 illustrates the features of the IC Cube.

CRD Cartridge or CRD


1 Bypass Cartridge

1 2 3 4 Suppressor Cartridge
2 or Suppressor Bypass
Cartridge

Column Heater and


5 3
Column Cartridge

4 EG Degas Cartridge

5 Injection Valve

Figure 2-18. IC Cube Features

Capillary CRD Cartridge or CRD Bypass Cartridge


IC
The CRD 200 (Capillary) cartridge (P/N 072054) contains a CRD 200
Carbonate Removal Device (Capillary). The CRD 200 (Capillary) removes
the carbonate peak contributed by the sample in hydroxide eluent chemistries.
Removal occurs immediately after suppression of the eluent, before the
sample reaches the detector. The CRD 200 (Capillary) is optimized for
operation at the flow rate range typically used with capillary columns.
The CRD and tubing connections inside the cartridge are not accessible.
Tubing exits the front of the cartridge to allow connection to other capillary
IC components.
Installation of a CRD 200 (Capillary) is optional. However, if one is not used,
a CRD bypass cartridge (P/N 072056) must be installed. The bypass cartridge

56 Doc. 065342-06 12/11


2 • DC Description

contains the plumbing connections necessary for eluent and waste flow
through the system.

Capillary Suppressor Cartridge or Suppressor Bypass Cartridge


IC
Two versions of capillary suppressor cartridges are available: ACES 300
Anion Capillary Electrolytic Suppressor cartridge (P/N 072052) and CCES
300 Cation Capillary Electrolytic Suppressor cartridge (P/N 072053). Each
cartridge holds a suppressor and the required tubing connections for eluent
and regenerant flow to the suppressor. The suppressor and tubing connections
inside the cartridge are not accessible. Tubing exits the front of the cartridge
to allow connection to other capillary IC components.
When the cartridge is installed in the IC Cube, pins on the rear of the cartridge
connect the suppressor to its power source. For details about the suppressors,
refer to the suppressor manuals. The manuals are on the Thermo Scientific
Reference Library DVD (P/N 053891).
Installation of a suppressor is optional. However, if one is not used, a
suppressor bypass cartridge (P/N 072055) must be installed. The suppressor
bypass cartridge contains the plumbing connections necessary for eluent and
waste flow through the system.

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Dionex ICS-5000 Operator’s Manual

Capillary Column Heater and Column Cartridge


IC
The IC Cube column heater provides a temperature-controlled compartment
for the capillary guard and separator columns. The heater temperature range is
from 5 °C above the temperature of the upper DC compartment to 80 °C.
A column cartridge slides into the column heater and is secured with two
thumbscrews. The column cartridge contains the capillary guard column (if
included) and the capillary separator column. To access the columns,
disconnect the inlet and outlet tubing, loosen the captive screws, and slide the
cartridge out of the oven. The cartridge hinges open, providing access to the
columns and column plumbing. The capillary columns are ordered separately.
For information about how to replace columns and column tubing, see
Section 9.26.2.

Capillary EG Degas Cartridge


IC
The EG degas (capillary) cartridge contains a tubing assembly that purges the
electrolysis gas from eluent that has been generated by an EG. After passing
through the degas tubing the eluent is directed to the injection valve and then
to the guard and separator columns.
The EG degas (capillary) cartridge also contains plumbing connections that
route the regenerant flow from the suppressor out of the IC Cube to the
regenerant inlet port of the Continuously Regenerated Trap Column
(Capillary) in the EG.
If the system does not include an EG, the eluent inlet line from the EG degas
cartridge is connected directly to the pump outlet. The regenerant outlet line is
directed to waste.

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2 • DC Description

Capillary IC Cube Eluent and Regenerant Flow


IC
The numbers on the schematic shown in Figure 2-19 indicate the flow path of
eluent and regenerant through the plumbing connections on an IC Cube
configured for conductivity detection.

ELUENT IN
ELUENT IN REGEN OUT
ELUENT OUT

6 5 14
ELUENT IN
9 ELUENT OUT
7 To CR-TC
ELUENT OUT 2 Regen In Port
ELUENT OUT
4 ELUENT IN
8 3 EG
CRD 200 CES 300 DEGAS

ELUENT OUT REGEN IN


From
Autosampler SAMPLE IN 1
10 13 SAMPLE OUT ELUENT IN
To Waste From CR-TC
Eluent Out Port

CELL IN 12 CELL OUT


Conductivity Detector
(Capillary)
11

Figure 2-19. IC Cube Eluent and Regenerant Flow Schematic for


Conductivity Detection

NOTE For the complete conductivity detection flow path, including


the flow through components installed inside the IC Cube
cartridges, see Section 2.14.3.

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The numbers on the schematic shown in Figure 2-20 indicate the flow path of
eluent and regenerant through the plumbing connections on an IC Cube
configured for electrochemical detection.

ELUENT IN
REGEN OUT
ELUENT OUT

5 10
6
ELUENT OUT
To CR-TC
ELUENT OUT 2 Regen In Port
4
CRD SUPPRESSOR
3 ELUENT IN EG
BYPASS BYPASS DEGAS

REGEN IN
From
Autosampler SAMPLE IN
1
9 SAMPLE OUT ELUENT IN
To Waste From CR-TC
Eluent Out Port

EC CELL
8 OUT

IN 7

Figure 2-20. IC Cube Eluent and Regenerant Flow Schematic for


Electrochemical Detection (PdH Electrode Shown)

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2 • DC Description

2.11.3 DC Interior Components for Analytical IC


Figure 2-21 shows the interior compartments of a DC that is configured with
the components for two analytical IC systems. System #1 is used for
electrochemical detection applications and system #2 is used for conductivity
detection applications.

Upper Compartment
1
Automation
1 Manager
Components

Electrochemical
2 Detector and Cell
3
2

Conductivity
3 Detector and
Suppressor

Lower Compartment

Columns and
4 4 Injection
Valves

Figure 2-21. Example DC Interior View


(Dual Analytical IC System Shown)

Upper Compartment Features for Analytical IC

The upper compartment consists of two sections:


• The top section houses an optional Dionex ICS-5000 Automation
Manager (AM). The AM contains various components required for
performing matrix elimination, large volume pre-concentration, post-
column reagent addition, and other functions. See Section 2.18 for details
about the AM.
• The lower section houses either one or two Dionex ICS-5000
Conductivity Detectors (CDs), one or two Dionex ICS-5000
Electrochemical Detectors (EDs), or one detector of each type. For details
about the CD, see Section 2.14. For details about the ED, see
Section 2.15.

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Suppressors for conductivity detection are also installed in the upper


compartment. The following types of suppressors can be used:
• Thermo Scientific Dionex SRS™ 300 Self-Regenerating Suppressor
(2 and 4 mm)
• Thermo Scientific Dionex AES™ Atlas™ Electrolytic Suppressor
• MMS™ 300 MicroMembrane™ Suppressor

Lower Compartment Features for Analytical IC

The lower compartment can hold up to two column sets (four columns) with
IDs of 1 mm to 9 mm and lengths of 100 mm to 250 mm.
The lower compartment also holds one or two injection valves. Two valve
versions (6-port and 10-port) are available. Both versions are electrically-
activated, two position valves. See Section 2.13 for details about the injection
valves.
The compartment tray slides forward about 10 cm (4 in) for easy access to
columns and valves. To pull the tray forward, use the handle installed in the
center of the compartment (see Figure 2-22).

Handle for pulling tray forward

Figure 2-22. DC Lower Compartment Tray Handle

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2 • DC Description

2.12 DC Temperature Control Zones


The following temperature control zones are possible with the DC, depending
on the options installed:
• DC upper compartment
• DC lower compartment
• Heated conductivity cell
Capillary • IC Cube capillary column heater
IC
• RCH-1 Reaction Coil Heater (installed in an AM)
The temperatures achieved for a particular zone can vary from the control
range, depending on the ambient temperature (see Table 2-3).

Temperature Control Achieved Temperatures (Based on Ambient)


Zone Range
Upper 10 to • If no temperature-controlled devices (CD cell,
compartment 40 °C IC Cube heater, or RCH-1) are on:
Minimum temperature  (ambient  22 °C)
• If a temperature-controlled device is set to
60 °C or above:
Minimum temperature  (ambient  17 °C).
Note: The achieved temperature can be
reduced another few degrees by setting the DC
upper compartment fan speed to high (see
page 64).
• Maximum temperature  (ambient  20 °C)
Lower 10 to Minimum temperature  (ambient 5 °C)
compartment 70 °C Maximum temperature  (ambient  50 °C)
CD cell 15 to Minimum temperature  (upper compartment
60 °C temperature + 5 °C)
IC Cube column 15 to Minimum temperature  (upper compartment
heater 80 °C temperature + 5 °C)
RCH-1 20 to Minimum temperature  (upper compartment
80 °C temperature + 5 °C)

Table 2-3. Achieved Temperatures per DC Temperature Zone

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Minimum temperatures are also affected by the ambient humidity. If the


humidity is high, the minimum temperatures achieved for a temperature zone
is not as low as those achieved in a low ambient humidity environment.

NOTE A DC Temperature Calibration Kit (P/N 063782) is available.


The kit includes the parts and instructions required to verify
the temperature calibration of the DC upper and lower com-
partments and to recalibrate, if required.

To set the fan speed of the DC upper compartment to high:


1. Open the Chromeleon 7 Instrument Configuration program or
Chromeleon 6.8 Server Configuration program.
2. Double-click the DC icon under the instrument or timebase.
3. Click the Thermal Controls tab and then double-click
Compartment_TC.
4. Under Fan Speed, click High Speed (see Figure 2-23).

Figure 2-23. Setting the DC Upper Compartment Fan Speed

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2 • DC Description

2.13 High-Pressure Valves


Up to four high-pressure valves can be installed in the DC. The following
valve models are available: 4-port (P/N 074525), 6-port (P/N 061961), and
10-port (P/N 061962).
Capillary In a capillary IC system, one 4-port high-pressure valve is installed on each IC
IC Cube. This valve is used for sample injection. Optionally, the 6-port valve can
be installed instead of the 4-port valve. In addition to the injection valve, one
or two high-pressure valves can be installed in the lower compartment. These
valves can be used for applications requiring auxiliary valves.
In an analytical IC system, one 6-port high-pressure valve is installed in the
lower compartment for each system configured in the DC.This valve is used
for sample injection. Optionally, one or two high-pressure valves can be
installed on an AM (see Section 2.18). These valves can be used for
applications requiring auxiliary valves.
Each valve has two operating positions. When configured as an injection
valve, liquid flows through either the Load or Inject path, depending on the
valve position. In the Load position, sample is loaded into the sample loop. In
the Inject position, sample is swept to the column for analysis.
When configured as an auxiliary valve, the flow path through system
components in each valve position depends on the component configuration.

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2.13.1 4-Port Valve


The 4-port valve (P/N 074525) is the standard injection valve for capillary IC
systems. It is installed in the IC Cube (see Figure 2-18). The valve has a
0.4 L internal sample loop. Figure 2-24 shows flow schematics for the 4-port
valve.

LOAD POSITION INJECT POSITION

Internal Internal
Sample In Sample In
Loop Loop
S S
To To
5 5
Column Column
W 6 3 W 6 3
To 2 To 2
Waste Waste

From Pump From Pump

= Sample = Eluent

Figure 2-24. Injection Valve Flow Schematics (4-Port Valve)

• In the Load position, sample flows from the syringe or autosampler line
(if installed), through the valve, and into the internal sample loop, where
it is held until injection. Excess sample flows out to waste. Eluent flows
from the pump, through the valve, and to the column, bypassing the
sample loop.
• In the Inject position, eluent flows from the pump, through the internal
sample loop, and on to the column, carrying the contents of the sample
loop with it. Section 5.3.1 describes how to inject samples with an
autosampler and Section 5.3.2 describes how to inject samples manually.

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2 • DC Description

2.13.2 6-Port Valve


The 6-port valve (P/N 061961) is the standard injection valve for analytical IC
systems. It is installed in the lower compartment of the DC (see Figure 2-21).
Figure 2-25 shows flow schematics for the 6-port valve.

LOAD POSITION INJECT POSITION

Sample Sample
Sample In Sample In
Loop Loop
S L S L
To To
5 4 5 4
Column Column
W 6 3 W 6 3
To 1 2 To 1 2
Waste L Waste L

From Pump From Pump

= Sample = Eluent

Figure 2-25. Injection Valve Flow Schematics (6-Port Valve)

• In the Load position, sample flows from the syringe or autosampler line
(if installed), through the valve, and into the sample loop, where it is held
until injection. Excess sample flows out to waste. Eluent flows from the
pump, through the valve, and to the column, bypassing the sample loop.
• In the Inject position, eluent flows from the pump, through the sample
loop, and on to the column, carrying the contents of the sample loop with
it. Section 5.3.1 describes how to inject samples with an autosampler and
Section 5.3.2 describes how to inject samples manually.
A 10 L PEEK sample loop (P/N 042949) is installed between ports L (1) and
L (4). Thermo Fisher Scientific offers sample loops in various sizes. If
needed, the pre-installed 10 L loop can be replaced with a loop that has a
different sample injection volume.

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2.13.3 10-Port Valve


The 10-port valve (P/N 061962) is an optional valve, available for various
applications. Figure 2-26 shows example flow schematics for the 10-port
valve when it is connected for an application that uses a concentrator column.

NOTE Other plumbing configurations for the 10-port valve are pos-
sible, depending on the components to be connected to the
valve and the application to be run. Refer to the appropriate
Application Note for more information.

LOAD POSITION INJECT POSITION


(Loop Loading) (Concentrator Loading)

Concentrator Concentrator
To Column To Column

6
Eluent 6
Eluent
Pump In Pump In
8 7 5 4 8 7 5 4
Large 9 3 Large 9 3
Loop 1 Loop 1
10 2 10 2
To Waste To Waste

Sample Sample
In Carrier In Carrier
To Waste Pump In To Waste Pump In

= Sample = Eluent = Carrier

Figure 2-26. Injection Valve Flow Schematics (10-Port Valve)


Example Connections: Large Loop to Concentrator

Liquid flows through either the Load or Inject path, depending on the valve
position. For the example shown in Figure 2-26, the flow occurs as follows:
• In the Load position, sample flows from the syringe or autosampler line,
through the valve, and into the sample loop. Excess sample flows out to
waste. Eluent flows from the eluent pump, through the valve, through the
concentrator column, and to the separator column. If sample was
previously loaded onto the concentrator column, it is swept to the
separator column for analysis.

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2 • DC Description

• In the Inject position, carrier liquid flows through the sample loop and on
to the concentrator column, carrying the contents of the sample loop with
it. Excess flows out to waste. Eluent flows from the pump, through the
valve, and to the separator column, bypassing the concentrator column.

2.14 CD Conductivity Detector


Each Dionex ICS-5000 Conductivity Detector (CD) consists of a heated
conductivity cell and the electronics required for collecting the conductivity
data and sending it to the computer and the analog output (if installed). The
CD is installed in the upper compartment of the DC (see Figure 2-21).
Two versions of CD are available:
• A capillary CD (P/N 072041), for use in systems running capillary flow
rates
• An analytical CD (P/N 061716), for use in systems running analytical
(standard bore or microbore) flow rates
The features and functions of the two CD versions are the same. However,
because the cell volumes of the two are different, the versions are not
interchangeable. The CD version must match the system type (capillary IC or
analytical IC). If the CD version and system type are mismatched,
chromatograms will be affected (for example, broad peaks or lowered
sensitivity).

2.14.1 Heated Conductivity Cell


The flow-through conductivity cell measures the electrical conductance of
analyte ions as they pass through the cell. Two passivated 316 stainless steel
electrodes are permanently sealed into the PEEK cell body. The cell design
provides efficient sweep-out, low volume (<1 L), and low dispersion.
Temperature control and compensation help ensure good peak reproducibility
and baseline stability.

Temperature Control

Temperature directly affects the conductivity of a solution. For example,


laboratory heating and air conditioning systems can cause a regular slow

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cycling in the baseline. This, in turn, can affect the reproducibility of an


analysis. The higher the conductivity, the more pronounced the effect.
To reduce the effect of temperature variation, the DC provides temperature
control of both the DC compartment and the cell. A heater inside the cell
regulates the cell temperature. The cell heater temperature range is from a low
of 5 °C above the temperature of the upper DC compartment to a high of
60 °C.

Temperature Compensation

Built-in temperature compensation helps minimize changes in the baseline or


in peak heights if the operating temperature is different from the temperature
at which the cell was calibrated. The default temperature compensation is
1.7% per °C. This can be reset to between 0% and 3.0% per °C, depending on
the eluent. If you notice that the baseline shifts up when the temperature
increases, the compensation factor is too low and should be reset to a higher
value.
To change the temperature compensation factor:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the conductivity detector.
4. Select the Temperature_Compensation property and enter the value.
5. For Chromeleon 6.8, click Execute.

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2 • DC Description

2.14.2 Suppressor
The suppressor reduces the eluent conductivity and enhances the conductivity
of the sample ions, thereby increasing detection sensitivity. Installation of a
suppressor is optional.
The capillary and analytical CDs can operate with the following suppressors:

CD Type Available Suppressors


Capillary CD Dionex ACES™ 300 (Capillary), Dionex
CCES™ 300 (Capillary)
Analytical CD Dionex AAES™, Dionex CAES™, Dionex
AMMS™ 300, Dionex CMMS™, Dionex
ASRS™ 300, Dionex CSRS™ 300

For details about any of the suppressors, including guidelines for selecting a
suppressor for your application, refer to the suppressor manuals. The manuals
are on the Thermo Scientific Reference Library DVD (P/N 053891).

Capillary Capillary IC Suppressor


IC
The suppressor for a capillary IC system is installed inside an IC Cube
capillary suppressor cartridge. For details about the IC Cube and the capillary
suppressor cartridge, see Section 2.11.2.

Analytical IC Suppressor

The analytical suppressor is installed on clips on the lower area of the


analytical CD (see Figure 2-27). The suppressor cable plugs into the
connector next to the detector.

Conductivity
1 Detector
3 1
Suppressor
2 (Optional)
(ASRS 300
2
model shown)

Suppressor
3
Cable

Figure 2-27. Analytical Conductivity Detector with Suppressor (System #1)

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NOTE It is also possible to control an analytical suppressor with a


Dionex ICS-5000 Electrochemical Detector (ED). Tabs for
installing the suppressor are provided on the front of the DC
(next to the ED). The cable connection is the same as for the
CD.

NOTE To prevent accumulation of oxygen or hydrogen gases, con-


nect a gas separator waste tube (P/N 045460) to the suppres-
sor waste line during installation For details, refer to Thermo
Scientific Dionex ICS-5000 Ion Chromatography System
Installation Instructions (Document No. 065343).

2.14.3 System Flow Schematics for Conductivity Detection


Figure 2-28 illustrates the flow path through a DC for a conductivity detection
application using suppression in recycle mode. For information about other
suppression modes, refer to the suppressor manuals. The manuals are on the
Thermo Scientific Reference Library DVD (P/N 053891).

NOTE The basic flow path is the same for both capillary IC and ana-
lytical IC systems. However, in capillary IC systems, connec-
tions to components installed inside IC Cube cartridges
(columns, suppressor, and CRD) are not visible.

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2 • DC Description

COND CELL For anion suppression


only (optional).
7
REGEN 10 9
CRD
OUT
6

8 SUPPRESSOR

SEPARATOR COLUMN

GUARD 4
SAMPLE

TEMP
= Eluent Flow STABILIZER
S L
= Regenerant Flow
4
5 For analytical
W C IC only
6 3 3

1 2
L P
2 PUMP or
WASTE VALVE 1 ELUENT
(Inject Position) ELUENT IN GENERATOR

Figure 2-28. DC Flow Schematic for Conductivity Detection


(Suppression in Recycle Mode)

• Eluent from the pump 1 flows into the injection valve 2 .


• After sample is loaded into the sample loop 3 and the injection valve is
toggled to the Inject position, eluent passes through the loop.
• The eluent/sample mixture is pumped first through a temperature
stabilizer (analytical IC only), through the guard and separator
columns 4 , and then through the suppressor 5 .
• From the suppressor, the mixture flows through a CRD 6 (if installed) to
the cell 7 , where the analytes are detected. A digital signal is sent to
Chromeleon.
• Finally, the mixture flows out of the cell and is recycled back into the
suppressor 8 , where it is used as the water source for the regenerant

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chamber. Flow is again routed through the CRD (if installed) 9 and then
to waste 10 .
Figure 2-29 illustrates the flow path through an EG and a DC for a
conductivity detection application using suppression in recycle mode.

DI WATER IN
FROM PUMP

1 7
9

EGC COND CELL For anion


6 suppression only
8 9
2
CRD 11
13 CR-TC
5
14 8
10
3 WASTE SUPPRESSOR
4 REGEN IN
EG
12 7
DEGAS

SEPARATOR COLUMN

GUARD 6
SAMPLE 3

2 1 TEMP
= Eluent Flow VALVE STABILIZER
S L
= Regenerant Flow
4
5
W C For analytical
6 5 3
IC only.
1 2 4P
L ELUENT IN
WASTE (Inject Position)

Figure 2-29. EG and DC Flow Schematic for Conductivity Detection


(Suppression in Recycle Mode)

• Deionized water from the pump 1 enters the EGC, which generates the
eluent. Eluent exits the EGC and passes through the CR-TC 2 (which
traps ionic contaminants), through the EG degas tubing, 3 and then into
the injection valve 4 .
• After sample is loaded into the sample loop 5 and the injection valve is
toggled to the Inject position, eluent passes through the loop.

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2 • DC Description

• The eluent/sample mixture is pumped through a temperature stabilizer


(analytical IC only), through the guard and separator columns 6 , and
then through the suppressor 7 .
• From the suppressor, the mixture flows through a CRD 8 (if installed) to
the cell 9 , where the analytes are detected. A digital signal is sent to
Chromeleon software.
• The mixture flows out of the cell and is recycled back into the
suppressor 10 , where it is used as the water source for the regenerant
chamber. Regenerant flow is routed through the CRD 11 (if installed),
through the EG degas tubing 12 , through the CR-TC 13 , and then out to
waste 14 .

2.15 ED Electrochemical Detector


One or two Dionex ICS-5000 Electrochemical Detectors (EDs) can be
installed in the DC. Each complete ED assembly consists of an amperometric
detection cell and the detector electronics required to collect data and send it
to the computer and the analog output (if installed). The detector is installed in
the upper compartment of the DC (see Figure 2-21). The cell mounts on the
front of the detector. The detector electronics are not accessible to the user.
The ED can perform the following electrochemical detection modes:
• DC amperometry (see Section 2.19.1)
• Integrated amperometry—includes pulsed amperometric detection (PAD)
and integrated pulsed amperometric detection (IPAD) (see Section 2.19.2)
• Cyclic voltammetry (see Section 2.19.3)

2.15.1 Electrochemical Detector Cell


The ED cell includes three different electrodes. It is a miniature flow-through
amperometric detection cell with a titanium cell body (the counter electrode),
a working electrode, and a combination pH-Ag/AgCl reference electrode (see
Figure 2-30) or a PdH reference electrode. The type of working electrode
used depends on the application. Four conventional (non-disposable) working
electrode types are available: gold, platinum, silver, and glassy carbon. Five
disposable working electrode types are available: gold on two different
substrates (polyester or PTFE), silver, platinum, and carbon.

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The ED cell can be used in either capillary IC or analytical IC systems. When


used in a capillary IC system, the inlet tubing is made of PEEK. When used in
an analytical IC system, the inlet tubing is made of titanium (see Figure 2-30).

Working
1 Electrode

Cell Body
3 2 (counter
2 electrode)
1
4 pH-Ag/AgCl
3 Reference
Electrode
Titanium Inlet
4 Tubing (for
analytical IC)

Figure 2-30. ED Cell with pH-Ag/AgCl Reference Electrode


(Cell Configured for Analytical IC Shown)

Cell Design

The ED cell is a thin-layer design. Eluent flows in a thin channel parallel to


the surface of a flat disk electrode. The resulting smooth flow minimizes
noise. The low volume (<0.2 L) of the channel also allows operation with
high efficiency, narrow bore columns, and capillary columns. The cell design
minimizes the electrical resistance between the working electrode and the
counter electrode by positioning the counter electrode (the cell body) directly
across the thin-layer channel from the working electrode. This results in a
wide linear dynamic range. The inlet tubing is in electrical contact with the
counter electrode and through it to ground. The working electrode current is
processed using low noise analog amplifiers and filters.

ED Cell Solvent Compatibility

The ED cell can be used with common reversed-phase solvents such as


methanol and acetonitrile. If a disposable working electrode on polyester
substrate is used, the percentage of methanol should not exceed 30% and the
percentage of acetonitrile should not exceed 10%. In addition, prolonged
exposure (more than 8 hours) of disposable gold electrodes on polyester
substrate to eluents containing hydroxide concentrations greater than 100 mM
is not recommended. Shorter rinse periods of 10 to 20 minutes (for example,

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2 • DC Description

the carbonate removal step during monosaccharide and disaccharide


chromatography) at high hydroxide concentrations do not affect the electrode
performance. If sustained highly alkaline eluent conditions are required, use a
disposable gold electrode on a PTFE substrate or a conventional gold
electrode. Refer to the disposable electrode manual (Document No. 065040)
for additional eluent compatibility information.
Because conventional working electrode blocks are made of Kel-F® and use a
gasket made of Ultem®, there is no restriction on the concentration of organic
solvents that can be used with them (providing the solvent is compatible with
PEEK tubing).
There is also no restriction on the use of organic solvents when disposable
gold electrodes on PTFE substrate and PTFE gaskets are used.

2.15.2 Combination pH–Ag/AgCl Reference Electrode


The pH-Ag/AgCl reference electrode is a standard combination pH electrode
containing a glass membrane pH half-cell and a Ag/AgCl half-cell. The
combination pH electrode monitors eluent pH.
The Ag/AgCl half-cell is typically used as the cell reference electrode. To
minimize changes in the baseline, the combination pH–Ag/AgCl electrode
can be used as the reference electrode during a pH gradient.

pH Dependence

The potentials at which many redox reactions take place on metallic


electrodes are pH-dependent, with the potential shifting -0.059 V per pH unit.
This is especially true for metal oxide formation, oxidation, and oxidative
desorption. Since the reference potential of the combination pH–Ag/AgCl
electrode also shifts by -0.059 V per pH unit, pH-dependent potential shifts at
the working electrode are canceled.

Correcting for pH Dependence

At an eluent pH of 7, the reference potential of the entire electrode is the same


as that of the Ag/AgCl half-cell. As the eluent pH is increased, the pH half-
cell potential decreases approximately 0.059 V per pH unit. For example, at
an eluent pH of 12, the reference potential of the pH half-cell would be -
0.295 V relative to the Ag/AgCl half-cell. Therefore, at pH 12, the potentials

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applied to the working electrode must be raised approximately 0.3 V when


switching from the “Ag” reference to the “pH” reference.
In acidic eluents, the reference potential of the pH half-cell is positive with
respect to the Ag/AgCl half-cell, and all applied potentials must be decreased
by 0.059 V per pH unit when switching from the “Ag” reference to the “pH”
reference.
Do not allow the pH-Ag/AgCl reference electrode to dry out. Make sure
that eluent is being pumped continuously through the cell at a low flow
rate (for example, 0.05 mL/min). If the cell will not be used for a short
time (less than 2 days), disconnect the tubing from the inlet and outlet
fittings and install fitting plugs. For longer shutdowns, remove the elec-
trode from the cell and store it in its storage cap filled with saturated
KCl solution. See Section 6.4 for detailed storage instructions.

Monitoring the ED Cell pH Readout

Monitoring the pH readout of a solution with a known composition lets you


detect any reference potential shift that may occur over time. This allows you
to determine when the pH-Ag/AgCl reference electrode needs regenerating or
replacing, thus improving the reproducibility of your analyses. For
instructions on how to monitor the pH readout, see Section 4.1.2.

NOTE Monitor the pH when the pH-Ag/AgCl reference electrode is


used in the Ag mode as well as in the pH mode.

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2.15.3 Palladium Hydrogen (PdH) Reference Electrode


The PdH reference electrode consists of palladium and platinum electrodes
immersed in an aqueous solution. With a potential applied between the two
electrodes, palladium is connected as a cathode and platinum as an anode. As
a consequence of the applied potential, hydrogen gas is generated at the
palladium electrode and oxygen gas at the platinum electrode. Whereas the
oxygen gas is swept out of the cell in the liquid stream, a portion of the
hydrogen gas is taken up by palladium metal. An equilibrium develops
between molecular hydrogen in the liquid phase and the adsorbed hydrogen in
palladium. The palladium hydrogen electrode becomes a reference electrode
with a half reaction of:
H+ + e- = ½ H2
Where the hydrogen is supplied by the following process:
Pd + ½ H2  Pd-Hads  Pd-Habs
The PdH reference electrode is thus similar to the standard hydrogen
electrode, which is based on the same half reaction between the hydronium
ions and molecular hydrogen. However, there are also some differences. For
example, palladium is not as good a catalyst for the electrode half reaction as
platinum. As a consequence, under identical conditions, the reference
potential of the palladium hydrogen electrode differs from that of the standard
hydrogen electrode by a constant potential. In addition, because hydronium
ions are involved in the reference half reaction, the potential of the PdH
electrode is pH dependent.

Waveforms for PdH Reference Electrodes in Chromeleon

When you create or edit an instrument method in Chromeleon 7 or a program


in Chromeleon 6.8, you can select a waveform created for use with the PdH
reference electrode. To use a waveform that was created for a pH-Ag/AgCl
electrode, select the waveform and then manually correct the potential values
in the Waveform Editor. The formula for correction is provided in the
Waveform Editor.

No pH Readout with the PdH Reference Mode

If the PdH electrode were connected to another reference electrode (for


example, a Ag/AgCl electrode), the PdH electrode could serve as a pH
indicator electrode. However, when the PdH electrode functions as a

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reference electrode, it cannot indicate pH. In the same manner, a glass


electrode alone cannot measure pH; it must be used with a suitable reference
electrode.
The pH readout of the ED cell is disabled when the PdH reference mode is
selected.

2.16 DC Rear Panel


Figure 2-31 illustrates the rear panel of the DC.

1 Tubing Chase (2)

2 Switched AC Sockets

Fuse Holder, Main


3 Power Switch, and
Power Receptacle

1 1 External Low Pressure


4
8
Valve Mounting Slots
5 USB Receptacle
5 (“B” Connector)
6
2
4 USB Ports (2)
6
(“A” Connectors)
7
3 External Low Pressure
7 Valve Connectors
9 Analog Output and
9
8 TTL/Relay Connectors
(optional)
9 Drain Port

Figure 2-31. DC Rear Panel

Tubing Chases

The tubing chases route tubing from the front compartment, through the DC
interior, and to the rear panel. Foam inserts insulate the chases.

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Switched AC Sockets

The two AC receptacles can be used to control the power to external devices.
Use Chromeleon to switch the power on and off. TTL inputs can also be used
to control the AC sockets (see Section 2.17.4).

Fuse Holder, Main Power Switch, and Power Receptacle

The fuse holder contains two 10-amp slow-blow fuses (P/N 954772). For
instructions on how to change the fuses, see Section 9.22.
The rear panel power switch is the main power switch for the DC. Turn on the
main power switch before initial operation and leave the switch on unless
instructed to turn it off (for example, before performing a service procedure).

NOTE For routine on/off control, use the POWER button on the front
of the DC (see Figure 2-16). To turn off the DC, press and
hold the POWER button for 2 seconds.

The power cord plugs into the IEC 320 three-prong receptacle.

The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the DC and is easily accessible.

Le cordon d'alimentation principal est utilisé comme dispositif principal


de débranchement. Veillez à ce que la prise de base soit située/installée
près du module et facilement accessible.

Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen


Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht
zugänglich ist.

USB Connections

The USB (Universal Serial Bus) receptacle (“B” type connector) allows
connection to the PC on which Chromeleon software is installed.
The two USB ports (“A” type connectors) allows connection to other USB
devices in the system (for example, the pump and eluent generator).
A 1.8 m (6 ft) USB cable (P/N 960777) is included in the DC Ship Kit
(P/N 072011).

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External Low Pressure Valve Outputs

Six outputs allow connection to externally-installed low-pressure (solenoid)


valves. Low-pressure valves can be used for on/off control of liquid flow (for
example, to turn flow on and off from a reagent reservoir). You control the
outputs with Chromeleon.
Two low-pressure valves can be installed on a regulator stand and four valves
can be installed on the rear of the DC.

Analog Output, TTL, and Relay Connectors (Optional)

If the I/O option (P/N 062201) is installed, the following connections are
provided:
• Two analog outputs (one for each detector)
• One +5V power output
• Two relay outputs
• Two TTL outputs
• Eight programmable TTL inputs
See Section 2.17 for details about the I/O option.

Drain Port

The drain port removes any liquid that collects in the drip tray in the bottom
of the DC. A clear corrugated drain hose (P/N 055075) is connected to this
port during installation. Place the drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
DC.
For correct drainage, make sure the drain hose is not bent, pinched, or
elevated at any point. Do not allow the end of the hose to be submerged
in waste liquid.

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2.17 I/O Option


When the I/O option (P/N 062201) is installed, two 12-pin connector strips
are on the DC rear panel. Figure 2-32 describes the functions assigned to each
connector pin.

Figure 2-32. Optional Rear Panel I/O Connector Strips

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2.17.1 I/O Option Connections


1. Locate the twisted pair of
wires (P/N 043598) and 12- Position 1
position connector plugs
Locking
(P/N 923686) (see Screws
Figure 2-33) provided with the
I/O option board. Position 12

Figure 2-33. 12-Position Connector Plug

2. For each I/O function to be used, connect an active wire (red) and a
ground wire (black) to the 12-position connector plug at the appropriate
pin locations. Refer to Figure 2-32 or the label on the DC rear panel for
the connector pin assignments.
To attach a wire to the plug, strip the end of the wire, insert it into the
plug, and use a screwdriver to tighten the locking screw. If necessary,
multiple ground wires can be attached to a single ground pin.

When attaching wires to the connector plug, be careful not to allow


stray strands of wire to short to an adjoining position on the connector.

3. Plug the connector into the appropriate 12-pin connector on the DC rear
panel.
4. Connect the wires from the DC connector plug to the appropriate
connector pins on the other modules. Additional connector plugs are
provided with other Dionex modules.

NOTE Check the polarity of each connection. Connect signal


wires to signal (+) pins and ground wires to ground (-)
pins.

5. If you connected a TTL input, verify that the correct function is assigned
to the input and that the correct input control type is selected. Select
different settings if necessary. Input functions and control types are
assigned from the Chromeleon 7 Instrument Configuration program or the
Chromeleon 6.8 Server Configuration program (see Section 2.17.4).

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2.17.2 Analog Outputs


When the I/O option is installed, two analog outputs (one for each detector)
are installed on the DC rear panel (see Figure 2-31). The analog outputs
supply a voltage signal proportional to the current measured by the detector
cell. The outputs can be connected to an analog-to-digital (A/D) converter
such as an integrator or other recording device. Refer to Section 2.17.1 and
the documentation for the device for connection instructions.
Several settings are available that allow you to configure the analog output
signal for your detector and connected device. Table 2-4 describes the
settings. You select the preferred settings on the detector panel on the
Chromeleon 7 ePanel Set (see Figure 2-34) or Chromeleon 6.8 panel tabset.

Analog Output Values Description


Setting
Full-scale voltage 0.01, 0.10, or 1.00 V Sets the voltage output of a full-
scale detector response. The
voltage to use depends on the
recording device to which the
analog output is connected. For
example, if the analog output is
connected to a device that
accepts input voltages up to 1 V,
select a full-scale voltage output
of 1 V.
Range Conductivity: Sets the full-scale detector
0.01 to 15,000 S response value. The range to use
DC Amperometry: depends on the detector readings
50 pA to 300 A expected for the application. For
Integrated example, selecting a range of
Amperometry: 20 micro Siemens (S) will limit
50 pC to 200 C you to viewing conductivity
readings of 20 S or less.

Table 2-4. Analog Output Configuration Settings

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Analog Output Values Description


Setting
Recorder Zero, Full Scale, Use this setting to calibrate a
calibration Normal recording device. Select Zero to
set the output signal to zero volts.
Select Full Scale to set the
output signal to the selected full-
scale voltage (0.01, 0.10, or
1.00 V). For normal operation,
select Normal (the default) to
output a signal corresponding to
the detector output.
Offset level 0 to 100% Use this setting to adjust the zero
position of the analog output
when it is plotted. The value
entered is a percentage of the
full-scale analog output. An offset
allows a recording device to plot
the signal if it becomes negative.
The offset level does not affect
the magnitude of the output
signal.
Polarity Positive, Negative Use this setting to set the polarity
of the analog output signal to
either positive (the default) or
negative. In applications in which
the analyte output is lower than
the background signal, the
polarity must be negative to
display peaks instead of dips on
the chromatogram.
Mark 10% of the full-scale Use this setting to send a positive
analog output pulse to the analog output as an
event marker. A mark is typically
used to indicate a sample
injection.

Table 2-4. Analog Output Configuration Settings (Continued)

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2 • DC Description

Figure 2-34. Conductivity Detector Control Panel


(Chromeleon 7 Version Shown)

2.17.3 Power, Relay, and TTL Outputs


The power, relays, and TTL outputs can be used to control functions in
external devices such as an autosampler or another Dionex module.
Depending on which pins are connected, the relay connection can be either
normally open (N.O.) or normally closed (N.C.) (see Figure 2-35). Choose
N.O. or N.C. based on what you want the state of the connected device to be
when the DC power is turned off. A normally open relay is open when the
relay is switched off and closed when the relay is turned on. A normally
closed relay is closed when the relay is off and is open when the relay is on.

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The relays can be programmed to switch any low-voltage device. Switched


current must be no more than 2 A at 24 VDC. Refer to Section 2.17.1 and the
documentation for the external device for connection instructions.

RELAY OUTPUT CONFIGURATION NOTES

Rear Panel Relay Output The relays are capable of


Pins (on DC Electronics) switching 2 A at 24 VDC.
N.O.
For a normally open
COM connection, connect a
N.C. COM pin and an N.O. pin.
Non-Energized Relay
For a normally closed
connection, connect a
N.O. COM pin and an N.C. pin.
COM
N.C.
Energized Relay

Figure 2-35. Relay Output Configuration

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You can control the power, relays, and TTL outputs from the DC ePanel in
Chromeleon 7 (see Figure 2-36) or the DC Control panel in Chromeleon 6.8.

Figure 2-36. Output Relays and TTL Control on DC ePanel in Chromeleon 7

NOTE It is possible to change the settings for the power, relays, and
TTL outputs while a Chromeleon 7 instrument method or
Chromeleon 6.8 program is running.

2.17.4 TTL Inputs


When connected to a controlling device, the TTL inputs can be programmed
to perform the following DC functions:
• Injection valves left and right (load/inject)
• AM high-pressure valves A and B (A/B)
• AM low-pressure valves A and B (open/closed)
• DC low-pressure valves A through F on the rear panel (open/closed)

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• ED detectors 1 and 2 (on/off)


• CD/ED detectors 1 and 2 auto-offset
• CD/ED detectors 1 and 2 mark
• Suppressors 1 and 2 (on/off)
• Reaction coil heater (on/off)
• A/C relays 1 and 2 (open/closed)

Assigning TTL Input Functions

TTL input control functions are assigned in the Chromeleon 7 Instrument


Configuration program or the Chromeleon 6.8 Server Configuration program.
You can assign one or more functions to each input.

NOTE If two timebases are sharing the DC, the TTL input functions
are shared between the timebases. For example, if TTL input
1 is assigned to control injection valve 1, that function is
assigned to both timebases. You do not need to associate a
TTL input with a particular timebase.

To select TTL input control functions:


1. Open the Chromeleon 7 Instrument Configuration program or
Chromeleon 6.8 Server Configuration program.
2. Double-click the DC icon under the instrument or timebase.

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2 • DC Description

3. Select the TTL Inputs tab (see Figure 2-37).

Figure 2-37. DC Server Configuration Properties: TTL Inputs

4. Select the name of the input and press the F2 key (or double-click the
name).

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The Device Configuration dialog box for the selected input appears.

Figure 2-38. Assign TTL Input Control Functions

5. In the Control Functions list, select the check box of one or more
functions to be controlled by this input. When connected to a controlling
device, the device can send a signal to the input to trigger the selected
functions.
6. By default, several functions are selected. Scroll down the list and disable
all unwanted functions.

TTL Input Control Types

The DC TTL inputs respond to four types of signals


to accommodate different controlling devices. The
default control type, Normal Edge, is compatible
with the output signals provided by Dionex
modules.
If the device connected to the DC does not send a normal edge signal, select
the appropriate control type. Refer to the documentation provided with the

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2 • DC Description

controlling device and the information below to determine the correct type.
Select the input control type in the Device Configuration dialog box for each
TTL input (see Figure 2-38).
• Normal Edge: In normal edge Action Off or No Effect
operation, the negative (falling)
TTL +5 V
edge of a signal turns on the NORMAL
function. EDGE
+0 V

The action of the positive (rising) Action On


edge depends on the function: For on/off or other functions that have two
options, the rising edge turns off the function. However, for functions with
only one option, the rising edge has no effect.
For example, for the injection valve position, the falling edge switches the
valve to Load and the rising edge switches the valve to Inject. Similarly,
for the detector start/stop, the falling edge starts the detector and the rising
edge stops it. For the detector mark and offset functions, the falling edge
turns on the function and the rising edge has no effect.
• Inverted Edge: The inverted edge Action On
mode works identically to the
TTL +5 V
normal edge mode except that the INVERTED
positive and negative edges are EDGE
+0 V
reversed in function. Action Off or No Effect

• Normal Pulse: In normal pulse


operation, the negative (falling) TTL +5 V
NORMAL
edge of the TTL signal is the active PULSE +0 V
edge and the positive (rising) edge
Action On Action Off
is ignored.
A pulse width of 50 ms or more is guaranteed to be detected. A pulse
width of 4 ms or less is guaranteed to be ignored. The action for pulse
widths that are greater than 4 ms and less than 50 ms is undefined.
• Inverted Pulse: The inverted pulse
Action On Action Off
mode operates identically to the
normal pulse mode except that the TTL +5 V
INVERTED
positive and negative edges are PULSE +0 V
reversed in function.

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2.18 Automation Manager


The Dionex ICS-5000 Automation Manager (AM) provides a mounting
location for various components used for performing matrix elimination, large
volume pre-concentration, post-column reagent addition, and other functions.
Each AM consists of a tray on which valves and other components are
installed (see Figure 2-39). The tray is installed in the upper compartment of
the DC (see Figure 2-21). Connections to other components in the system
(pump, injection valve, reagent reservoirs, etc.) depend on the application.
Refer to Chapter 3 for the configuration schematic for your application.

Low-Pressure Low-Pressure Temperature


Valve #1 Valve #2 Stabilizer

RCH-1
Reaction Coil

High-Pressure High-Pressure
Valve #1 Valve #2

Figure 2-39. Dionex ICS-5000 Automation Manager

NOTE Because the AM requires the full width of the DC upper com-
partment, an IC Cube cannot be installed in the DC when an
AM is installed.e AM is available in the following configura-
tions:

Components Included Part Number


Two 10-port high-pressure valves 061738
Two low-pressure 3-way valves
One 10-port high-pressure valve 061736
One low-pressure 3-way valve

Figure 2-40. AM Configurations

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2 • DC Description

Components Included Part Number


One 6-port high-pressure valve 061740
One low-pressure 3-way valve
AutoPrep configuration: 066343
10-port high-pressure valve
AutoPrep sample loop
AutoPrep standard loops
AM tray with no valves 061734

Figure 2-40. AM Configurations (Continued)

In addition to the configurations described above, you can order the following
components separately for installation on an AM:

AM Component Part Number


High-pressure valve, 6-port 061961
High-pressure valve, 10-port 061962
Low-pressure valve, 3-way 061971
Low-pressure valve, 2-way 061745
RCH-1 Reaction Coil Heater 061746
Temperature stabilizer, standard bore, 0.25 mm 062561
(0.010 in) ID
Temperature stabilizer, microbore, 0.125 mm 062562
(0.005 in) ID

Figure 2-41. AM Components Available Separately

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2.18.1 AM High-Pressure Switching Valves


Up to two high-pressure switching valves can be installed on an AM. Two
models are available: 6-port (P/N 061961) and 10-port (P/N 061962). Both
models are electrically-activated, two-position valves. Figure 2-42 and
Figure 2-43 show the liquid flow path through the valve ports at each valve
position.

POSITION A POSITION B
5 4 5 4

6 3 6 3

1 2 1 2

Figure 2-42. High-Pressure Switching Valve Flow Schematics:


6-Port Valve

POSITION A POSITION B
6 6

5 7
8 7 4 8 5 4
3 9
9 3
1 1
10 2 10 2

Figure 2-43. High-Pressure Switching Valve Flow Schematics:


10-Port Valve

Valve port connections to chromatography components vary, depending on


the application. Refer to Chapter 3 for the configuration schematic for your
application.
Valves are controlled by Chromeleon (see Section 2.18.3).

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2 • DC Description

2.18.2 AM Low-Pressure Valves


Up to two low-pressure valves can be mounted on an AM. The valves are
either two-way or three-way valves. The two-way valves provide on/off
control of liquid flow in one direction, while the three-way valves provide
on/off control in two directions (see Figure 2-44).

OFF POSITION ON POSITION

Note:
0 0 When the valve is
off (i.e., it is not
COM (N.O.) COM (N.O.)
energized), port 0 is
open (N.O.) and port
1 1 1 is closed (N.C.).
(N.C.) (N.C.) Conversely, when
the valve is on, port
1 is open and port 0
N.C. = normally closed
is closed.
N.O. = normally open
COM = common flow

Figure 2-44. Three-Way Low-Pressure Valve Flow Schematics

Valve port connections to chromatography components vary, depending on


the application. Refer to Chapter 3 for the system flow schematic for your
application.
Valves are controlled by Chromeleon (see Section 2.18.3).

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2.18.3 AM High- and Low-Pressure Valve Control


Chromeleon is used to control the high- and low-pressure valves. For
automated control, commands for valve control can be included in a
Chromeleon 7 instrument method or a Chromeleon 6.8 program. To add AM
valve control commands to a Chromeleon 7 instrument method, use the
Script Editor (see Figure 2-45).

Figure 2-45. Chromeleon 7 Script Editor

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To add AM valve control commands to a Chromeleon 6.8 program, use the


Relay and State Devices Options page in the Program Wizard (see
Figure 2-46).

Figure 2-46. Chromeleon 6.8 Program Wizard Relay and State


Devices Options Page

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For manual control of AM valves, execute commands from the DC ePanel in


Chromeleon 7 (see Figure 2-47) or the DC Control panel in Chromeleon 6.8.

Figure 2-47. Valve Control on DC ePanel in Chromeleon 7

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2.18.4 RCH-1 Reaction Coil Heater


The RCH-1 Reaction Coil Heater (P/N 061746) can hold up to two reaction
coils. The heater has an operating temperature range of from 5 °C above the
temperature of the upper compartment up to 80 °C.
For automated control of the heater, commands can be included in a
Chromeleon 7 instrument method (see Figure 2-48) or Chromeleon 6.8
program.

Figure 2-48. Instrument Wizard DC Options Page in Chromeleon 7

For direct control of the heater, use the controls on the DC ePanel in
Chromeleon 7 or the Control panel in Chromeleon 6.8.

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2.19 Electrochemical Detection Modes


The Dionex ICS-5000 Electrochemical Detector can perform the following
electrochemical detection modes:
• DC amperometry (see Section 2.19.1)
• Integrated amperometry—includes pulsed amperometric detection (PAD)
and integrated pulsed amperometric detection (IPAD) (see Section 2.19.2)
• Cyclic voltammetry (see Section 2.19.3)

2.19.1 DC Amperometric Detection


In DC amperometry, a constant potential is applied to the working electrode.
The potential can be entered into a Chromeleon 7 instrument method (see
Figure 2-49) or Chromeleon 6.8 program.

Figure 2-49. DC Amperometry Instrument Method Wizard Page


in Chromeleon 7

The applied voltage can be changed up to 10 times during the run. The actual
number of potential changes allowed depends on the available data storage

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2 • DC Description

capacity, which is determined by the length of the run and the data sampling
rate.
For direct control, enter the potentials on the DC ePanel in Chromeleon 7 or
the Control panel in Chromeleon 6.8.

2.19.2 Integrated and Pulsed Amperometric Detection


Integrated and pulsed amperometric detection are similar to DC amperometry
(see Section 2.19.1) in that molecules are oxidized or reduced at the surface of
an electrode. However, with these detection modes, a series of potential
changes is repeated over time. By repeatedly pulsing between optimized high
positive and negative potentials, the electrode surface is continually
regenerated. Current is measured by integration during a portion of the
repeating potential vs. time waveform. See Section 2.19.4 for more
information about waveforms.

Pulsed Amperometric Detection

In pulsed amperometric detection (PAD), current is integrated at a single


constant potential (see Figure 2-50).

t2
+0.7

Delay Integration

Potential
(Volts)

+0.1
t1
-0.1
t3
E1. Detection Potential
E2. Positive Cleaning
0.0 0.2 0.4 0.6 Potential
Time (Seconds) E3. Negative Cleaning
E1 E2 E3 Potential

Figure 2-50. Example Pulsed Amperometry Waveform

The potentials, labeled E1, E2, and E3, are applied for durations t1, t2, and t3,
respectively. At t1, the E1 potential is applied. After a delay, the signal is

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measured by integrating the current for a fixed time. Current integrated for a
fixed time is charge and the units are coulombs. At t2 and t3, positive and
negative cleaning pulses are added to the waveform. This waveform period
repeats until the end of data acquisition or until another waveform is
specified.

Integrated Pulsed Amperometric Detection

With integrated pulsed amperometric detection (IPAD), current is integrated


at two or more potentials (see Figure 2-51).

+0.60

+0.35
Potential
(Volts)
-0.10

-0.60 Integration

0.0 0.2 0.4 0.6 0.8


Time (Seconds) E1, E2. Detection Potentials
E3. Positive Cleaning Potential
E1, E2 E3 E4 E4. Negative Cleaning Potential

Figure 2-51. Example Integrated Amperometry Waveform

With the example waveform shown in Figure 2-51, the current is integrated
both while the potential is swept across the metal oxide formation wave and
also during the reverse sweep across the oxide reduction wave. This technique
minimizes baseline shift and the peak dips that can occur when an eluting
analyte’s effect on oxide suppression is greater than the detector response
from the analyte.
As with pulsed amperometric detection, the waveform period repeats until the
end of data acquisition or until another waveform is specified.

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2.19.3 Cyclic Voltammetry


The determination of the optimum potentials to use in amperometry begins
with an electrochemical technique called voltammetry, in which the current
that results from oxidation or reduction reactions is measured against the
voltage applied to the system. The applied voltage is changed (scanned)
within preset limits.
Chromeleon 6.8 supports cyclic voltammetry. In cyclic voltammetry, the
voltage is first scanned in one direction and then reversed so that the voltage
at the end of the scan is the same as at the beginning. This results in a
triangular waveform (see Section 2.19.4).
In the cyclic voltammetry mode, the detector measures the current at a rate of
1 kHz (i.e., 1000 raw data points per second are collected). The data is
compressed before storage to 20 Hz.

2.19.4 Waveforms
A waveform is a series of steps, defined as points on a plot of potential vs.
time. Waveforms must be defined for the cyclic voltammetry and integrated
amperometry modes.

Cyclic Voltammetry Waveforms

Cyclic voltammetry waveforms are defined by three points, each with a time
and a potential. The waveform forms a triangle, with the first point always at
time zero and the first and third points always having the same potential.

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Figure 2-52 shows an example of a triangular waveform used in cyclic


voltammetry.

0.60 (14.0, 0.60)

0.40

0.20

0.00
Volts 0.00 5.00 10.00 15.00 20.00 25.00 30.00
-0.20

-0.40

-0.60

-0.80 (0.00, -0.80 (28.0, -0.80)


Seconds

Figure 2-52. Example Cyclic Voltammetry Waveforms

In this example, the potential is scanned from -0.80 to +0.60 V and then from
+0.60 to -0.80 V. The total time for one waveform period is 28 s. This
provides a sweep rate of 0.1 V/s as shown in the equation below.

2  V - = Sweep Rate
-----------------------------------
CV Cycle Time

 1.4 V = 0.1 V
2-------------------- ---
28s s

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Cyclic voltammetry waveforms are defined manually on the Chromeleon 6.8


electrochemical detector Control panel. Click the CV Mode button to display
the following window.

Figure 2-53. Cyclic Voltammetry Control Panel

Integrated Amperometry Waveforms

Integrated amperometry waveforms are included in an instrument method in


Chromeleon 7 or a program in Chromeleon 6.8. Integrated amperometry
waveforms have the following characteristics:
• The duration of one waveform period can be between 0.05 and 2.0 s, with
a step resolution of 10 ms. A waveform can have no more than 100 steps.
• The maximum waveform period is 2.0 s. However, for 2D data, because
only one data point is generated per waveform period, the effective
maximum length of a waveform period depends on the data collection
rate (the rate at which Chromeleon collects digital data points from the
detector). The relationship is as follows:

Data Collection Rate = 1/Waveform Period


• Multiple waveforms can be defined for a single run, provided they all
have the same cycle duration. Up to 15 waveform changes per run are
allowed.
• Each waveform can have only one integration interval. However, 3D
amperometric data can be reprocessed after the run with integration
intervals at multiple points in the waveform (see Section 2.19.5).
• The integration interval generates one integrated data point per waveform.

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Chromeleon provides several pre-programmed waveforms.


You can use a pre-programmed waveform, without modification, or modify it
for your application. You can also define a new waveform. Waveforms are
defined and modified in the Waveform Editor (see Figure 2-54).

Figure 2-54. Waveform Editor in Chromeleon 7

To view the Waveform Editor, click Edit on the ED Options page in the
Instrument Method Wizard (Chromeleon 7) or Program Wizard (Chromeleon
6.8).

Analytical vs. Scanning Waveforms

The pre-programmed analytical waveforms supplied with Chromeleon are


designed for quantitative analysis of specific compounds (alcohols, amino
acids, carbohydrates, etc.). With analytical waveforms, integration occurs
either while a single constant potential is being applied over time (see the
example waveform in Figure 2-50) or while a series of stepped potentials is
being applied (see the example waveform in Figure 2-51).

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2 • DC Description

With scanning waveforms, integration occurs while the potential is being


increased linearly over time (see the example scanning waveform in
Figure 2-55). Although scanning waveforms are typically not as useful for
quantitative analysis as analytical waveforms, when used to collect 3D
amperometric data, scanning waveforms can be optimized to provide
characteristic I-t plots (see Section 2.19.5). Comparison of I-t plots of a
known substance with an unknown can help to identify unknown peaks or to
determine whether a substance is coeluting with another.

E4
1.0

E2
0.0
Potential
(Volts) E1 E1
-1.0 Integration E3

-2.5
0.0 0.5 1.0 1.5 2.0
Time (Seconds)

E1. Pre-adsorption potential


E2. Scanning period
E3. Negative cleaning potential
E4. Positive cleaning potential

Figure 2-55. Example Scanning Waveform

2.19.5 Storing and Reprocessing Amperometry Data


Chromeleon provides storage of 2D and 3D pulsed amperometry and
integrated amperometry data. For 2D data, Chromeleon stores the detector’s
response at each waveform period’s integration interval. One integrated data
point per waveform period is stored. This allows you to produce a
chromatogram similar to the example shown in Figure 2-56. The retention

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time (in minutes) is on the x-axis and the detector response (in
nanoCoulombs) is on the y-axis.

Analytical Column: CarboPac PA10


(4 x 250 mm) and Guard
Eluent: 18 mM NaOH
Flow Rate: 1.5 mL/min
Detection: Pulsed Amperometry
Electrode: Gold
40 Waveform: Quadruple Potential
2
Peaks: 1. L-Fucose
1 2. D-Galactosamine
3. D-Glucosamine
3 4. D-Galactose
5 5. D-Glucose
Response 4 6. D-Mannose
(nC)
6

0 5 10
Retention Time (Minutes)
Minutes

Figure 2-56. Example Chromatogram for a Pulsed Amperometry Application

For 3D amperometry data, Chromeleon stores raw data points at a rate of


1 KHz throughout the entire run. Each raw 3D data point is defined by the
following attributes: the detector current (1) recorded at a particular
waveform time (2) and at a specific retention time (3). As a result, the two-
dimensional view of an integrated amperometry chromatogram (retention
time vs. integrated current) is extended by a third dimension (waveform time).
Thus, data for the entire waveform period—not just the integration
intervals—are collected.

Displaying and Reprocessing 3D Data

This section describes how to display and reprocess 3D amperometry data


using Chromeleon 6.8. If you are using Chromeleon 7, the features described
here are available by displaying the data in a contour plot. For details, refer to
the Chromeleon 7 Help.
In Chromeleon 6.8 you can display and reprocess 3D amperometry data in the
3D Amperometry View window (see Figure 2-57). To open the window,

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2 • DC Description

double-click the sample in the Browser to open the chromatogram. On the


View menu, click 3D-Amperometry.

Sample Chromatogram
Injection Data Plot*

I-t Plot
3D Amperometry
(current vs.
Data Plot
waveform
time)

Waveform
Plot

Figure 2-57. 3D Amperometry View Window in Chromeleon 6.8

*The chromatogram plot shown in Figure 2-57 was obtained by plotting


integrated current (charge, nC) vs. retention time.
The window is divided into several display areas:

Sample injection data Displays information about the sample.


Chromatogram plot Displays a chromatogram of data selected
from the selected integration interval in
the 3D amperometry data plot.
3D amperometry data plot Displays the raw 3D amperometry data.
Waveform/I-t plot Displays an I-t plot (current vs. waveform
time) of selected data and optionally a
waveform plot.

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In Chromeleon 6.8, the raw 3D amperometry data plot can be viewed as either
an Iso or a 3D (wireframe) plot. For both plot types, colors are used to
represent the ranges of response values.
The Iso view is the default view for the 3D raw data. This is a top down view
of the data (imagine you are looking down on the data from above the plot)
(see Figure 2-58). The x-axis is the retention time (min) and the y-axis is the
waveform period (ms). The z-axis, which is represented by different colors in
the plot, is the response (nA).

waveform time (ms)


z

)
nA
e(
ns
po
res

x
retention time (min)

Figure 2-58. 3D Amperometry Data in Chromeleon 6.8: Iso View

NOTE The 3D data shown in Figures 2-58 and 2-59 were collected
using an analytical waveform (see “Analytical vs. Scanning
Waveforms” on page 108).

To switch to the 3D plot view, right-click on the Iso plot, select Decoration
and click the Iso/3D Plot tab. The 3D view projects the response values in the
third dimension, which allows you to see the height of responses as well as the
colors representing different magnitudes of detection signal along the z-axis

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2 • DC Description

(see Figure 2-59). For this view, imagine you are standing in front and slightly
to the left of the plot.

z y

s)
(m
response (nA)

e
ti m
m
or
ef
av
w

x
retention time (min)

Figure 2-59. 3D Amperometry Data in Chromeleon 6.8: 3D View

Baseline Correction

Based on the peak recognition algorithm or by peaks obtained with a user


drawn base line, Chromeleon can calculate a baseline I-t plot for each data
point of a peak. Each I-t plot measured at a given retention time can be
corrected by subtracting the calculated baseline I-t plot from the 3D
amperometry data. By definition, if baseline correction is enabled, 3D
amperometry data is zero unless a peak is present.

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ICS-5000
TC TC Description

2.20 TC Front Features


A status bar on the front of the Dionex ICS-5000 Thermal Compartment (TC)
includes LEDs (light emitting diodes) that indicate the status of several TC
components and functions (see Figure 2-60).

LOAD INJECT LOAD INJECT

CONNECTED ALARM VALVE 1 VALVE 2 OVEN POWER

Figure 2-60. TC Status Bar

LED Label If the LED Is On If the LED Is Flashing


CONNECTED The TC is connected to a Does not flash.
Chromeleon 7 instrument
or a Chromeleon 6.8
timebase.
ALARM A sensor detected the Does not flash.
presence of a gas or
humidity leak inside the
TC, or a valve or oven
error was detected. Check
the Chromeleon Audit Trail
for the cause.
VALVE 1 LOAD Indicates whether the Valve error. See
VALVE 2 LOAD injection valve is in the Section 8.30 for
VALVE 1 INJECT Load or Inject position. troubleshooting.
VALVE 2 INJECT

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LED Label If the LED Is On If the LED Is Flashing


OVEN The TC is at its set The TC is transitioning to
temperature. the set temperature. The
TC is not ready for
operation.
If the LED is flashing and
the ALARM LED is
lighted, an oven error has
been detected. See
Section 8.30 for
troubleshooting.
POWER When the power is on, this Does not flash.
LED is lighted.
Use the POWER button
on the front of the TC for
routine on/off control. To
turn on the TC, press the
POWER button. To turn off
the TC, press and hold the
POWER button for
2 seconds.

NOTE The main power switch is on the TC rear panel (see


Figure 2-62).

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2 • TC Description

2.21 TC Interior Components


Figure 2-61 illustrates the interior of the TC. The components installed in
your TC may vary, depending on your application.

2 3

4
5
6

Slots for Column ID Chip


1 4 Guard Column
Cards (A, B, C, and D)

2 Injection Valves 5 Column Brackets

3 Separator Column 6 Temperature Stabilizer

Figure 2-61. TC Interior View (Dual System Configuration Shown)

Injection Valves

The TC can hold one or two electrically-actuated, high-pressure injection


valves. Two valve models are available:
• A 2-position, 6-port Rheodyne TitanHP™ injection valve
• A 2-position, 10-port Rheodyne TitanHP™ injection valve
See Section 2.23 for details about the injection valves.

Column Brackets

The column brackets are installed in the TC at the factory. The TC can hold up
to three columns with an inner diameter of 1 to 9 mm and a maximum length
of 30 cm (11.8 in). Columns are attached to the brackets with special column
clips (P/N 064786; set of six clips).

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Temperature Stabilizers (Optional)

Installation of a temperature stabilizer (standard bore, P/N 064548;


microbore, P/N 064650) ensures that (a) the temperature of the stationary
phase remains constant over the total column length and (b) the column and
the eluent have the same temperature during the analysis.
When these conditions are met, the analytical separation is performed at the
nominal temperature. This minimizes fronting and tailing of peaks, as well as
retention time variations.

Column ID Chip Card Slots

The TC column ID (identification) system lets you store column-specific


information on a memory card and read the information at any time. Up to
four column ID chip cards can be installed at the same time. The TC is
shipped with two column ID chip cards (P/N 5710.1500). An optional
Column ID Kit (P/N 066353) containing five chip cards is available.
See Section 2.24 for details about the column ID system.

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2 • TC Description

2.22 TC Rear Panel


Figure 2-62 illustrates the rear panel of the TC.

1 2 3

1 Main Power 2 Digital I/O 3 USB Receptacle 4 Drain Port


Switch, Fuse Connectors (2) (“B” Connector)
Holder, and Power
Receptacle

Figure 2-62. TC Rear Panel

Main Power Switch, Fuse Holder, and Power Receptacle

The rear panel power switch is the main power switch for the TC. Turn on the
main power switch before initial operation, and leave the switch on unless
instructed to turn it off (for example, before performing a service procedure).

NOTE For routine on/off control of the TC, use the POWER button
on the front of the module. To turn off the TC, press and hold
the POWER button for 2 seconds.

The fuse holder contains two 2-amp fuses (P/N 954776). For instructions on
how to change the fuses, see Section 9.33.
The power cord plugs into the IEC 320 three-prong receptacle.

The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the TC and is easily accessible.

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Le cordon d'alimentation principal est utilisé comme dispositif principal


de débranchement. Veillez à ce que la prise de base soit située/installée
près du module et facilement accessible.

Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen


Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht
zugänglich ist.

Digital I/O Connectors

The two 6-pin mini-DIN connectors can be used to exchange digital signals
with any external device capable of being controlled through a relay or TTL
input. The two connectors are identical in function.

Relay_Com Relay_N.O.*

Digital Input Digital_GND

Not Used Not Used

* N.O. = Normally open contact

Figure 2-63. Digital I/O Connector

When the relay is activated, the connection is between Com and N.O.

Connection Description
Digital Input <---> Digital_GND 0 to +5 V
Relay_Com <---> Relay_N.O. Switching voltage: 100 VDC
Switching current: 0.25 A
Carry current: 1.0 A
Switching capacity: 3 W
Contact resistance: Max. 150 megohms

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2 • TC Description

Use the 6-pin mini-DIN signal cable (P/N 6000.1004) provided in the TC
Ship Kit (P/N 064789) to connect the TC to an external device. For details
about the pin assignments, refer to Table 2-5.

Pin Signal Name Signal Level Core Core Label


Color
1 Not occupied ---- Pink Analog High
2 Not occupied ---- Gray Analog Low
3 Digital_GND 0V Green Digital GND
5 Digital Input 0 to +5 V Yellow Digital Input
6 Relay_N.O. 100 VDC/0.25 A/3 W Brown Digital Output
8 Relay_Com 100 VDC/0.25 A/3 W White Dig./Out (GND)
Black Shield

Table 2-5. Pin Assignments for the TC Mini-DIN Signal Cable

USB Receptacle

The USB (Universal Serial Bus) receptacle (“B” type connector) provides a
connection to the PC on which Chromeleon is installed. Select one of the
following methods to establish the connection:
• Connect the TC directly to the USB receptacle on the PC.
• Connect the TC to the PC through another USB device in the system (for
example, the pump).
The TC Ship Kit (P/N 064789) includes a 1 m (3 ft) USB cable (P/N 063246).

Drain Port

The drain port removes any liquid that collects in the drip tray in the bottom
of the TC. A clear corrugated drain hose (P/N 055075) is connected to this
port during installation. Place the drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
TC.

For correct drainage, make sure the drain hose is not bent, pinched, or
elevated at any point. Do not allow the end of the hose to be submerged
in waste liquid.

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2.23 Injection Valves


The TC is available in the following configurations:

TC Description Part Number


TC with no injection valves 074108
TC with one 2-position, 6-port high-pressure injection valve 074109
TC with two 2-position, 6-port high-pressure injection valves 074112
TC with one 2-position, 6-port high-pressure injection valve 074113
and one 2-position, 10-port high-pressure injection valve
(The 6-port valve is installed on the left side of the module.)

2.23.1 Injection Valve Operation


The 6-port injection valve has two operating positions: Load and Inject.
Liquid flows through either the Load or Inject path, depending on the valve
position.
Figure 2-64 shows flow schematics for the 6-port valve.

LOAD POSITION INJECT POSITION

To Waste To Waste
Sample In Sample In

W (6) W (6)
S (5) S (5)

L (4) L (4)

To Column To Column
From Pump From Pump

= Sample = Eluent

Figure 2-64. TC Injection Valve Flow Schematics (6-Port Valve)

• In the Load position, sample is loaded into the sample loop, where it is
held until injection. Eluent flows from the pump, through the valve, and
to the column, bypassing the sample loop. Sample flows from the syringe

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2 • TC Description

or autosampler line (if installed), through the valve, and into the sample
loop. Excess sample flows out to waste.
• In the Inject position, sample is swept to the column for analysis. Eluent
flows from the pump, through the sample loop, and on to the column,
carrying the contents of the sample loop with it. Section 5.3.1 describes
how to inject samples.
The 10-port injection valve has two operating positions: 10_1 and 1_2. Liquid
flows through the path between either ports 10 and 1 or ports 1 and 2,
depending on the valve position.
Figure 2-65 shows example flow schematics for the 10-port valve when it is
connected for an application that uses a concentrator column.

10_1 POSITION 1_2 POSITION


(Loop Loading) (Concentrator Loading)

Concentrator Concentrator

To Column To Column
6 6
Eluent Eluent
5 Pump In 7 4 Pump In
7 4 5
8 8
9
Large 9 3 To Waste Large 3
Loop To Waste
10 1 Loop 1
10 2
2

Sample In Carrier Pump In Sample In Carrier Pump In


To Waste To Waste

= Sample
= Carrier
= Eluent

Figure 2-65. TC Injection Valve Flow Schematics (10-Port Valve)


Example Connections: Large Loop to Concentrator

• In the 10_1 position, sample flows from the syringe or autosampler line,
through the valve, and into the sample loop. Excess sample flows out to
waste. Eluent flows from the eluent pump, through the valve, through the
concentrator column, and to the separator column. If sample was
previously loaded onto the concentrator column, it is swept to the
separator column for analysis.

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• In the 1_2 position, carrier liquid flows through the sample loop and on to
the concentrator column, carrying the contents of the sample loop with it.
Excess flows out to waste. Eluent flows from the pump, through the
valve, and to the separator column, bypassing the concentrator column.

2.23.2 Injection Valve Plumbing


Figure 2-66 shows the injection valve connections for the 6-port valve. The
injection valve is plumbed at the factory with all tubing and fittings for
connection to the pump, sample loading port, column, and waste. A 25 L
PEEK sample loop (P/N 042857) is installed between ports L (1) and L (4).
Thermo Fisher Scientific offers sample loops in various sizes. If needed, the
pre-installed 25 L loop can be replaced with a loop that has a different
sample injection volume.

(Green)

TO INJECT SAMPLE IN
VALVE -W (from door
inject port or
autosampler)
W (6)

S (5)

25 μL SAMPLE LOOP
(Orange) L (4)

TO INJECT
VALVE -P TO INJ (Red - microbore)
VALVE -C (Black - standard bore)

Figure 2-66. Injection Valve Plumbing (6-Port Valve)

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2 • TC Description

2.24 Column Identification (ID) System


The electronic column ID system stores column-specific information on a
column ID chip card (P/N 5710.1500) that is connected to a column for the
column life cycle (see Figure 2-67).

Column ID Chip Card

Figure 2-67. Column ID (Identification) System

The columns to be monitored are selected in the TC Properties dialog box in


the Chromeleon 7 Instrument Configuration program or the Chromeleon 6.8
Server Configuration program. To select column properties (see below) for
storage and to review the stored information at any time, use the TC ePanel in
Chromeleon 7 or the TC Control panel in Chromeleon 6.8. The properties are
also available in the Chromeleon Commands dialog box. Information on the
column ID chip card is continuously updated, as long as the column and the
chip card are installed in the TC.

Column Properties

Two types of information can be stored on the column ID chip card:


• Primary column properties are entered once by the column manufacturer
or the user and are never changed during the lifetime of the column. The
primary properties are the product ID, serial number, batch/lot number,
date of manufacture, and custom information.
• Secondary column properties are entered by the user and can be changed
whenever required by any Chromeleon user with Expert privileges.
Secondary properties include the column manufacturer, diameter, length,
particle size, maximum number of injections, pH limits, and upper
pressure limit. For a complete list of secondary properties, refer to the
Chromeleon Help.

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2.25 Gas and Humidity Sensors


The TC contains two sensors to detect any gas or humidity that may
accumulate inside the TC. When a certain concentration of gas or humidity is
reached (while the door is closed), the following events occur:
• The corresponding sensor is activated.
• The ALARM LED on the front of the TC lights (red), and remains red as
long as the sensor is exposed to gases or humidity.
• The error is logged in the Chromeleon Audit Trail.
• A beep sounds.

What to do when an alarm occurs:

1. Find and eliminate the leak.


2. If you are using Chromeleon 7: Open the Commands dialog box (press
the F8 key). Select the TC and click the Commands tab. Click the
ClearAlarmLED button.
3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door and
resuming operation.

Adjusting the Sensor Sensitivity

Follow these steps to change the sensitivity setting of the gas or humidity
sensor, or to turn off a sensor:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the TC.
4. If you are using Chromeleon 7: Click the Parameters tab page for the
TC, click the GasLeakSensor or HumidityLeakSensor parameter.
Select the new sensitivity setting (or select Off to disable the sensor).
5. If you are using Chromeleon 6.8, click the plus sign beside TC to display
the items underneath. Under TC_Temp, select the GasLeakSensor or

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2 • TC Description

HumidityLeakSensor parameter. Select the new sensitivity setting (or


select Off to disable the sensor) and click Execute.

2.26 TC Theory of Operation


The fundamental requirement for a thermal compartment intended for
chromatography applications is the ability to maintain the preset temperature
as precisely as possible. The TC contains advanced electronic circuitry that
maintains the selected temperature with a precision of ±0.1 °C.
The TC can be heated from 5 to 85 °C in 0.1 °C increments. An increase in
temperature from 20 to 50 °C (or a decrease from 50 to 20 °C) is typically
realized in less than 20 minutes. Columns can be warmed up to 85 °C. If the
ambient temperature changes during the analysis, increased heating or cooling
ensures that the column temperature remains constant.
Operating IC columns at temperatures above 70 °C (158 °F) may affect
column performance. Before selecting the TC temperature, refer to the
column manual for the recommended operating conditions. Column
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).

The thermo-optimized design of the TC reduces the time required to


equilibrate the temperature between the column and the eluent. Peltier
elements in the TC heat up and cool down the columns. They also help to
bring the air and all of the installed components (including the injection
valves) to the selected temperature.
If necessary, a temperature stabilizer (standard bore, P/N 064548; microbore,
P/N 064650) can be installed in the TC. Installation of a temperature stabilizer
ensures that:
• The stationary phase temperature remains constant over the total column
length.
• The column and the eluent have the same temperature during the analysis.
Under these conditions, the separation is performed at the nominal
temperature. This minimizes fronting and tailing of peaks, as well as retention
time variations.

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The temperature achieved may vary from the control range, depending on the
ambient temperature (see the table below).

Control Range Achieved Temperatures (Based on Ambient)


5 to 85 °C Minimum temperature 18 °C below ambient
Maximum temperature 70 °C above ambient

For example, if the ambient air temperature in the lab is 30 °C and you set the
temperature to 5 °C, the actual temperature achieved will be about 12 °C.
Do not touch any metal parts inside the TC while it is heating up or after
it reaches the set point temperature. Wait for the compartment to cool
down before servicing any parts.

Ne touchez à aucune des pièces métalliques à l'intérieur du TC pendant


qu'il chauffe ou après qu'il ait atteint la température de consigne.
Attendez que le compartiment soit refroidi avant de réparer les pièces.

Berühren Sie im TC keine metallischen Teile, während dieses


aufgeheizt wird oder nachdem die Solltemperatur erreicht ist. Warten
Sie, bis die Kammer abgekühlt ist, ehe Sie Wartungsarbeiten
durchführen.

2.26.1 Predictive Performance


The Predictive Performance feature of the TC provides various functions for
estimating the lifetime of replaceable parts and for planning and recording
service and qualification procedures.
A partial list of the TC Predictive Performance functions is provided below.
Refer to the Chromeleon Help for details.
• Monitoring of the total cooling and heating workload performed by the
compartment and the total operating hours since initial operation
• Monitoring of the injection valve usage
• Reminders for service and qualification periods, including display of
warning messages when limits are approaching or overdue
Predictive Performance commands and parameters are available in the
Chromeleon Commands dialog box.

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3 • Configurations

3.1 Overview
This chapter provides example component and plumbing drawings for the
following Dionex ICS-5000 system configurations:

Dionex ICS-5000 IC System Configuration See


Capillary IC: Dual RFIC-EG System (CD/CD) page 130
Capillary IC: Dual RFIC-EG System (CD/ED) page 131
Hybrid System: Dual RFIC-EG System (CD Analytical/CD page 132
Capillary)
Analytical IC: Single System without EG (CD) page 133
Analytical IC: Single RFIC-EG System (CD) page 134
Analytical IC: Dual RFIC-EG System (CD/CD) page 135
Analytical IC: Dual RFIC-EG System (CD/ED) page 136
Analytical IC: Single RFIC-EG System with Matrix Elimination page 137
Using a DP and a 6-Port Valve
Analytical IC: Single RFIC-EG System with Matrix Elimination page 138
Using an SP and a 10-Port Valve
Analytical IC: Single RFIC-EG System with Post-Column page 139
Reagent Addition (Bromate)
Analytical IC: Single RFIC-EG System with ED and VP (for page 140
Carbohydrate Analysis)

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To pump #2 inlet via the pump rear chase Pump (front view)

To pump #1 inlet via the pump rear chase Seal


Wash
Pump

System #2

(pump not to scale) To waste

To EGC
#2 In Piston
Seal
Wash
System #1

Deionized Deionized
Water Water

To EGC
#1 In To waste

From IC Cube #2 EG Degas Regen Out


DC (front view) To IC Cube #2 EG Degas Eluent In
ELUENT IN ELUENT IN
EG EG
ELUENT IN
ELUENT OUT
REGEN OUT ELUENT IN
ELUENT OUT
REGEN OUT
(left side view) System #1 System #2 (right side view)
ELUENT IN ELUENT IN
ELUENT OUT ELUENT OUT

ELUENT OUT ELUENT OUT


ELUENT OUT ELUENT OUT
ELUENT IN EG ELUENT IN EG
From CRD 200 CES 300 DEGAS CRD 200 CES 300 DEGAS

autosampler ELUENT OUT REGEN IN ELUENT OUT REGEN IN EGC EGC


SAMPLE IN SAMPLE IN

SAMPLE OUT ELUENT IN SAMPLE OUT ELUENT IN


(capillary) (capillary)

CELL IN CELL OUT CELL IN CELL OUT


Conductivity Detector Conductivity Detector
(Capillary) (Capillary)

System #1 System #2

From
autosampler
To waste
To waste
From IC Cube #1
EG Degas Regen Out Regen Out
Regen Out
Regen In Regen In

Eluent In Eluent In Eluent Out


To IC Cube #1
EG Degas
Eluent In Eluent Out

To waste

To waste

Figure 3-1. Capillary IC: Dual RFIC-EG System (CD/CD)

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3 • Configurations

Pump (front view)


To pump #2 inlet via the pump rear chase

To pump #1 inlet via the pump rear chase Seal


Wash
Pump

System #2

To waste
(pump not to scale)
To EGC
#2 In Piston
Seal
Wash
System #1

Deionized Deionized
Water Water

To waste
To EGC
#1 In
From IC Cube #2 EG Degas Regen Out
DC (front view) To IC Cube #2 EG Degas Eluent In
ELUENT IN
EG EG
System #1
ELUENT IN

(left side view) System #2


ELUENT IN REGEN OUT
ELUENT OUT ELUENT OUT
REGEN OUT
(right side view)
ELUENT IN
ELUENT OUT ELUENT OUT

ELUENT OUT ELUENT OUT


ELUENT OUT
ELUENT IN EG ELUENT IN EG
From CRD 200 CES 300 DEGAS
CRD
BYPASS
SUPPRESSOR
BYPASS DEGAS

autosampler ELUENT OUT REGEN IN REGEN IN EGC EGC


SAMPLE IN
(capillary)
SAMPLE IN

SAMPLE OUT ELUENT IN SAMPLE OUT ELUENT IN


(capillary)

CELL IN CELL OUT EC CELL


Conductivity Detector OUT
(Capillary)
IN

System #1 System #2

From
autosampler
To waste
To waste
From IC Cube #1
EG Degas Regen Out Regen Out
Regen Out
Regen In Regen In

Eluent In Eluent In Eluent Out


To IC Cube #1
EG Degas
Eluent In Eluent Out

To waste

To waste

Figure 3-2. Capillary IC: Dual RFIC-EG System (CD/ED)

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Dionex ICS-5000 Operator’s Manual

To pump #2 inlet via the pump rear chase Pump (front view)

To pump #1 inlet via the pump rear chase Seal


Wash
Pump

System #2
To EGC
#2 In
(pump not to scale) To waste

A
Piston B
Seal C
Wash
System #1 D

Deionized Deionized
A B
Water Water
D C
Mixer To waste
To EGC #1 In
From the suppressor Regen Out via the DC rear chase
From the IC Cube EG Degas Regen Out
DC (front view) To the IC Cube EG Degas Eluent In
ELUENT IN
EG EG
ELUENT IN
ELUENT OUT
REGEN OUT
(left side view) System #1 System #2 (right side view)
ELUENT IN
ELUENT OUT

ELUENT OUT
ELUENT OUT
ELUENT IN EG
DEGAS
From autosampler CRD 200 CES 300

To waste
ELUENT OUT REGEN IN EGC
SAMPLE IN

SAMPLE OUT ELUENT IN (capillary)


EGC
Cell In Cell Out CELL IN CELL OUT
Conductivity Detector
(Capillary)

Regen Out Eluent Out


System #2 Regen Regen
Out In
Eluent In Regen In
Eluent Eluent
Out In

Regen
Out Regen Out
In Out Eluent
Eluent
Out

ELUENT OUT
System #1 In

REGEN IN
Regen In
Separator
Regen In
CR-TC Eluent In Eluent
Guard
(5) S L (4) Out
Temp .
Stabilizer W C
(6) (3) Backpressure
Device To the degasser Regen In via the EG rear chase
From autosampler
(1) L P (2) To waste
To waste

To waste

Figure 3-3. Hybrid System: Dual RFIC-EG System (CD Analytical/CD Capillary)

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3 • Configurations

To the pump inlet via the pump rear chase

Eluent

DC (front view) Pump (front view)

Seal
Wash
Pump

Cell In Cell Out

Regen Out Eluent Out

Eluent In Regen In
Piston
Seal
Wash

Pump inlet
Separator

Guard
(5) S L (4)
Temp.
Stabilizer W C
(6) (3)
Mixer On/Off Valve
(1) L P (2)
From AS
To waste
To AS/Waste

Figure 3-4. Analytical IC: Single System with no EG (CD)

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Dionex ICS-5000 Operator’s Manual

Pump (front view)


To the pump inlet via the pump rear chase
Seal
Wash
Pump

(pump not to scale)

Piston
Seal

Pump inlet
Wash
Deionized
Water

On/Off
Mixer
Valve
To waste
From the suppressor Regen Out via the DC rear chase

DC (front view)
EG
(left side view)

EGC

Regen Regen
Cell In Cell Out Out In

Regen Out Eluent Out Eluent Eluent


Out In
Eluent In Regen In
Regen
Out
In Out Eluent Eluent
Out

ELUENT OUT
In

REGEN IN
Separator
Regen In
Guard CR-TC
(5) S L (4)
Temp .
Stabilizer W C
(6) (3) Backpressure
Device
(1) L P (2) To the degasser Regen In via the EG rear chase
From AS
To AS /Waste

To Waste

Figure 3-5. Analytical IC: Single RFIC-EG System (CD)

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3 • Configurations

To pump #2 inlet via the pump rear chase Pump (front view)
A
To pump #1 inlet via the pump rear chase Seal B
Wash
Pump C
D

System #2 A B

D C
Mixer
To waste
(pump not to scale)
A
Piston B
Seal C
System #1 Wash D

Deionized Deionized
Water Water A B

Mixer D C

To waste

From suppressor #1 Regen Out via the DC rear chase From suppressor #2 Regen Out via the DC rear chase
DC (front view)
EG EG
(left side view) (right side view)
System #1 System #2

To the degasser #2 Regen In via the EG rear chase


EGC EGC

Cell In
Regen Regen Regen Regen
Cell Out Cell In Cell Out
Out In Out In
Regen Out Eluent Out Regen Out Eluent Out Eluent Eluent Eluent Eluent
Out In Out In
Eluent In Regen In Eluent In Regen In
Regen
Regen To inject valve
Out #2 port P (2)
Eluent Eluent Out Eluent
In Out Out In Out

ELUENT OUT
In Out

REGEN IN

ELUENT OUT
REGEN IN
Separator #2
Separator #1
Regen In Eluent
Guard #2 Guard #1 Regen In
Backpressure Device

In
CR-TC CR-TC
(5) S L (4) (5) S L (4)
Temp. Temp.
Stabilizer W C W C Stabilizer
(6) (3) From AS (6) (3)
To the degasser #1 Regen In via the EG rear chase
From AS (1) L P (2) To AS /Waste (1) L P (2) To waste
To AS /Waste Backpressure Device

System #1 System #2 To waste

Figure 3-6. Analytical IC: Dual RFIC-EG System (CD/CD)

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Dionex ICS-5000 Operator’s Manual

To pump #2 inlet via the pump rear chase Pump (front view)
To pump #1 inlet via the pump rear chase A
Seal B
Wash
Pump C
D

System #2 A B

Mixer
Mixing D C
Chamber
To waste
(pump not to scale)
A
Piston B
Seal
C
Wash
System #1 D

Deionized
Eluent
Water A B

Mixing
Mixer D C
Chamber
To waste

From suppressor #1 Regen Out via the DC rear chase


From the ED cell out via the DC rear chase
DC (front view) From pump #2
EG EG
(left side view) (right side view)
System #1 System #2

To the degasser #2 Regen In via the EG rear chase


EGC EGC

Cell In Cell Out


Regen Regen Regen Regen
Regen Out Eluent Out Out In Out In

Eluent Eluent Eluent Eluent


Eluent In Regen In Out In Out In

To the degasser #2 Regen Regen To inject valve


Out Out #2 port P (2)
In Out Eluent In Out Eluent

ELUENT OUT

ELUENT OUT
In

REGEN IN
Separator #2

REGEN IN
In
Separator #1 To inject
valve #1 Eluent Eluent
Regen In Regen In
Out
Backpressure Device

Guard #2 Guard #1 port P (2) Out


CR-TC CR-TC
(5) S L (4) (5) S L (4)
Temp . Temp .
W C W C
Stabilizer (6) (3) Stabilizer
From AS (6) (3)
To AS /Waste (1) L To the degasser #1 Regen In via the EG rear chase To waste
From AS (1) L P (2) P (2)
To AS /Waste Backpressure Device

System #1 System #2 To waste

Figure 3-7. Analytical IC: Dual RFIC-EG System (CD/ED)

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3 • Configurations

To pump #2 inlet via the pump rear chase


Pump (front view)
To pump #1 inlet (A) via the pump rear chase

Seal

Pump inlet
Wash
Pump

Pump #2

On/Off
Mixer Valve
To waste
(pump not to scale)
A
Piston B
Seal C
Wash D
Pump #1
Deionized Deionized
Water Water
(carrier) A B

Mixer D C

To waste
From the suppressor Regen Out via the DC rear chase

DC (front view)
EG
(left side view)
5 4

3 Large Loop
6
1 2
From AS
To AS/Waste

EGC

To inject valve sample port


Regen Regen
Cell In Cell Out Out In

Regen Out Eluent Out Eluent Eluent


Out In
Eluent In Regen In
Regen
In Out Out
Eluent

ELUENT OUT
In

REGEN IN
Separator Eluent
Regen In Out
Guard CR-TC
(5) S L (4)
Temp .
Stabilizer W C
(6) (3)
Backpressure
(1) L P (2) Device To the degasser Regen In via the EG rear chase
To AS /Waste

To Waste

Figure 3-8. Analytical IC: Single RFIC-EG System with Matrix Elimination Using a DP and a 6-Port Valve

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Dionex ICS-5000 Operator’s Manual

To pump #2 inlet via the pump rear chase


Pump (front view)
To pump #1 inlet (A) via the pump rear chase
Injection Valve
Connections Key Seal

Pump inlet
Wash
Concentrator Pump

To column
Pump #2
Sample in 6 Eluent in
On/Off
Mixer Valve
7 5 To waste
8 4
9 (pump not to scale)
1 3 To waste
10 A
2 Piston B
Seal
Carrier pump in Wash
C
D
To waste Pump #1
Deionized Deionized
Water Water
(carrier) A B

Mixer D C

To waste
From the suppressor Regen Out via the DC rear chase

DC (front view)
EG
(left side view)

EGC

Cell In Regen Regen


Cell Out
Out In
Regen Out Eluent Out Eluent Eluent
Out In
Eluent In Regen In
Regen
Out
In Out Eluent

ELUENT OUT
In

REGEN IN
Separator
Regen In Eluent
Out
Guard CR-TC
6
7 5
8 4
Concentrator
9 3
1 Backpressure Device
10 2 To the degasser Regen In via the EG rear chase
From AS
Large Loop
To AS /Waste
To Waste

Figure 3-9. Analytical IC: Single RFIC-EG System with Matrix Elimination Using an SP and a 10-Port Valve
138 Doc. 065342-06 12/11
3 • Configurations

To pump #2 inlet via the pump rear chase


To Regen In Pump (front view)
via the DC To pump #1 inlet (A) via the pump rear chase
rear chase
To 3-way valve #1 COM Port Seal

Pump inlet
Wash
via the DC rear chase
Pump

Pump #2

On/Off
Mixer Valve
To waste
(pump not to scale)
A
Piston B
Seal C
Wash D
Deionized To the
Water
Deionized Pump #1
Reagent absorbance
Water
(Regen) or PDA
detector A B

Mixer D C

From the suppressor Regen Out via the DC rear chase To waste

DC (front view)
plug EG
Reagent in M N.O. M
CO N.O.
(left side view)
CO
from pump #2 N.C. N.C.

RCH-1

EGC
To waste

Cell In Cell Out Regen Regen


Out In
Regen Out Eluent Out Eluent Eluent
Out In
Eluent In Regen In
Regen
Out
In Out Eluent

ELUENT OUT
In

REGEN IN
Separator Eluent
Regen In Out
CR-TC
(5) S L (4) Guard
Temp.
Stabilizer W C
(6) (3)
Backpressure
From AS
(1) L P (2) To the degasser Regen In via the EG rear chase
Device
To AS /Waste

To Waste

Figure 3-10. Analytical IC: Single RFIC-EG System with Post-Column Reagent Addition (Bromate)

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Dionex ICS-5000 Operator’s Manual

Pump (front view)


To the pump inlet via the pump rear chase
Seal
Wash
Pump

(pump not to scale)


A
Piston B
Seal C
Wash D
Deionized
Water
VP A B
Ballast
Bottle To the Mixer D C
VP
To waste

DC (front view)
EG
(left side view)

From the degasser Regen Out


EGC

Regen Regen
Out In

Eluent Eluent
To the CR -TC Regen In Out In

Regen
Out
In Out Eluent Eluent
Out Plu

ELUENT OUT
In

REGEN IN
CarboPac PA20
Regen In
CR-TC
(5) S L (4)
Temp . Amino Trap or PA 20 Guard
Stabilizer W C
(6) (3) Backpressure
Device
(1) L P (2) To the CR-TC Regen In via the EG rear chase
From AS From the degasser Eluent Out
To AS /Waste

To Waste

Figure 3-11. Analytical IC: Single RFIC-EG System with ED and VP (for Carbohydrate Analysis)

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4 • Startup

This section is an overview of the steps required to start up the Dionex ICS-
5000 system components and prepare the system to run samples. The
operating parameters (flow rate, compartment temperature, suppressor
current, etc.) depend on the application you plan to run. Refer to the column
manual, as well as the schematics in Chapter 3 of this manual, for the required
operating parameters.

NOTE Before beginning operation, be sure to perform any special


startup procedures required for the columns, suppressors, etc.
Startup procedures are described in the quick start guides and
manuals provided on the Thermo Scientific Reference
Library DVD (P/N 053891).

4.1 Operating Precautions

4.1.1 EG Operating Precautions


In an analytical IC system, the EGC requires at least 14 MPa (2000 psi) of
system backpressure. This ensures optimal removal of electrolysis gas from
the eluent produced by the cartridge.
During system equilibration, monitor the Current Pressure reading on the
Pump panel in Chromeleon; the pressure should remain between 14 and
21 MPa (2000 and 3000 psi). If necessary, increase the system backpressure
by installing a backpressure coil between the injection valve and the ELUENT
OUT port on the EGC. For instructions, refer to Section 9.17.

The recommended maximum operating pressure for the EG in an


analytical IC system is 21 MPa (3000 psi). Excessive backpressure may
rupture the tubing inside the RFIC Eluent Degasser.

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DO NOT CAP THE WASTE CONTAINER: The Dionex ICS-5000 Eluent


Generator (EG), Atlas Electrolytic Suppressor, and Self-Regenerating
Suppressor (SRS) use an electrolytic process that results in the
production of small amounts of oxygen or hydrogen gas. To ensure that
the gas is not trapped in a closed container and allowed to concentrate,
install a 1.3 cm (0.52 in) ID black gas separator waste tube (P/N 045460)
in an uncapped waste container. Connect the Waste, Gas Separator line
to the waste tube.

NE FERMEZ PAS LE CONTENEUR DE GAZ RÉSIDUEL: Le Dionex ICS-


5000 Eluent Generator (EG), le Atlas Electrolytic Suppressor, et le Self-
Regenerating Suppressor (SRS) travaillent avec un proces
d´électrolyse, qui produit des petites quantités de gaz d´oxygène ou
d´hydrogène. Afin de garantir que le gaz ne soit pas enfermé dans un
conteneur fermé et puisse s´y concentrer, connectez un tube noir à gaz
résiduel (diamètre intérieur = 1,3 cm; n° de commande 045460) à un
conteneur ouvert (non fermé). Connectez le conteneur résiduel au tube
résiduel/gaz séparateur (désigné: « Waste, Gas Separator»).

VERSCHLIESSEN SIE DEN ABFALLBEHÄLTER NICHT: Der Dionex ICS-


5000 Eluent Generator (EG), Atlas Electrolytic Suppressor und Self-
Regenerating Suppressor (SRS) verwenden einen Elektrolyseprozess,
wodurch kleine Mengen an Sauerstoff und Wasserstoff entstehen.
Führen Sie einen schwarzen Gasabscheiderschlauch (ID = 1,3 cm;
Bestell-Nr. 045460) in einen offenen (unverschlossenen) Abfallbehälter,
damit sich das Gas nicht in einem geschlossenen Behälter sammelt
und aufkonzentriert. Verbinden Sie die mit Waste, Gas Separator
bezeichnete Leitung mit dem Abfallschlauch.

If you select a low flow rate that allows the system pressure to drop below
14 MPa (2000 psi) and you do not turn off the EG, the EG will continue to
generate eluent at the concentration set for the last step of the last Chromeleon
7 instrument method or Chromeleon 6.8 program.
If this occurs, the eluent concentration will increase in proportion to the
decrease in the flow rate. In extreme cases, excessive heat buildup can occur
and damage the EGC.
For a complete list of operating precautions for EGCs and CR-TC trap
columns, refer to the product manuals. The manuals are provided on the
Thermo Scientific Reference Library DVD (P/N 053891).

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4 • Startup

4.1.2 ED Cell Operating Precautions


To maintain good reproducibility of detection results:
• Prepare all eluents with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
• Avoid contamination of the cell with incompatible eluents.
• Never apply potential to the electrode unless a stream of eluent or water is
flowing through the cell.
• Do not allow a pH-Ag/AgCl reference electrode to dry out. Make sure
that eluent is pumped continuously through the cell. If the cell will not be
used for a short time (less than 2 days), disconnect the tubing from the
inlet and outlet fittings and all fitting plugs. For longer shutdowns, see
Section 6.4.
• Be careful to keep the polished surface of the ED cell body clean and dry
when not in use. The gold, spring-loaded (pogo) contact must also remain
clean and dry. If a salt bridge forms, it can cause an electrical short
between the working electrode contact and the cell body.
• If the conventional (nondisposable) working electrode becomes
discolored or if you notice a degradation in performance (baseline noise,
tailing peaks, etc.), polish the electrode as instructed in Section 9.28.4.
• Over the lifetime of the conventional working electrode, the surface may
gradually become pitted or receded. Receded electrodes can be repaired
by sanding with 600 grit sandpaper. Continue sanding until the metal
surface is again flush with the Kel-F electrode block surface. Then, polish
the electrode (see Section 9.28.4).
• To help determine when the pH-Ag/AgCl reference electrode needs
regenerating or replacing, monitor the pH value displayed on the detector
panel in Chromeleon (see page 144).
• To have an alarm displayed in the Audit Trail if the pH exceeds certain
values, set pH limits in Chromeleon (see page 145).

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Dionex ICS-5000 Operator’s Manual

To monitor the pH-Ag/AgCl reference electrode pH:

1. At installation, calibrate the pH electrode (see Section 9.28.6).


2. When you run your first chromatographic instrument method or program,
note the pH value displayed on the Chromeleon panel (see Figure 4-1).

Figure 4-1. Monitoring the pH-Ag/AgCl Reference Electrode pH

3. Thereafter, monitor the pH value to determine whether there is a shift in


the pH. A shift in the pH reading for the same eluent composition
indicates a change in the Ag/AgCl reference potential.
If the pH value shifts by 0.5 pH unit from the value first observed, check
the pH-Ag/AgCl reference electrode (see Section 8.28.6).

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4 • Startup

To set ED cell pH limits:

You can set upper and lower pH limits in the Chromeleon 7 Instrument
Method Wizard (see Figure 4-2) or Chromeleon 6.8 Program Wizard. The
Audit Trail displays an alarm if the limits are exceeded.

Figure 4-2. Setting pH Limits in Chromeleon 7

NOTE To disable the alarm, set the upper limit to 14 and the lower
limit to 0.

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4.2 System Startup Checklist


 Prepare the samples (see page 147)
 Fill the autosampler vials and load the sample tray (see page 149)
 Start Chromeleon (see page 149)
 Set up the eluent reservoirs (see page 153)
 Set up the piston seal wash system (see page 154)
 Start the pump (see page 157)
 Set the pressure limits (see page 158)
 If an EG is installed, start the EG and set the eluent concentration (see
page 161)
 Start the DC (see page 165) or TC (see page 169)
 Equilibrate the system and verify operational readiness (DC: see
page 166; TC: see page 170)

NOTE You can use the Smart Startup feature in Chromeleon to auto-
mate system startup and equilibration. Refer to the Chrome-
leon Help for details.

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4 • Startup

4.3 Preparing Samples


This section provides basic information about collecting, storing, and
preparing samples for analysis.

NOTE Sample preparation can be performed while the system is


equilibrating.

4.3.1 Collecting and Storing Samples


Collect samples in high density polyethylene, polystyrene, or polycarbonate
containers that have been thoroughly cleaned with ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the specifications
listed in Section 1.5. Do not clean containers with strong acids or detergents
because these can leave traces of ions on the container walls. The ions may
interfere with the analysis.
If samples will not be analyzed on the day they are collected, filter them
through clean 0.45 micron filters immediately after collection; otherwise,
bacteria in the samples may cause the ionic concentrations to change over
time. Refrigerating the samples at 4C (39 F) will reduce, but not eliminate,
bacterial growth.
Analyze samples containing nitrite or sulfite as soon as possible. Nitrite
oxidizes to nitrate, and sulfite to sulfate, thus increasing the measured
concentrations of these ions in the sample. In general, samples that do not
contain nitrite or sulfite can be refrigerated for at least one week with no
significant change in anion concentration.

4.3.2 Pretreating Samples


Analyze rainwater, drinking water, and air particulate leach solutions directly
with no sample preparation (other than filtering and if required, diluting).
Filter groundwater and wastewater samples through 0.45 micron filters before
injection, unless samples were filtered after collection.
A Low-Volume High-Pressure Inline Filter (P/N 074505) is available for
removing particulates down to 0.45 micron from samples. Connect the inline
filter between the autosampler outlet and the sample inlet port on the injection
valve. For details, see the instructions provided with the inline filter.

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Before injection, pretreat samples that may contain high concentrations of


interfering substances by putting them through Thermo Scientific Dionex
OnGuard™ cartridges. Refer to the installation and troubleshooting guide for
the Dionex OnGuard cartridge for instructions. The guide is located on the
Thermo Scientific Reference Library DVD (P/N 053891).

4.3.3 Diluting Samples


Because the concentrations of ionic species in different samples can vary
widely from sample to sample, no single dilution factor can be recommended
for all samples of one type. In some cases (for example, many water samples),
concentrations are so low that dilution is not necessary.
To dilute the sample, use eluent or ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5. When
using carbonate eluents, diluting with eluent minimizes the effect of the water
dip at the beginning of the chromatogram. If you dilute the sample with
eluent, also use eluent from the same lot to prepare the calibration standards.
This is most important for fluoride and chloride, which elute near the water
dip.
To improve the accuracy of early eluting peak determinations, such as
fluoride, at concentrations below 50 ppb, dilute samples in eluent or spike the
samples with concentrated eluent to minimize the water dip. For example,
spike a 100 mL sample with 1.0 mL of a 100 X eluent concentrate.

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4 • Startup

4.3.4 Filling the Autosampler Vials and Loading the Sample Tray
Follow the instructions in the autosampler manual to fill the vials or well
plates and load them into the sample tray or carousel. The autosampler
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).

4.4 Starting Chromeleon 7

4.4.1 Starting the Chromeleon 7 Instrument Controller Service


To start the Chromeleon 7 Instrument Controller Service, right-click the
Chromeleon tray icon (which is crossed out in red) and click Start
Chromeleon Instrument Controller. The icon changes to gold to
indicate that the Instrument Controller Service is starting. When the
Instrument Controller Service is running (idle), the icon changes to gray .
If the Chromeleon Tray Icon is not on the taskbar, click Start > All Programs
> Chromeleon 7 > Services Manager to open the Services Manager and
click Start Instrument Controller.

4.4.2 Starting the Chromeleon 7 Client


1. To start the Chromeleon 7 client, click Start > All Programs >
Chromeleon 7 > Chromeleon 7.
2. To display the Chromeleon 7 ePanel Set, click the Instruments category
bar on the Console. Click your instrument in the Navigation Pane.
Chromeleon 7 connects to the instrument and displays the ePanel Set (see
Figure 4-3). The ePanel Set opens to the Home panel by default. This
panel displays basic status information for each instrument in the system.

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In addition, a limited number of device functions can be controlled


directly from this panel. You can also access the Audit Trail from here

Figure 4-3. Example Chromeleon 7 ePanel Set

4.5 Starting Chromeleon 6.8

4.5.1 Starting the Chromeleon 6.8 Server


To start the Chromeleon 6.8 Server, right-click the Chromeleon Server
Monitor icon (which is crossed out in red) on the Windows taskbar and
click Start Server. The icon changes to gold to indicate that the
Chromeleon Server is starting. When the Chromeleon Server is running (idle),
the icon changes to gray .
If the Server Monitor icon is not on the Windows taskbar, click Start > All
Programs > Chromeleon > Server Monitor to open the Server Monitor and
click Start.

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4 • Startup

4.5.2 Starting the Chromeleon 6.8 Client


1. To start the Chromeleon 6.8 client, click Start > All Programs >
Chromeleon > Chromeleon.
2. To display the Chromeleon 6.8 panel tabset, click View > Default Panel
Tabset or click the toolbar button . The panel tabset opens to the
Home panel by default (see Figure 4-4). This panel displays basic status
information for each instrument in the system. In addition, a limited
number of device functions can be controlled directly from this panel.
You can also access the Audit Trail from here.

Figure 4-4. Example Chromeleon 6.8 Panel Tabset

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ICS-5000
DP/SP DP/SP Startup

4.6 Setting Up the Eluent Reservoirs


1. Rinse the eluent reservoirs with ASTM Type I (18 megohm-cm) filtered
and deionized water.

NOTE Always use ASTM Type I (18 megohm-cm) filtered


and deionized water that meets the specifications
listed in Section 1.5 to prepare eluent and regenerant
or to rinse eluent reservoirs.

2. If an EG is not installed, prepare the eluent for the application. For


instructions, refer to the manual for the column. Column manuals are
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
3. Fill the reservoirs with prepared eluent or deionized water (if an EG is
installed).
4. Locate the end-line filters (P/N 045987) provided in the pump ship kit:

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water to remove any loose
particles.
5. Install an end-line filter on the end of each reservoir’s eluent line.
6. Install the reservoir caps, making sure the end of each line extends to the
bottom of the reservoir, and that each filter is submerged in liquid. This
prevents air from being drawn through the eluent lines. Hand-tighten the
caps.

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NOTE A High-Pressure Inline Filter (P/N 044105) can be


used to remove particulates down to 0.45 micron from
eluent. Connect the inline filter between the pump out-
let and the eluent inlet port on the injection valve. For
details, see the instructions provided with the inline
filter.

4.7 Setting Up the Piston Seal Wash System


Replumbing the Seal Wash System (DP only) (Optional)

The standard piston seal wash system is designed for use with only one of the
two pumps in a DP module. When the DP is shipped from Thermo Fisher
Scientific, the seal wash system is connected to pump 1 (the bottom pump). If
you want to connect the seal wash system to pump 2 (the top pump), follow
the instructions in this section.

NOTE For users who need to operate a piston seal wash system for
both pumps in the DP, Thermo Fisher Scientific offers an
External Seal Wash Kit (P/N 063518) or a second seal wash
system (P/N 068661).

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4 • DP/SP Startup

1. Note the tubing connected from the peristaltic pump to the seal wash tube
on the secondary pump head on pump 1 (see Figure 4-5, item 1 ).
Disconnect this tubing from the pump head and connect it to the seal wash
tube on the secondary pump head on pump 2.

Connection from
peristaltic pump to
1 secondary pump
head

Connection between
4 2 pump heads

Seal Wash Reservoir


1 3 Inlet Line
2
3

Seal Wash Reservoir


4
Outlet Line

Figure 4-5. Piston Seal Wash Connections to Pump 1

2. Disconnect the short piece of tubing between the primary and secondary
pump heads on pump 1 (see Figure 4-5, item 2 ). Connect this tubing to
the pump heads on pump 2.
3. Disconnect the seal wash reservoir inlet line from the primary pump head
on pump 1 (see Figure 4-5, item 3 ). Connect the inlet line to the primary
pump head on pump 2.
4. When you finish these connections, go to the next section to continue
setting up the seal wash system.

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Setting Up the Seal Wash System (All pumps)

1. Add ASTM Type I (18 megohm-cm) filtered and deionized water that
meets the specifications listed in Section 1.5 to the seal wash reservoir
(P/N 064155).
The liquid level should be between the Min. and Max. markers on the
reservoir label. Do not overfill the reservoir.
2. Place the cap on the reservoir and tighten fingertight.
3. Insert the reservoir into the holder on the component panel.
4. Check that the tubing is engaged in the peristaltic pump (see Figure 4-6).
If it is not, lift the lever on the peristaltic pump up and to the right, insert
the tubing neatly between the lever and the rotor, and release the lever to
secure the tubing.

Tubing to
Secondary
Pump Head Lever

Outlet Tubing
from Seal Wash
Reservoir

Rotor

Figure 4-6. Peristaltic Pump

5. Follow these steps to activate the piston seal wash function:


a. Open the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset.
b. Press the F8 key to open the Commands dialog box.
c. Select the pump name.
d. For Chromeleon 7, click the Properties tab on the right pane of the
dialog box. For Chromeleon 6.8, scroll through the list of commands
and properties under the pump name.

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4 • DP/SP Startup

e. Select the RearSealWashSystem property and select the Interval


option.
f. For Chromeleon 6.8, click the Execute button.

4.8 Starting the Pump


1. Press the POWER button on the front of the DP/SP.
2. If any of the following conditions applies, prime the pump (see
Section 9.5) before proceeding:
• The eluent has been changed.
• The eluent line is new (empty).
• The eluent line contains air.
3. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the Pump tab to display the Pump panel (see Figure 4-7).

Enter a new flow rate


or click the switch to
start the pump at the
selected flow rate.

Enter the maximum


and minimum
pressure limits.

Figure 4-7. Setting the Pump Flow Rate and Pressure Limits
(Chromeleon 7 Version Shown)

4. Enter the Flow rate required for your application. This starts the pump
flow, also.

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5. If the preferred flow rate is already selected, but the pump flow is off,
click the switch to start the pump at the selected flow rate.

NOTE After starting the pump or changing the flow rate, wait
at least 5 minutes (longer for flow rates below
1.0 mL/min) before beginning an analysis. This allows
the DP/SP to stabilize the flow rate.

6. Enter the minimum and maximum pressure limits. Setting pressure limits
ensures that the DP/SP will automatically stop if a system malfunction
occurs. Table 4-1 lists the default pressure limits for capillary and
analytical pumps.

Pump Configuration Default Low Default High


Pressure Limit Pressure Limit
Capillary pump not linked 0 41 MPa (6000 psi)a
to an EGC
Capillary pump linked to an 1.4 MPa (200 psi) 35 MPa (5000 psi)b
EGC
Analytical pump not linked 0 35 MPa (5000 psi)
to an EGC
Analytical pump linked to 1.4 MPa (200 psi) 21 MPa (3000 psi)
an EGC

Table 4-1. Default Pressure Limits for DP/SP Pumps


a. Capillary IC pumps shipped before February 17, 2011 were rated for lower
operating pressures than the pumps currently being shipped. Refer to the im-
portant note on the next page for details.
b. If the installed version of EG degas (capillary) cartridge is not rated for
35 MPa (5000 psi), change the default high pressure limit to 21 MPa
(3000 psi). Refer to the important note on the next page for details.

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Capillary IMPORTANT
IC
Capillary IC pumps shipped before February 17, 2011 were rated for lower
operating pressures than the pumps currently being shipped. The older
pumps can be operated at pressures up to 35 MPa (5000 psi) (without
RFIC) and up to 21 MPa (3000 psi) (with RFIC). Before operating at
pressures above these limits, verify that you have the appropriate pump.
• HPC is stamped on the secondary
pump heads of the older (lower
pressure rated) capillary IC pumps.

• HPC-2 is stamped on the secondary


pump heads of the newer (higher
pressure rated) capillary IC pumps.

A Capillary Pump High Pressure Upgrade Kit (P/N 075994) is available for
converting a lower pressure rated capillary IC pump to a higher pressure
rated pump.

IMPORTANT

If your system includes a capillary pump linked to an


EGC, check the label on the EG degas (capillary)
cartridge in the IC Cube and verify that 5000 psi is
printed on the label (see the figure on the right).
If 5000 psi is not on the label, you must change the high 5000 psi
pressure limit to 21 MPa (3000 psi) or replace the
cartridge with an EG degas (capillary) cartridge that is
rated for 35 MPa (5000 psi) (P/N 074459).
P/N 074459

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EG EG Startup

4.9 Entering the Eluent Concentration


1. Press the POWER button on the front of the EG.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the EG tab to display the EG panel (see Figure 4-8).

Figure 4-8. Example EG Panel (Chromeleon 7 Version Shown)

3. Enter a value in the Target Concentration box. For help in selecting an


eluent concentration, see Section 4.10.
If the pump flow is on, entering a new Target Concentration value
automatically turns on the power to the EGC, also.
4. If the pump flow is off, first turn on the flow and then click the switch
under EG1 Control (or EG2 Control). This turns on the power to the
EGC at the selected Target Concentration value.
5. If the CR-TC switch is off, click the switch to turn on the power to the
CR-TC.

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4.10 Selecting an Eluent Concentration


The allowable eluent concentration depends on several factors: the flow rate,
suppressor type, EGC type, and cartridge configuration. For details, refer to
Table 4-2 and Table 4-3.

Single-Cartridge or Independent Dual-Cartridge Configuration

In the single-cartridge configuration, the EG contains one EGC. In the


independent dual-cartridge configuration, the EG contains two EGCs
operating independently on separate systems (each cartridge is linked to a
different DP/SP). For details, refer to the EGC manual. Cartridge manuals are
included on the Thermo Scientific Reference Library DVD (P/N 053891).

EGC Eluent Concentration Range


KOH (Capillary) 0.1 to 200 mM at 0.001 to 0.010 mL/min flow
0.1 to X mM at 0.010 to 0.030 mL/min
where X = 2/flow
MSA (Capillary) 0.1 to 200 mM at 0.001 to 0.010 mL/min flow
0.1 to X mM at 0.010 to 0.030 mL/min
where X = 2/flow
K2CO3 0.1 to 15 mM at 0.1 to 1.0 mL/min flow
0.1 to X mM at 1.0 to 2.0 mL/min flow
where X = 15/flow
KOH 0.1 to 100 mM at 0.1 to1.0 mL/min flow
0.1 to X mM at 1.0 to 3.0 mL/min flow
where X = 100/flow
LiOH 0.1 to 80 mM at 0.1 to  1.0 mL/min flow
0.1 to X mM at 1.0 to 3.0 mL/min flow
where X = 80/flow
MSA 0.1 to 100 mM at 0.1 to 1.0 mL/min flow
0.1 to X mM at 1.0 to 3.0 mL/min flow
where X = 100/flow
NaOH 0.1 to 100 mM at 0.1 to 1.0 mL/min flow
0.1 to X mM at 1.0 to 3.0 mL/min flow
where X = 100/flow

Table 4-2. Eluent Concentration Ranges for Single-Cartridge and


Independent Dual-Cartridge Configurations

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4 • EG Startup

Linked Dual-Cartridge Configuration

In the linked dual-cartridge configuration, the EG contains two EGCs, linked


to a single pump. Note that the allowable eluent concentration for a linked
cartridge is less than when the cartridge is defined as independent. For details,
refer to the EGC manual. EGC manuals are included on the Thermo Scientific
Reference Library DVD (P/N 053891).

EGCs Eluent Concentration Range Comment


K2CO3/EPM 0.1 to 15 mM at 0.1 to 1.0 ml/min The total of the eluent
Electrolytic pH flow concentrations from
Modifier 0.1 to X mM at 1.0 to 2.0 ml/min both cartridges
flow (K2CO3 and EPM)
where X = 15/flow must not exceed the
specified range. The
EPM concentration
must not exceed
10 mM. See the notes
below for additional
information.
KOH/KOH 0.1 to 50 mM at 0.1 to1.0 mL/min The eluent
KOH/MSA flow concentration range
KOH/NaOH 0.1 to X mM at 1.0 to3.0 mL/min for each cartridge is
MSA/MSA flow 50% of the range for
MSA/NaOH where X = 50/flow an independent
NaOH/NaOH cartridge
LiOH/LiOH 0.1 to 40 mM at 0.1 to1.0 mL/min The eluent
flow concentration range
0.1 to X mM at 1.0 to3.0 mL/min for each cartridge is
flow 50% of the range for
where X = 40/flow an single-independent
cartridge.
KOH (Capillary)/ 0.1 to 100 mM at 0.001 to The eluent
MSA (Capillary) 0.01 mL/min concentration range
0.1 to X mM at 0.01 to 0.1mL/min for each cartridge is
where X = 1/flow 50% of the range for
an independent
cartridge.

Table 4-3. Eluent Concentration Ranges for


Linked Dual-Cartridge Configurations

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Notes for Generating Carbonate/Bicarbonate Eluent

If an EGC III K2CO3 and an EPM III Electrolytic pH Modifier are installed
(EGC_1 and EGC_2, respectively):
1. Set EGC_1 Target Concentration to the concentration of K2CO3
required for your application
2. Set EGC_2 Target Concentration to the concentration of KHCO3
required.
The K2CO3 cartridge generates the total of the two target concentrations and
the EPM modifies the total to achieve the K2CO3/KHCO3 eluent mixture that
you require.
For example:
For a 3.50 mM K2CO3/1.00 mM KHCO3 eluent, set EGC_1 to 3.50 mM and
EGC_2 to 1.00 mM.
The K2CO3 cartridge generates 4.50 mM K2CO3 (indicated in the Applied
Concentration field for the K2CO3 EGC). The EPM modifies the 4.50 mM
K2CO3 eluent to achieve the required 3.50 mM K2CO3/1.00 mM KHCO3
mixture.

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ICS-5000
DC DC Startup

4.11 Starting the DC


1. Press the POWER button on the front of the DC.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the DC tab to display the DC panel (see Figure 4-9).

Figure 4-9. DC Control Panel (Chromeleon 7 Version Shown)

3. For each of the following temperature control devices installed in the


DC—Compartment, Column, Reaction Coil, IC Cube—enter the
preferred Set temperature. This turns on the device, also.
If the preferred temperature is already selected but the device is off, click
the corresponding switch to turn on the device.

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4. If a suppressor is installed: Under Suppressor 1 (or Suppressor 2), select


the suppressor Type, set the Mode to On, and enter the Current required
for your application.
5. If a CD is installed: Click the CD tab to open the CD panel.
6. Under Cell Heater, set the Cell Heater Mode to On and enter the Cell
Heater Set Point.

4.12 Equilibrating the System and Verifying Operational


Readiness
NOTE You can also use the Smart Startup feature in Chromeleon to
automate system startup and equilibration. Refer to the
Chromeleon Help for details.

1. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, verify


that each device listed below (if installed in your system) is turned on and
the selected setting for the device (flow rate, eluent concentration,
temperature, and so on) is correct for your application:
• Pump
• EGC
• CR-TC
• EPM
• Suppressor
• Temperature control devices (DC compartment, DC column
compartment, IC Cube, CD cell heater, reaction coil heater)
2. Click Monitor Background on the toolbar above the Chromeleon 7
ePanel Set or on the Home panel of the Chromeleon 6.8 panel tabset.
Chromeleon begins plotting the detector signal and pump pressure
readings.
3. View the detector signal and monitor the background. Refer to the column
manual for the appropriate background for your application. The column
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).

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4 • DC Startup

4. Offset the detector background and zero the reading by clicking the
Autozero button.
5. Verify that the detector baseline is at the expected reading for your
application and is stable. See Section 8.11 for troubleshooting
information if the reading is too high. See Section 8.2 for troubleshooting
information if the baseline is drifting or is excessively “noisy” (there are
large fluctuations in readings).
6. Monitor the DP/SP pressure and make sure it is at the expected reading
for the installed column and it is stable.
7. Verify that all installed temperature control devices are at their set points
and are stable.
The system is now ready for operation.
Capillary Because capillary IC systems use low flow rates and consume very little
IC eluent, you can leave a capillary IC system on at all times, allowing it to
remain equilibrated and always ready to run the next sample.

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TC TC Startup

4.13 Starting the TC


1. Press the POWER button on the front of the TC.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the TC tab to display the TC panel (see Figure 4-10).

Figure 4-10. TC Panel (Chromeleon 7 Version Shown)

3. Click the Oven switch (Chromeleon 7) or the Oven on button


(Chromeleon 6.8) to turn on the oven.
4. Set the temperature required for the application.

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4.14 Equilibrating the System and Verifying Operational


Readiness
NOTE You can also use the Smart Startup feature in Chromeleon to
automate system startup and equilibration. Refer to the
Chromeleon Help for details.

1. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, verify


that the TC temperature is at its set point and is stable.
2. Monitor the pump pressure; make sure it is at the expected reading for the
installed column and is stable.
3. Verify that the detector baseline is at the expected reading for your
application and is stable.
The system is now ready for operation.

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5 • Operation

5.1 Controlling Modules Directly


When the Thermo Scientific Dionex ICS-5000 Ion Chromatography System
is not running automated analyses, you can directly control the system
modules by issuing commands from the ePanel Set in Chromeleon 7 or the
panel tabset in Chromeleon 6.8. For example, you can turn on the pump flow,
set the eluent concentration, or set the compartment temperature.

To display the Chromeleon 7 ePanel Set:

1. On the Console, click the Instruments category bar.


2. In the Navigation Pane, click the instrument that you want to control.
Chromeleon 7 connects to the instrument and displays the ePanel Set.

To display the Chromeleon 6.8 panel tabset:

1. Click View > Default Panel Tabset or click the toolbar button .
2. Select the Chromeleon server and click OK.
3. If more than one timebase is configured on the server, Chromeleon 6.8
displays a panel tabset for each timebase. Click the Expand Timebase
View button for the timebase that you want to control.

To issue direct control commands to a module:

1. On the ePanel Set or panel tabset, click the tab for the module.
2. Use the controls (buttons, sliders, etc.) on the panel to issue commands.
3. If the function that you want to perform is not available from the panel,
press the F8 key to open the Commands dialog box. You can access all
commands available for the system from this dialog box.

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5.2 Analyzing Samples


Figure 5-1 shows the basic steps used to
analyze a sample in a chromatography Load the sample
system.
To analyze a sample with a Dionex ICS-
Autozero
5000 system, you add sample injections to a
Chromeleon sequence. The sequence
determines how the group of injections will
Inject the sample
be analyzed and the order in which they will
be run. A sequence typically includes the
following elements:
Start data
• A predefined list of commands and acquisition
parameters for controlling Dionex ICS-
5000 modules and acquiring sample
Stop data
data (called an instrument method in acquisition
Chromeleon 7 or a program in
Chromeleon 6.8).
Evaluate
• The chromatographic data acquired for sample data
each injection.

Figure 5-1. Sample Analysis Overview

• A predefined set of instructions for evaluating the acquired data (called a


processing method in Chromeleon 7 or a quantification method in
Chromeleon 6.8).
• Templates for displaying chromatographic data on the screen and for
printing reports.

NOTE A Virtual Column Separation Simulator is available in


Chromeleon that can help you determine the best oper-
ating parameters (column, eluent, flow rate, tempera-
ture) for a particular analysis. Refer to the Chromeleon
Help for details.

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5.2.1 Creating a New Sequence in Chromeleon 7


In Chromeleon 7, two methods are available for creating a new sequence:
eWorkflows and the Sequence Wizard.
• eWorkflows provide predefined templates and rules for creating new
sequences. If they have been defined for your laboratory, eWorkflows are
the preferred method for creating a new sequence.
• If eWorkflows are not available, use the Sequence Wizard.

Using eWorkflows

1. On the Console, click the eWorkflows category bar (see Figure 5-2). In
the Navigation Pane, click the eWorkflow name.
2. In the work area, click the instrument name and then click Launch.

Figure 5-2. eWorkflow View in Chromeleon 7

3. The eWorkflow Wizard opens. Complete the steps in the wizard. For
details about an eWorkflow Wizard page, click the Help icon .

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4. After you finish the eWorkflow Wizard, the sequence is displayed in the
Console Data view (see Figure 5-3).

Figure 5-3. New Sequence in Chromeleon 7

Using the Sequence Wizard

1. On the Console menu bar, click the Create button.


2. The Sequence Wizard opens. Complete the steps in the wizard, specifying
the number of samples and standards that you want, and the instrument
method, processing method, and report template to use. For details about
a wizard page, click the Help icon .

NOTE If preferred, you can create the sequence first and then
specify the methods and report template later. You can
also edit other details of the sequence (for example,
add or remove samples) after you finish the wizard.

3. After you finish the wizard, the new sequence is displayed in the Console
Data view (see Figure 5-3).

5.2.2 Creating a New Sequence in Chromeleon 6.8


In Chromeleon 6.8, two wizards are available to help you create a new
sequence: the Sequence Wizard and the Application Wizard.
• If the program and quantification method have already been created, use
the Sequence Wizard.
• If you want to create a new program and quantification method, in
addition to the sequence, use the Application Wizard.

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5 • Operation

Using the Sequence Wizard

1. On the Sequence Control panel in the Chromeleon 6.8 panel tabset, click
Create Sequence (see Figure 5-4).

Figure 5-4. Sequence Control Panel in Chromeleon 6.8

2. Complete the steps in the Sequence Wizard, specifying the number of


samples and standards that you want and the program and quantitation
method to use. For help at any time, click the Help button on the
Sequence Wizard page.

NOTE If preferred, you can create the sequence first and then
specify the program and quantitation method later.
You can also edit other details of the sequence (for
example, add or remove samples) after you finish the
wizard.

3. After you finish the Sequence Wizard, the new sequence is displayed in
the Chromeleon 6.8 Browser.

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Using the Application Wizard (Chromeleon 6.8 only)

1. Click Application Wizard on the Sequence Control panel (see


Figure 5-4).
2. Select a suppressor type (if used) and then select an application template
from the list.

NOTE Instead of selecting an application template, you can


use the Virtual Column Separation Simulator. Refer to
the Chromeleon 6.8 Help for details.

3. Click Next> and select the in a new sequence via Sequence Wizard
option.
4. Click Next> to go to the Sequence Wizard.
5. Complete the steps in the Sequence Wizard, specifying the number of
samples and standards that you want. For help at any time, click the Help
button on the Sequence Wizard page.
After you finish the Sequence Wizard, a sequence is created and
displayed in the Chromeleon 6.8 Browser. A program and quantification
method appropriate for the selected application are copied to the
sequence.

5.2.3 Starting a Sequence

Starting a Sequence in Chromeleon 7

1. Click Start on the sequence control bar (see Figure 5-5).

Figure 5-5. Starting a New Sequence in Chromeleon 7

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5 • Operation

2. The sequence is appended to the instrument queue and a Ready Check is


performed. If the Ready Check passes and the instrument is not currently
running another sequence, the sequence is started.

Figure 5-6. Running Sequence in Chromeleon 7

Starting a Sequence in Chromeleon 6.8

1. On the Sequence Control panel, click Load Sequence (see Figure 5-7).
2. Select the sequence from the list and click Open. The sequence is added
to the Sequence table.
3. Click Start Batch (see Figure 5-7).

Figure 5-7. Starting a Sequence in Chromeleon 6.8

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5.3 Loading Samples Into the Sample Loop or


Concentrator
Two methods are available for loading samples:
• Loading samples with an autosampler (see Section 5.3.1)
• Loading samples with a syringe through the sample loading ports on the
DC front door (see Section 5.3.2)

5.3.1 Loading Samples with an Autosampler


1. Verify that the autosampler output line is connected to the sample port on
the DC (or TC) injection valve. Direct the waste line as required for this
autosampler model.
2. Prepare and fill the sample vials and place them in the autosampler tray or
carousel. Refer to the autosampler manual for detailed instructions.
Autosampler manuals are provided on the Thermo Scientific Reference
Library DVD (P/N 053891).
3. Create a sequence in Chromeleon that specifies the vials from which to
take sample injections and the order in which the injections should be run.
4. Specify a Chromeleon 7 instrument method or Chromeleon 6.8 program
that includes the appropriate load and inject commands for the
autosampler. See the examples in Section 5.4.

5.3.2 Loading Samples with a Syringe


This section describes two methods for using a syringe to load sample into the
DC injection valve sample loop:
• Loading sample with a syringe through the sample loading port on the
front of the DC (push method)
• Loading sample with a vacuum syringe through the sample loading port
on the front of the DC (pull method)

Loading Samples with a Syringe (Push Method)

1. Verify that a luer adapter fitting is installed on the sample loading port on
the front of the DC and that tubing is connecting the sample loading port

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5 • Operation

to the sample port on the injection valve. If not, refer to Section 9.20 for
connection instructions.
2. Fill a syringe with a calibration standard or sample.
3. Insert the syringe into the sample loading port on the front of the DC.
4. Verify that the injection valve is in the Load position. If it is not, switch
the valve by clicking the valve control on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset, or by pressing the VALVE button on the
front of the DC.
5. Overfill the sample loop with several sample loop volumes. Excess
sample will exit through the injection valve waste line.
6. Leave the syringe in the port. This prevents the sample from exiting the
loop before injection.
7. Switch the injection valve to the Inject position.

5.3.3 Loading Samples with a Vacuum Syringe (Pull Method)


1. Verify that a luer adapter fitting is installed on the sample loading port on
the front of the DC and that tubing is connecting the sample loading port
and the injection valve. If this is not the case, refer to Section 9.20 for
connection instructions.
2. Disconnect the waste line from the injection valve and replace it with a 25
to 30 cm (10 to 12 in) piece of PEEK or PTFE tubing (see Figure 5-8).
3. Place the free end of the line into the sample.
4. Verify that the injection valve is in the Load position. If it is not, switch
the valve by clicking the valve control on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset, or by pressing the VALVE button on the
front of the DC.
5. Insert a 5 cc syringe into the sample loading port on the DC front door
(see Figure 5-8) and pull out the plunger to draw the sample into the
injection valve.

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6. Switch the injection valve to the Inject position.

Sample Port
g e
Syrin

(5) S L (4) Guard

W C
(6) (3)

(1) L P (2)

Valve

Sample

Figure 5-8. Loading Sample with a Vacuum Syringe (Pull Method)

5.4 Autosampler Commands for Loading and Injecting


Samples
Commands for loading and injecting a sample using an autosampler are
included in a Chromeleon 7 instrument method or Chromeleon 6.8 program.
When you create an instrument method or program with the Chromeleon
software wizard, the specific autosampler commands required for your model
of autosampler and the type of injection to be performed are added
automatically.
An Inject command to switch the injection valve to the Inject position is
always included. The Inject command occurs at time 0.00. This is when the
sample enters the high-pressure side of the system and defines the beginning
of a chromatogram. Wait commands to pause the instrument method or
program while the autosampler is performing the injection are also included.
For Dionex AS-DV and AS autosamplers, a Load command is required to
switch the injection valve to the Load position. A separate Load command is
not needed for the Dionex AS-AP.

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5 • Operation

Figure 5-9 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS-AP Autosampler.

Figure 5-9. Commands for Loading and Injecting a Sample with a Dionex
AS-AP (Chromeleon 7 Script Editor Shown)

Figure 5-10 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS-DV Autosampler.

Figure 5-10. Commands for Loading and Injecting Sample with a Dionex
AS-DV (Chromeleon 7 Script Editor Shown)

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Figure 5-11 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS Autosampler.

Figure 5-11. Commands for Loading and Injecting a Sample with a Dionex
AS (Chromeleon 7 Script Editor Shown)

For details about controlling an autosampler, refer to the operator’s manual


for your autosampler. The manuals are provided on the Thermo Scientific
Reference Library DVD (P/N 053891).

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6 • Shutdown

ICS-5000
DP/SP DP/SP Shutdown
If the Dionex ICS-5000 Dual Pump (DP) or Dionex ICS-5000 Single Pump
(SP) will not be operated for a period of one week or more, follow the
instructions below:
• Fill the pump with methanol (or a similar alcohol, such as 2-propanol or
ethanol). If the eluents in the pump are not miscible with water, replace
the eluents step-by-step.
• Fill the seal wash reservoir with wash solution (see Section 2.2.5).
• Rinse out buffers. This will reduce the time required for column
equilibration when you resume operation.
• Disconnect the tubing from the peristaltic pump on the component panel:
lift the lever up and to the right, remove the tubing, and release the lever
(see Figure 6-1).

Tubing

Rotor

Lever

Figure 6-1. Peristaltic Pump for Seal Wash System

Before shipping the pump:

• Empty the seal wash reservoir.


• Disconnect the tubing from the peristaltic pump on the component panel:
press the lever to the right, remove the tubing, and release the lever (see
Figure 6-1).

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ICS-5000
EG EG Shutdown

6.1 Short-term Shutdown


If the shutdown is for 3 months or less, follow the instructions below.
To prepare the EG for the shutdown:
1. Turn off the EG, including all consumables installed in the EG (the CR-
TC, suppressor, etc.).
2. Verify that the current to the EGC and the suppressor is off.
Supplying power to the EGC when there is no eluent flow can severely
damage the cartridge.

3. Store the EGC in the EG during the shutdown.


To restart the EG:
1. Select the parameters for the analysis on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset. For EG startup information, see
Section 4.9.
2. In an analytical IC system, if the EG has been shut down for more than 3
to 4 days, hydrate the suppressor as instructed in the product manual.
Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).
3. Let the system equilibrate before collecting data.

6.2 Long-term Shutdown


If the shutdown is for 3 months or more, follow the instructions below.
To prepare the EG for the shutdown:
1. Turn off the EG, including all consumables installed in the EG (the CR-
TC, suppressor, etc.).

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2. Verify that the current to the EGC and the suppressor is off.
Supplying power to the EGC when there is no eluent flow can severely
damage the cartridge.

3. If you plan to store the EGC in the EG, no further action is required.
If you plan to store the cartridge outside the EG (for example, in the
original shipping container), follow the instructions in Section 9.14.1, to
remove the EGC from the EG, and the instructions in Section 9.14.3, to
store the EGC.
To restart the EG:
1. Select the parameters for the analysis on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset. For EG startup information, see
Section 4.9.
2. Condition the EGC. For instructions, see “Conditioning the Capillary
EGC” on page 343 or “Conditioning the Analytical EGC” on page 348.
3. Hydrate the CR-TC (see “Installing and Flushing the New CR-TC” on
page 350).
4. Hydrate the suppressor as instructed in the product manual. Suppressor
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).
5. Let the system equilibrate before collecting data.

Before shipping the EG:

1. Follow the instructions in Section 9.14.1, to remove the EGC from the
EG.
2. Plug all fittings. Tighten the vent fitting (capillary EGC) or cap the vent
port (analytical EGC). This will prevent the evaporation of water in the
electrolyte reservoir.
Make sure the EGC packaging conforms to hazardous material
shipping requirements. Refer to the Material Safety Data Sheet (MSDS)
shipped with the EGC for the chemical description.

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ICS-5000
DC DC Shutdown

6.3 Consumables Storage


The columns, suppressors, and other consumable items used with a Dionex
ICS-5000 system have various short- and long-term storage requirements.
Refer to the manuals for the individual products for instructions. These
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).

6.4 ED Cell Storage

6.4.1 Short-term Storage of the ED Cell


If the cell will not be used for a short period of time (less than 2 days),
disconnect the tubing from the inlet and outlet fittings and all fitting plugs.

NOTE If the pH-Ag/AgCl reference electrode remains in the cell but


eluent is not being pumped through the cell, the pH-Ag/AgCl
reference electrode frit may partially dry out. If this occurs,
regenerate the electrode by soaking it in a solution containing
1 M KCl and 1 M HCl.

6.4.2 Long-term Storage of the pH-Ag/AgCl Reference Electrode


If the cell will not be used for 2 days or more, remove the pH-Ag/AgCl
reference electrode and store it in a solution of saturated KCl, as instructed in
the procedure below.
1. Prepare a saturated solution of KCl in ASTM filtered, Type I
(18 megohm-cm) deionized water that meets the specifications listed in
Section 1.5.
2. Locate the cap in which the electrode was shipped and fill it two-thirds
full with the prepared KCl solution.
3. Remove the pH-Ag/AgCl reference electrode from the cell.
4. Insert the electrode into the cap and screw on the cap (see Figure 6-2).

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5. Make sure there is no air bubble in the cap. Add more KCl solution if
needed.

Storage
Cap

Figure 6-2. pH-Ag/AgCl Reference Electrode in Storage Cap

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ICS-5000
TC TC Shutdown

6.5 Consumables Storage


The columns and other consumable items used with a Dionex ICS-5000
system have various short- and long-term storage requirements. Refer to the
manuals for the individual products for instructions. These manuals are
provided on the Thermo Scientific Reference Library DVD (P/N 053891).

6.6 Short-term Shutdown


Before a TC shutdown of less than one week, no special procedure is
required.

6.7 Long-term Shutdown


Before interrupting TC operation for more than one week or before shipping
the TC, rinse the fluid connections with deionized water.

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7 • Maintenance

This section describes routine maintenance procedures for the Dionex ICS-
5000 system that users may perform. All other maintenance procedures must
be performed by Thermo Fisher Scientific personnel.
For information about maintenance procedures for the EGC, CR-TC trap
column, or suppressor, refer to the appropriate product manual. These
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).

7.1 System Maintenance Checklists

7.1.1 Daily Maintenance


 Check for leaks.
 Wipe up liquid spills.
 Check eluent reservoirs for microbial growth; clean reservoirs and replace
eluent as needed.
 Check eluent reservoir levels and refill as needed.
 Check waste containers and empty as needed.
For detailed daily maintenance instructions for each module, see:

DP/SP page 195


EG page 197
DC page 199
TC page 201

7.1.2 Weekly Maintenance


 Check end-line filters on eluent lines. When end-line filters are new, they
are pure white. Replace filters if they become discolored, if bacterial

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buildup is evident, or if eluent flow is blocked. See Section 4.6 for


instructions.
 Check for plugged or blocked tubing connections.
Capillary  Check eluent reservoir levels and refill as needed.
IC
Capillary  Check waste containers and empty as needed.
IC
For detailed weekly maintenance instructions for each module, see:
DP/SP page 195
EG page 197
DC page 199
TC page 201

7.1.3 Periodic Maintenance


 Clean eluent reservoirs (when making fresh eluent or as needed) (see
Section 9.4).
 (Optional) Have Thermo Fisher Scientific perform the performance
qualification (PQ) procedure for IC systems.
For detailed periodic maintenance instructions for each module, see:
DP/SP page 196
DC page 199
TC page 201

NOTE There are no periodic maintenance instructions for the EG.

7.1.4 Annual Maintenance


 Thermo Fisher Scientific recommends performing preventive
maintenance on each module annually. Preventive Maintenance Kits
contain all the required parts for these procedures. The following kits are
available:
DP/SP Preventive Maintenance Kits
• ICS-5000 Analytical Pump Preventive Maintenance Kit
(P/N 075038)

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7 • Maintenance

• ICS-5000 Capillary Pump Preventive Maintenance Kit (P/N 075039)


DC/TC Preventive Maintenance Kits
• 0.4 L Internal Loop High-Pressure Valve Preventive Maintenance
Kit (P/N 075040)
• 6-Port High-Pressure Valve Preventive Maintenance Kit
(P/N 075041)
• 10-Port High-Pressure Valve Preventive Maintenance Kit
(P/N 075042)

NOTE There is no Preventive Maintenance Kit for the EG.

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ICS-5000
DP/SP DP/SP Routine Maintenance

This section describes routine maintenance procedures that users may perform
for the Dionex ICS-5000 Dual Pump (DP) or Dionex ICS-5000 Single Pump
(SP). All other maintenance procedures must be performed by Thermo Fisher
Scientific personnel.

7.2 DP/SP Daily Maintenance


• Check for leaks at the following locations: the eluent proportioning valves
(gradient pump only), vacuum degas chambers, and eluent reservoirs.
Tighten or replace any leaking fittings.
• Wipe up liquid spills and rinse dried reagents off pump components with
deionized water. Dry the leak sensor thoroughly; if the sensor is not dry, it
will remain activated and continue to report a leak to the Audit Trail.
• Check the liquid level in the seal wash reservoir. The liquid level should
remain between the Min. and Max. markers on the reservoir label.
• Check eluent reservoirs for microbial growth; clean reservoirs and replace
eluent as needed. Rinse each eluent reservoir thoroughly (inside and out)
with ASTM filtered, Type I (18 megohm-cm) deionized water that meets
the specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, clean the reservoir as instructed in Section 9.4.
• Check the liquid level in each eluent reservoir and refill as required.

7.3 DP/SP Weekly Maintenance


• The end-line filters (P/N 045987) on the eluent lines may need to be
replaced weekly, depending on water quality and eluent conditions. For
example, replace the filters weekly when using an EGC to generate
carbonate/bicarbonate eluent.
When the end-line filters are new, they are pure white. Replace the filters
whenever they become discolored, if bacterial buildup is evident, or if
eluent flow is blocked.

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NOTE It is especially important to regularly replace end-line


filters when using aqueous eluents. Aqueous eluents
may contaminate the filters with bacteria or algae,
causing cause flow restrictions to the pump.
End-line filters are provided in the pump ship kit.

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5 to remove any loose particles.
• Replace the seal wash solution. ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5 is
appropriate for most applications.
• Check the tubing connected to the peristaltic pump. If the tubing is
blocked or crimped, replace it (see Section 9.9).
Capillary • Check the liquid level in each eluent reservoir and refill as required.
IC

7.4 DP/SP Periodic Maintenance


• Make fresh eluent as needed.
• Replace piston seals every 6 to 12 months (see Section 9.7).
Capillary • Clean eluent reservoirs every 3 months with methanol or isopropyl
IC alcohol, as instructed in Section 9.4.

7.5 DP/SP Annual Maintenance


Thermo Fisher Scientific recommends performing preventive maintenance
annually. The following kits are available:
• ICS-5000 Analytical Pump Preventive Maintenance Kit (P/N 075038)
• ICS-5000 Capillary Pump Preventive Maintenance Kit (P/N 075039)

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ICS-5000
EG EG Routine Maintenance

This section describes routine maintenance procedures for the Dionex ICS-
5000 Eluent Generator (EG) that users may perform. All other maintenance
procedures must be performed by Thermo Fisher Scientific personnel.
For information about maintenance procedures for the EGC, CR-TC trap
column, or suppressor, refer to the appropriate product manual. These
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).

7.6 EG Daily Maintenance


• Locate and repair leaks inside the EG (see Section 9.13) and wipe up
liquid. Rinse dried eluents off components with deionized water.
• Rinse the EG drip tray with deionized water (to prevent formation of salt
crystals) and dry the drip tray thoroughly. Rinse and dry the leak sensor,
also; if the sensor is not dry, it will remain activated and continue to report
a leak to the Audit Trail.
• Check the waste container and empty as needed.

7.7 EG Weekly Maintenance


• Check all lines for crimping. Move (or reroute) pinched lines and replace
damaged lines (see Section 9.12). For help in isolating the cause of a
tubing restriction, see Section 9.13.
• Monitor the system backpressure. A gradual increase in backpressure can
indicate clogging of the EGC inlet frit from particulates in the eluent
water.

7.8 EG Annual Maintenance


• Check the expiration date and remaining lifetime of the EGC on the EG
ePanel in Chromeleon 7 or the Control panel in Chromeleon 6.8.

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ICS-5000
DC DC Routine Maintenance

This section describes routine maintenance procedures for the Dionex ICS-
5000 Detector/Chromatography Module (DC) that users may perform. All
other maintenance procedures must be performed by Thermo Fisher Scientific
personnel.

7.9 DC Daily Maintenance


• Check the DC components for leaks or spills. Wipe up spills. Isolate and
repair leaks (see Section 8.26). Rinse off any dried eluent with ASTM
filtered, Type I (18 megohm-cm) deionized water that meets the
specifications listed in Section 1.5.
• Check the waste container and empty as needed.

NOTE If you are using an electrochemical detector, also see the spe-
cial maintenance considerations that are described in
Section 4.1.2.

7.10 DC Weekly Maintenance


• Check liquid lines for crimping or discoloration. Relocate any pinched
lines. Replace damaged lines.
• Check for excess condensation inside the DC. Condensation may build up
when the DC is operated in a highly humid environment and the majority
of the applications are run at cold temperatures. To remove condensation,
run the DC at its maximum temperature for at least 48 hours.

7.11 DC Periodic Maintenance


• Inspect the door seal for signs of damage. A defective seal impairs the
performance of the instrument. If the seal is defective, contact Technical
Support for Dionex products.

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7.12 DC Annual Maintenance


Thermo Fisher Scientific recommends performing preventive maintenance
annually. The following kits are available:
• 0.4 L Internal Loop High-Pressure Valve Preventive Maintenance Kit
(P/N 075040)
• 6-Port High-Pressure Valve Preventive Maintenance Kit (P/N 075041)
• 10-Port High-Pressure Valve Preventive Maintenance Kit (P/N 075042)

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ICS-5000
TC TC Routine Maintenance

This section describes routine maintenance procedures for the Dionex ICS-
5000 Thermal Compartment (TC) that users may perform. All other
maintenance procedures must be performed by Thermo Fisher Scientific
personnel.

7.13 TC Daily Maintenance


• Check the TC components for leaks or spills. Wipe up spills. Isolate and
repair leaks (see Section 8.31). Rinse off any dried eluent with ASTM
filtered, Type I (18 megohm-cm) deionized water that meets the
specifications listed in Section 1.5.
• Check the liquid level in the waste container and empty as needed.

Neutralize acidic and caustic wastes before disposal. Dispose of all


wastes in accordance with local regulations.

Neutralisez les déchets acides ou caustiques avant de les jeter. Jetez


les déchets aux règlements locaux.

Neutralisieren Sie säurehaltige und ätzende Abfälle vor ihrer


Entsorgung. Entsorgen Sie alle Abfälle entsprechend den lokalen
Bestimmungen.

7.14 TC Weekly Maintenance


• Check liquid lines for crimping or discoloration. Relocate any pinched
lines. Replace damaged lines.

7.15 TC Periodic Maintenance


• Clean the interior of the TC, using a lint-free cloth. Use paper to absorb
any liquid inside the module. The cleaner the module, the more effective
the sensors are at detecting excessive gas or humidity.

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• Check for excess condensation inside the TC. Condensation may build up
when the TC is operated in a highly humid environment and the majority
of applications are run at cold temperatures. To remove condensation, run
the TC at its maximum temperature for at least 72 hours.
Some IC columns should not be operated at temperatures above 70 °C
(158 °F). Remove all columns from the TC before beginning the
maintenance procedure above.

• Inspect the door seal for signs of damage. A defective seal impairs the
performance of the instrument. If the seal is defective, contact Technical
Support for Dionex products.

7.16 TC Annual Maintenance


• Thermo Fisher Scientific recommends performing preventive
maintenance annually. The following kits are available:
• 6-Port High-Pressure Valve Preventive Maintenance Kit
(P/N 075041)
• 10-Port High-Pressure Valve Preventive Maintenance Kit
(P/N 075042)

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8 • Troubleshooting

This chapter is a guide to troubleshooting minor issues that may arise during
operation of the Dionex ICS-5000 system. Turn to the section of this chapter
that best describes the operating problem or symptom that has been observed.
Each section lists possible causes of the problem or symptom in order of
probability. A systematic troubleshooting approach is the most effective way
to determine the root cause.
If you are unable to resolve a problem by following the instructions here,
contact Technical Support for Dionex products. In the U.S. and Canada, call
1-800-346-6390. Outside the U.S. and Canada, call the nearest Thermo Fisher
Scientific office. Please have this chapter at hand when talking with Technical
Support personnel.

8.1 Audit Trail Error Messages


The instrument control firmware installed in each Dionex ICS-5000 module
periodically checks the status of certain parameters. If a problem is detected,
it is reported to Chromeleon and logged in the Audit Trail. Each error
message is preceded by an icon that identifies the seriousness of the
underlying problem (see the table below). For most modules (except for the
TC), you can change the severity level assigned to a problem whenever
appropriate.

Icon Default Description


Severity Level
Warning A message is displayed in the Audit Trail, but
the current run is not interrupted.
Error A message is displayed in the Audit Trail, and
the system attempts to correct the problem
(sometimes by using an alternative parameter).
An Error never interrupts the current analysis;
however, if it occurs during the Ready Check,
the analysis will not be started.
Abort A message is displayed in the Audit Trail, and
the running batch is aborted.

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8.1.1 DP/SP Error Messages


Table 8-1 lists the most frequently observed DP/SP-related error messages
and their default severity levels. For troubleshooting assistance, refer to the
page indicated in the table.

DP/SP-Related Audit Trail Error Message Default See


Severity
Level
A program with this name already exists. Abort page 227
Abnormal drive current for x.x seconds. Warning page 227
Camshaft index too early. Abort page 228
Camshaft index too late. Abort page 228
Camshaft sensor always alight. Abort page 228
Camshaft sensor missing or dark. Abort page 228
Degasser malfunction. Warning page 228
Excessive drive current. Camshaft x.x. Abort page 229
Invalid flow value. Abort page 229
Leak detected. Flow stopped. Abort page 229
Left-hand pump block carryover pressure is too Abort page 230
high.
Motor malfunction. Abort page 230
Motor position error. The motor is overloaded. Abort page 230
Pressure fallen below lower limit. Abort page 231
Relay 4 is configured for inject synchronization. Abort page 232
Please change pump configuration.
Right-hand pump block carryover pressure is Abort page 230
too high.
The maximum purge pressure was exceeded. Abort page 232
The pressure in the left-hand working cylinder Abort page 233
exceeded the safety limit.
The pressure in the right-hand working cylinder Abort page 233
exceeded the safety limit.

Table 8-1. DP/SP Error Messages

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8 • Troubleshooting

DP/SP-Related Audit Trail Error Message Default See


Severity
Level
The system pressure exceeded the safety limit. Abort page 233
This function cannot be adjusted by the user. Abort page 234
Upper pressure limit exceeded. Abort page 234

Table 8-1. DP/SP Error Messages (Continued)

8.1.2 EG Error Messages


Table 8-2 lists the EG-related error messages and their default severity levels.
For troubleshooting assistance, refer to the page indicated in the table.

EG-Related Audit Trail Error Message Default See


Severity
Level
Concentration out of range! The maximum value Error page 241
at time %1 is %2.
Concentration out of range! The maximum value Error page 241
is %1.
CR-TC1 open circuit. Abort page 241
CR-TC2 open circuit.
CR-TC1 over current. Abort page 242
CR-TC2 over current.
CR-TC1 stopped because EGC1 OFF. Abort page 242
CR-TC2 stopped because EGC2 OFF.
CR-TC1 stopped due to zero flow. Abort page 243
CR-TC2 stopped due to zero flow.
The CR-TC mode is off for a virtual pump. Abort page 243
CR-TC mode will be turned off for invalid flow. Abort page 243
Flow range for analytical EGC: 0.100 - 3.000
mL/min, capillary EGC: 0.001 - 0.100 mL/min.
Current linked pump is capillary. Please install a Abort page 244
capillary EGC.

Table 8-2. EG Error Messages

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EG-Related Audit Trail Error Message Default See


Severity
Level
Current linked pump is analytical. Please install Abort page 244
an analytical EGC.
EG1 cartridge disconnected. Abort page 244
EG2 cartridge disconnected.
EG1 invalid activation date. Abort page 245
EG2 invalid activation date.
EG1 invalid concentration. Abort page 245
EG2 invalid concentration.
EG1 invalid flow. Abort page 245
EG2 invalid flow.
EG1 invalid flow rate-concentration. Abort page 246
EG2 invalid flow rate-concentration.
EG1 invalid ion count. Abort page 246
EG2 invalid ion count.
EG1 invalid serial number. Abort page 247
EG2 invalid serial number.
EG1 over current. Abort page 247
EG2 over current.
EG1 over power. Abort page 248
EG2 over power.
EG1 over voltage. Abort page 248
EG2 over voltage.
EG1 wrong cartridge error. Abort page 249
EG2 wrong cartridge error.
The EG mode is off due to pump pressure alarm Abort page 249
or leak.
The EG mode is off for a virtual pump. Warning page 249
EG mode will be turned off for invalid flow. Warning page 249

Table 8-2. EG Error Messages (Continued)

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8 • Troubleshooting

EG-Related Audit Trail Error Message Default See


Severity
Level
EG mode will be turned off for invalid flow. Flow Abort page 250
range for analytical EGC: 0.100 - 3.000 mL/min,
capillary EGC: 0.001 - 0.100 mL/min.
EGC-1 is not linked to a compatible pump. Warning page 250
EGC-2 is not linked to a compatible pump.
EGC cannot be used due to invalid ion count. Abort (can’t page 251
be changed)
EGC is either not installed or invalid cartridge Abort page 251
number. Please install a capillary EGC.
EGC is either not installed or invalid cartridge Abort page 251
number. Please install an analytical EGC.
EGC is either not installed or invalid cartridge Abort page 252
number. Please install an EGC.
Leak sensor wet. Warning page 252
pH modifier must be used with a different type of Error page 252
cartridge.
Pump is disconnected. The EG mode is off. Warning page 253

Table 8-2. EG Error Messages (Continued)

8.1.3 DC Error Messages


Table 8-3 lists the DC-related error messages and their default severity levels.
For troubleshooting assistance, refer to the page indicated in the table.

DC-Related Audit Trail Error Message Default See


Severity
Level
CD cell option disconnected. Abort page 259
CD cell over safe temperature. Abort page 260
Column temperature open circuit. Abort page 260
Column over safe temperature. Abort page 260
Column temperature calibration error. Warning page 261

Table 8-3. DC Error Messages

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DC-Related Audit Trail Error Message Default See


Severity
Level
Compartment temperature open circuit. Abort page 261
Compartment over safe temperature. Abort page 261
Compartment temperature calibration error. Warning page 261
ED cell current exceeds limits error. Warning page 261
ED cell option disconnected. Abort page 262
ED cell working electrode disconnected. Abort page 263
ED pH offset calibration failed. Warning page 263
ED pH slope calibration failed. Warning page 264
ED reference electrode disconnected. Warning page 264
High pressure valve 1 error. Abort page 265
High pressure valve 2 error.
High pressure valve 3 error.
High pressure valve 4 error.
IC Cube 1 heater over safe temperature. Error page 266
IC Cube 2 heater over safe temperature.
Lower door opened. Warning page 267
Lower leak sensor wet. Warning page 267
Reaction coil open circuit. Abort page 267
Reaction coil over safe temperature. Abort page 268
Suppressor over-current. Abort page 268
Suppressor over-power. Abort page 268
Suppressor over-voltage. Abort page 269
Suppressor stopped for flow rate. Warning page 269
Upper door opened. Warning page 269

Table 8-3. DC Error Messages (Continued)

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8 • Troubleshooting

8.1.4 TC Error Messages


Table 8-4 lists the TC-related error messages and their default severity levels.
For troubleshooting assistance, refer to the page indicated in the table.

TC-Related Audit Trail Error Message Default See


Severity
Level
AcqOff without previous AcqOn. Error page 275
Acquisition is still on at program end. Error page 275
All samples scheduled for run on timebases x Error page 275
need to specify the same value for property
(nominal) Temperature.
All samples scheduled for run on timebases x Error page 275
need to specify the same value for property
TempCtrl.
All samples scheduled for run on timebases x Error page 276
need to specify the same value for property y.
Can't execute “Disconnect” command during Warning page 276
data acquisition.
Can't execute “Standby” command during data Warning page 276
acquisition.
Can't find download image TC3000.HEX. Abort page 276
Can't start acquisition at negative retention Error page 277
times.
Can't start acquisition: The server configuration Abort page 277
does not fulfill the license conditions.
Can’t start TC firmware. A firmware download Abort page 277
may be necessary.
Can't use device “x” as a source of the column Error page 278
pressure. Please check the property
“SystemPressure” for a valid device name. The
device must have the “Pressure” property
available.

Table 8-4. TC Error Messages

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TC-Related Audit Trail Error Message Default See


Severity
Level
Can't use device “x” as a source of the column Error page 278
pressure. Please check the property “y” for a
valid device name. The device must have the
“Pressure” property available.
Card data checksum error. Error page 279
Command is not available in demo mode. Abort page 279
Communication error: x. Abort page 279
Communication time-out. Abort page 280
Configuration doesn’t match. X not installed. Warning page 280
Configuration mismatch (x — CM uses y, Abort page 280
Column Compartment uses z). Please use the
Server Configuration program to check the
installation.
Current flow is out of limits defined for the Warning page 280
column.
Current pressure is out of limits defined for the Warning page 281
column.
Current temperature is out of limits defined for Warning page 281
the column.
Data buffer overrun. Abort page 281
Device control feature is not available! Please Abort page 282
check key code and CM Features (see “About
Chromeleon...” in the client's Help menu).
Device is not remote. Abort page 282
Device not found on the USB. Abort page 283
Either the current date is later than the Warning page 283
expiration date for x or the program or batch will
end later than 24 hours before the expiration
time for y.
Error deleting flash memory. Abort page 283
Error during storing of the card data to the chip Error page 284
card.

Table 8-4. TC Error Messages (Continued)

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8 • Troubleshooting

TC-Related Audit Trail Error Message Default See


Severity
Level
Error finishing download. Abort page 277
Error programming flash memory. Abort page 284
Executing this command will reset associated Warning page 284
counter values stored in the module.
Firmware download failed. Abort page 285
Firmware download in progress. Please wait. Error page 285
Gas leak detected. Error page 285
Humidity leak detected. Error page 285
Illegal parameter. Abort page 286
Invalid date/time format. Either use “DD MMM Error page 286
YYYY” or “current [ + [Nyear[s]] [Nmonth[s]]
[Nday[s]]].” Examples: “31 Dec 1999,” “current +
1year 6months.”
Invalid enumerated value. Warning page 286
Next qualification of this module is due in x Warning page 286
day(s) (due date is [date]).
Next qualification of this module is overdue (due Warning page 287
date was [date]).
Next qualification of this module is overdue (due Error page 287
date was [date]). Module may no longer be used.
Next qualification of this module was due on Warning page 287
[date]. Allowing x more grace day(s).
Next service of this module is due in x day(s) Warning page 287
(due date is [date]).
Next service of this module is overdue (due date Warning page 287
was [date]).
No chip card in the reader for the column x. Error page 288
No response from x for x seconds. Warning page 288
No response from x for x seconds. Device Abort page 288
disconnected.

Table 8-4. TC Error Messages (Continued)

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TC-Related Audit Trail Error Message Default See


Severity
Level
Operating columns above 70 °C could affect Warning page 289
column performance. Verify recommended
column operating conditions before setting
temperature above 70 °C.
Parameter x value exceeded its allowed range. Warning page 289
Set to closest valid value y.
Primary property “x” is already assigned and Error page 290
cannot be changed.
Properties cannot be changed. A chip card has Error page 290
not been inserted properly. Check the CardState
property for all cards and reinsert those
indicating “BusBlocked.”
Properties cannot be changed if the Error page 290
compartment door is open.
Properties cannot be changed—there is no card Error page 291
in the card reader.
Raw data file x cannot be created. Warning page 291
Raw data file x cannot be created. Continuing Warning page 291
with network failure protection.
Raw data file x cannot be written. Warning page 291
Raw data file x cannot be written. Continuing Warning page 291
with network failure protection.
Starting data acquisition manually will overwrite Warning page 292
any data which has been acquired so far.
TC—Firmware download failed. Abort page 277
TC is not remote. Abort page 282
The command can format only chip cards with Error page 292
an invalid data structure.
The communication interface is closed. Error page 292
Reconnect the instrument.
The compartment door is open; a batch or a Warning page 293
program may need to wait until the door has
been closed. Please close the door.

Table 8-4. TC Error Messages (Continued)

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8 • Troubleshooting

TC-Related Audit Trail Error Message Default See


Severity
Level
The counter [name] (value: x) has exceeded its Warning page 293
limit (y). Module should no longer be used.
Replace the [name].
The data format stored on the chip card is Error page 293
unsupported (format version x).
The injections limit for the column has been Warning page 294
exceeded.
The injections limit will be exceeded for the Warning page 294
column x.
The nominal temperature must be set within the Error page 294
current limits.
The nominal temperature value is out of range Error page 294
defined by the active column ID.
The oven is not fully operable yet. Check the Error page 294
values of “Standby,” “Ready,” “Door,” and
“CardState.”
The primary column ID property “x” will be Warning page 295
changed. The property can't be changed in the
future.
The upper limit must be higher than the lower Error page 295
limit.
The Warning threshold must be higher than the Error page 296
Limit threshold.
The Warning threshold must be lower than the Error page 296
Limit threshold.
There was already an AcqOff command for this Warning page 296
channel before.
There was already an AcqOn command for this Warning page 296
channel before.
This function cannot be adjusted by the user. Abort page 297
This operation may affect the oven's operation Warning page 297
on timebase x, which is currently running a
batch.

Table 8-4. TC Error Messages (Continued)

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TC-Related Audit Trail Error Message Default See


Severity
Level
Two AcqOn commands for the same channel. Error page 296
The second chromatogram will overwrite the
first.
Unknown error code. Warning page 297
Unknown format of the card data. Error page 297
USB/LAN communication error. Please check Abort page 283
communication cable and instrument’s power.
Value for [name] parameter is not within valid Warning page 289
range. Value passed (x) will be substituted by y.
Value x replaced by valid table entry y. Warning page 289
X position error. Abort page 298
You do not have the privilege to approve the Error page 298
module's qualification.
You do not have the privilege to change the Error page 298
performance limits.
You do not have the privilege to change the Error page 298
qualification intervals.

Table 8-4. TC Error Messages (Continued)

8.2 Noisy Baseline


• Eluent is contaminated
1. Clean all eluent reservoirs thoroughly (inside and out) with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, follow the cleaning instructions in Section 9.4.
2. Flush the system with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
3. Replace all end-line filters (P/N 045987). See Section 4.6 for
instructions.
4. Prepare new stock solution.

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8 • Troubleshooting

5. Prepare fresh eluent. To ensure eluent purity, prepare all eluents with
spectro-grade eluents, reagent-grade chemicals, and ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5.
• DP/SP not properly primed
Prime the pump (see Section 9.5).
• Piston seal is damaged
If the piston seal is damaged, it allows liquid leaks. Leaks are usually
visible, and thus easily detected. If necessary, replace the piston seal (see
Section 9.7).
• Inadequate system or cell backpressure
Add backpressure tubing to the cell outlet (see Section 9.27.4) or to the
pump (if no column is installed).
• (Analytical EG only) System backpressure is below 14 MPa (2000 psi)
The optimal system backpressure is 16 MPa (2300 psi) in an analytical IC
system with an EG installed,. Low system backpressure may cause high
baseline noise as the eluent concentration increases in the gradient. To
correct this, install a backpressure coil in the EG after the RFIC Eluent
Degasser (see Section 9.17).
• Flow system leak ahead of cell
Check all fittings and liquid lines for leaks. Tighten or, if necessary,
replace all liquid line connections (see Section 9.19).
• Rapid changes in ambient temperature
Make sure the column is installed in a thermostatically controlled
compartment and the compartment door is closed.
• Insufficient system equilibration following changes to operating
parameters; especially apparent when operating at high sensitivities
Allow a longer system equilibration time (up to 2 hours) before starting
operation.

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Noisy Baseline: CD Only

• Incorrect suppressor operating conditions


Refer to the suppressor manual for troubleshooting information.
Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).
• Cell above or below temperature
Contact Technical Support for Dionex products for assistance.
• Detector electronics not functioning correctly
Run the detector dummy cell diagnostics from the Wellness panel (see
Section 9.27).
• Inappropriate suppressor operating conditions
Refer to the suppressor manual for the correct operating conditions.
Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).
• Temperature compensation setting not optimized
Optimize the selected setting (see Section 2.14).
• Trapped gases in cell
Release any trapped gases in the cell by loosening the lines to and from
the cell and then retightening them. Also loosen and retighten the fittings
to and from the suppressor eluent ports.
• Inadequate system backpressure
In an analytical IC system, add backpressure tubing to the cell outlet (see
Section 9.27.4).

Noisy Baseline: ED Only

• (DC Amperometry and Integrated Amperometry modes) Air bubbles


trapped inside cell
While wearing gloves and eye protection and with the pump running and
all plumbing connected, generate a slight temporary backpressure by
putting your finger over the end of the cell outlet tubing for 2 to

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8 • Troubleshooting

3 seconds. Repeat two or three times. If the baseline does not improve,
check the other causes of baseline instability described in this section.
Do not block the end of the cell outlet tubing for longer than the
recommended 2 to 3 seconds. Doing so creates high backpressure,
which can break the pH-Ag/AgCl reference electrode glass membrane.

NOTE To prevent air from becoming trapped in the cell in the future,
increase the backpressure on the cell by connecting backpres-
sure tubing to the cell outlet. The backpressure limit for the
ED cell is 690 kPa (100 psi). Do not exceed this limit.

• (DC Amperometry and Integrated Amperometry modes) Frequent,


random spikes in the baseline
The pH-Ag/AgCl reference electrode diaphragm is plugged. First, try
regenerating the pH-Ag/AgCl reference electrode frit by soaking the
electrode in a solution of 1 M KCl plus 1 M HCl. If this does not
eliminate the spiking, replace the electrode (P/N 061879).
• (DC Amperometry and Integrated Amperometry modes) Regular
baseline oscillation on high-sensitivity ranges
Reconnect the short length of titanium tubing to the cell inlet (see
Figure 2-30).
• (DC Amperometry and Integrated Amperometry modes) Dirty or
pitted conventional (nondisposable) working electrode
Polish the working electrode (see Section 9.28.4). If you are using a
disposable electrode, replace it.
• (Integrated Amperometry mode) Regular baseline oscillations
1. Check the pump pressure plot to verify that the pump is working
properly.
2. Air bubbles may be trapped inside the cell. While wearing gloves and
eye protection, generate a slight temporary backpressure by putting
your finger over the end of the cell outlet tubing for 2 to 3 seconds.

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Repeat two or three times. If the baseline does not improve, check the
other causes of baseline instability described in this section.
Do not block the end of the cell outlet tubing for longer than the
recommended 2 to 3 seconds. Doing so creates high backpressure,
which can break the pH-Ag/AgCl reference electrode glass membrane.

NOTE To prevent air from becoming trapped in the cell in the


future, increase the backpressure on the cell by con-
necting backpressure tubing to the cell outlet. The
backpressure limit for the ED cell is 690 kPa
(100 psi). Do not exceed this limit.

3. The water used to prepare the eluent may contain trace contaminants.
Remake the eluent, using ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.

8.3 Poor Retention Time Reproducibility


• Liquid leaks
1. Check for leaks from the piston seals. Replace the piston seal on any
head with a leak (see Section 9.7).
2. Check for leaks throughout the remainder of the system, including the
check valves, injection valve, and columns. Tighten or replace fittings
as needed.
• DP/SP not primed
Prime the pump (see Section 9.5).
• Liquid lines incompletely flushed after an eluent change
Attach a 10 cc syringe (P/N 054578) to the waste port on the priming
valve. Open the priming valve (turn the knob one-half turn
counterclockwise). Draw at least 20 mL of the new eluent through the
liquid lines before operation.
• Inoperative eluent proportioning valve (gradient pump only)
The proportioning valve assembly should be replaced. Contact Technical
Support for Dionex products for assistance.

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8 • Troubleshooting

• Inoperative check valves


Replace the check valve cartridges (see Section 9.6).
• Insufficient mixing (gradient pump only)
The static mixer may be dirty or contaminated. Flush with IPA (isopropyl
alcohol). If this does not eliminate the problem, install a new mixer (GM-
3, P/N 042126; GM-4, P/N 049135).
• Eluent is contaminated
1. Clean all eluent reservoirs thoroughly (inside and out) with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, follow the cleaning instructions in Section 9.4.
2. Flush the system with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
3. Replace all end-line filters (P/N 045987). See Section 4.6 for
instructions.
4. Prepare new stock solution.
5. Prepare fresh eluent. To ensure eluent purity, prepare all eluents with
electrochemical-grade chemicals, and ASTM Type I (18 megohm-
cm) filtered and deionized water that meets the specifications listed in
Section 1.5.
• Problem unrelated to the pump
1. The eluent concentration may be wrong, or the eluent may have been
prepared with impure chemicals/eluents or water. To ensure eluent
purity, prepare all eluents with spectro-grade eluents, reagent-grade
chemicals, and ASTM Type I (or better) filtered and deionized water
that meets the specifications listed in Section 1.5.
2. The column may be the source of the problem. Refer to the column
manual for troubleshooting assistance. Column manuals are provided
on the Thermo Scientific Reference Library DVD (P/N 053891).
3. The injection valve may be the source of the problem. Rebuild the
injection valve (see Section 9.22).

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8.4 Peak Retention Times Are Too Early


• Eluent concentration setting is too high
The correct eluent concentration setting depends on several factors (the
flow rate, EGC type, etc.). Refer to Section 4.9 for a list of valid
concentration ranges for the cartridges, and then edit the program as
required.
• DP/SP flow rate is too low
Increase the DP/SP flow rate.
• Inoperative eluent proportioning valve (gradient pump only)
The proportioning valve assembly should be replaced. Contact Technical
Support for Dionex products for assistance.

8.5 Peak Retention Times Are Too Late


• Eluent concentration setting is too low
The correct eluent concentration setting depends on several factors (the
flow rate, EGC type, etc.). Refer to Section 4.9 for a list of valid
concentration ranges for the cartridges, and then edit the program as
required.
• DP/SP flow rate is too high
Decrease the DP/SP flow rate.
• Inoperative eluent proportioning valve (gradient pump only)
The proportioning valve assembly should be replaced. Contact Technical
Support for Dionex products for assistance.

8.6 No Peaks
• EG power is not turned on
1. Check that the POWER button on the front of the EG is turned on.
2. Check that the EG main power switch (on the rear panel) is turned on.

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8 • Troubleshooting

3. Check that the main power cord is plugged into both the EG rear
panel connector and the power source. Check that the wall outlet has
power.
• Injection valve is not actuating or the sample loop is plugged
1. Test the valve by manually switching the position from the DC ePanel
in Chromeleon 7 or Control panel in Chromeleon 6.8.
2. Check the sample loop for blockage. Clean or replace the loop if
needed.
• Detector not properly installed
CD: An electronics connector on the back of the detector plugs into a
receptacle on the detector compartment. Push on the detector to make
certain the connector is securely connected (see Figure 8-1).
• ED: Verify that the signal cables from the cell are connected to the
detector block. In addition, an electronics connector on the back of the
detector plugs into a receptacle on the detector compartment. Push on the
detector to make certain the connector is securely connected (see
Figure 8-1).

Push here to ensure that the


detector’s electrical
connection is secure.

Figure 8-1. Detector Connection

ED Only

• Cell is off
Turn on the cell from the detector ePanel (in Chromeleon 7) or Control
panel (in Chromeleon 6.8).

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8.7 Tailing Peaks


• Excess tubing void volumes
Check tubing connections for void volumes.
• (CD) Long tubing lengths connecting
Minimize all tubing lengths between the injection valve and the detector.
• (DC Amperometry and Integrated Amperometry modes) Dirty or
pitted conventional (nondisposable) working electrode
Clean the working electrode with water and dry with pressurized air or
nitrogen.
Polish the working electrode (see Section 9.28.4). If you are using a
disposable electrode, replace it.
Capillary • Capillary tubing fittings incorrectly installed
IC
Incorrectly installed fittings on capillary tubing can increase void
volumes, causing chromatograms with tailing peaks (see Figure 8-2).

Figure 8-2. Tailing Peaks Caused by Incorrectly Installed


Capillary Tubing Fittings

To correctly install fittings on capillary tubing, follow the instructions in


Section 9.1.

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8 • Troubleshooting

8.8 Low System Backpressure


• Loose fitting
Make sure there are no liquid leaks in the flow system. Check tubing
connections throughout the system (including the check valves, injection
valves, and columns) and tighten or replace fittings as needed.
• RFIC Eluent Degasser tubing is ruptured
If flow from the EG waste line is normal but there is no flow through the
columns, the tubing assembly inside the RFIC Eluent Degasser has
ruptured. Replace the degasser (see Section 9.16).
• Internal EGC leak (from membrane barrier)
Leakage from the membrane barrier may trip the DP/SP low pressure
limit and shut down the pump. If all other causes of the low system
pressure have been eliminated, replace the EGC (see Section 9.14).

NOTE The EG leak sensor cannot immediately detect leakage from


the membrane barrier because these leaks exit the EG through
the vent line.

8.9 High System Backpressure


• Restriction in the system plumbing
1. Begin pumping eluent through the system (including the columns) at
the flow rate normally used.
2. Work backward through the system, beginning at the flow cell exit.
One at a time, loosen each fitting and observe the pressure. The
connection at which the pressure drops abnormally indicates the point
of restriction. If the EGC is the source of the high backpressure,
replace the outlet frit as instructed in the EGC manual. The manual is
on the Thermo Scientific Reference Library DVD (P/N 053891).
3. If the restriction has caused such high pressure that the system cannot
be operated, you must work forward through the system, adding parts
one at a time until an abnormal pressure increase (and hence, the
restriction) is found.

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• TC temperature stabilizer is blocked


Rinse the temperature stabilizer and the temperature stabilizer inlet line,
using an appropriate solvent. If necessary, replace the temperature
stabilizer (standard bore, P/N 064548; microbore, P/N 064650).

8.10 Low Detector Output


• Insufficient sample injected
Increase the injection size or concentration.

ED Only

• Working electrode fouled


1. If a disposable working electrode is being used, replace the electrode.
2. For conventional (nondisposable) electrodes, clean the working
electrode with ASTM Type I (18 megohm-cm) filtered and deionized
water that meets the specifications listed in Section 1.5. Dry with
pressurized air or nitrogen. If the electrode is pitted, polish the
electrode (see Section 9.28.4).
3. Check the value of the reference potential shift (see “Using a Digital
Voltmeter to Determine Reference Potential Shift” on page 274). If
the value fluctuates by more than 30 mV, electrode passivation may
occur because potentials that are too high are being applied.
Recalibrate the pH-Ag/AgCl reference electrode (see Section 9.28.6).
If the problem persists, replace the pH-Ag/AgCl reference electrode
(see Section 9.28.5).

Analog Output Option

• Analog output range set too high


Select a more sensitive analog output range.

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8 • Troubleshooting

8.11 High Background


• CR-TC is contaminated
Clean the trap column as instructed in the CR-TC manual. The manual is
included on the Thermo Scientific Reference Library DVD (P/N 053891).
• Wrong eluent
Check that you are using the correct eluent for your application. For ED
detectors, verify that the pH readout is correct for your eluent.
• Background signal not offset from detector signal
Before injecting sample, allow the background signal to equilibrate, and
then press Autozero on the detector ePanel in Chromeleon 7 or Control
panel in Chromeleon 6.8.

CD Only

• Background not suppressed by suppressor


Verify that the suppressor is turned on and the current is set to the correct
value. Refer to the suppressor manual for additional troubleshooting
guidance. Suppressor manuals are included on the Thermo Scientific
Reference Library DVD (P/N 053891).
• Regenerant fails to suppress background
Use a higher regenerant flow rate. Refer to the suppressor manual for the
suggested regenerant flow rate for your application.

ED Only

• (Integrated Amperometry mode) Excessive number or length of


integration intervals and/or incorrect potential for the integration
Verify that the length and potential of the integration interval is correct
(refer to the column manual for the settings required for your application).
Column manuals are included on the Thermo Scientific Reference Library
DVD (P/N 053891).

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• (DC Amperometry and Integrated Amperometry modes)


Amperometric detection cell working electrode shorted to counter
electrode
Clean the working electrode with water and dry with pressurized air or
nitrogen.
Remove any precipitate on the counter electrode by cleaning the spot
directly opposite the working electrode with a lint-free tissue.
• (DC Amperometry and Integrated Amperometry modes)—Leak
between gasket and electrode, or between gasket and cell body
Remove any precipitate with water and a lint-free tissue and then install a
new gasket (see Section 9.28.3).
Turn the yoke knob (see Figure 9-53) a full 360 degrees to completely
engage the knob.

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ICS-5000
DP/SP DP/SP Troubleshooting

8.12 Troubleshooting DP/SP Error Messages


If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon Audit Trail.

A program with this name already exists.

This error occurs if you attempt to save a modified Chromeleon 7 instrument


method or Chromeleon 6.8 program under the name of an existing instrument
method or program.
To troubleshoot:
Enter a new name for the modified instrument method or program or select
Save to save your changes under the existing instrument method or program
name.

Abnormal drive current for x.x seconds.

If this error occurs, the tubing between the pump heads may be blocked or the
fitting may be overtightened.
To troubleshoot:
Inspect the tubing for blockage or crimping and replace if needed (see
Section 9.3). Be careful to not overtighten fittings. If the message appears
again, contact Technical Support for Dionex products for assistance.

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Camshaft index too early.


-or-

Camshaft index too late.

This error is caused by an internal error in the pump drive mechanism.


To troubleshoot:
Turn off the DP/SP power for 30 seconds and then turn it on again. If the error
message appears again, contact Technical Support for Dionex products for
assistance.

Camshaft sensor always alight.


-or-

Camshaft sensor missing or dark.

This error is caused by an internal error in the pump drive mechanism.


To troubleshoot:
Turn off the DP/SP power for 30 seconds and then turn it on again. If the error
message appears again, contact Technical Support for Dionex products for
assistance.

Degasser malfunction.

The vacuum degassing module monitors the vacuum system continuously. If a


problem is detected, this error occurs.
To troubleshoot:
1. Check all tubing connections to the vacuum degassing module for
leakage; tighten loose fitting connections. Be careful not to overtighten
fittings.
2. Turn off the DP/SP power for 30 seconds and then restart the pump.
3. If the message appears again, the vacuum degassing module should be
replaced. Contact Technical Support for Dionex products for assistance.

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8 • DP/SP Troubleshooting

Excessive drive current. Camshaft x.x.

This error occurs if the drive current is above the allowed value. When this
message appears, the DP/SP stops running.
To troubleshoot:
One or more tubing connections may be plugged, blocked, or crimped. Check
all tubing connections and replace as needed (see Section 9.3). Be careful not
to overtighten fittings.

Invalid flow value.

This error occurs if you enter an invalid value for the DP/SP flow rate in
Chromeleon.
To troubleshoot:
Select a flow rate within the DP/SP flow rate range. For the flow rate range
for each type of DP/SP, refer to Section 1.5.

Leak detected.

This error occurs if the DP/SP leak sensor detects a liquid leak inside the
enclosure. When this error occurs, the pump stops running.
To troubleshoot:
To find and eliminate the source of the leak, see Section 8.15.

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Left-hand pump block carryover pressure is too high.


-or-

Right-hand pump block carryover pressure is too high.

This error occurs if the pressure in the primary pump head exceeds the
maximum allowed. (“Right-hand” refers to the bottom pump; “left-hand”
refers to the top pump in a dual-pump module.)
To troubleshoot:
1. Make sure that the tubing between the pump heads and the tubing leading
to the priming/outlet block is not plugged or blocked. Replace tubing
connections as needed (see Section 9.3). Be careful not to overtighten
fittings.
2. Inspect the outlet check valve for blockage. Replace the check valve
cartridge if needed (see Section 9.6).

Motor malfunction.

This error occurs if an internal error in the pump drive mechanism occurs.
To troubleshoot:
Turn off the DP/SP power for 30 seconds, and then turn on the power again. If
the error message appears again, contact Technical Support for Dionex
products for assistance.

Motor position error. The motor is overloaded.

This error occurs if the pump motor is overloaded.


To troubleshoot:
1. One or more tubing connections may be plugged or blocked. Check all
tubing connections and replace as needed (see Section 9.3). Be careful not
to overtighten fittings.
2. If the “Upper pressure limit exceeded message” is also displayed, refer to
page 234 for additional troubleshooting steps.

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8 • DP/SP Troubleshooting

Pressure fallen below lower limit.

This error occurs if the DP/SP pressure falls below the low pressure limit
specified in Chromeleon.
To troubleshoot:
1. The eluent supply may be depleted. Check the Eluent Level Display on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset to verify
that eluent is present in the selected channel. If the eluent reservoir is
empty, refill it (or select a channel that does have eluent). Prime the pump
before resuming operation (see Section 9.5).
2. Check all eluent lines for air bubbles. If air is trapped in a line, replace the
end-line filter (P/N 045987). See Section 4.6 for instructions. Verify that
the end of each filter extends to the bottom of the reservoir and is
submerged in eluent. Prime the pump (see Section 9.5).
3. Eluents may be insufficiently degassed. Check the vacuum degassing
module.
4. Check all tubing connections for leaks; tighten loose fitting connections.
Be careful not to overtighten fittings.
5. Make sure the priming valve is closed (see Figure 2-3). To close the
valve, turn the knob clockwise until closed. Tighten no more than
fingertight.
Do not use any tools to tighten the priming valve! Overtightening may
destroy the cap seal. Open or close the priming valve only when the
system pressure is down.

6. A check valve may be defective. Replace the check valve cartridges (see
Section 9.6) and then prime the pump (see Section 9.5).

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Relay 4 is configured for inject synchronization. Please change


pump configuration.

This error occurs if you attempt to use relay 4 as a standard relay in a


Chromeleon 7 instrument method or Chromeleon 6.8 program, but the relay
has been set to synchronize the gradient with the autosampler sample
injection.
To troubleshoot:
Define the relay as a standard relay or specify a different relay for use in the
program.

The maximum purge pressure was exceeded.

If the DP/SP pressure exceeds 5 MPa (725 psi) during priming, this error
occurs and the priming process is aborted.
To troubleshoot:
1. Verify that the priming valve is open. (To open the valve, turn the knob
one-half turn counterclockwise.)
2. Check fittings for overtightening. Check tubing for crimping and replace
it as necessary (see Section 9.3). Be careful not to overtighten fittings.

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8 • DP/SP Troubleshooting

The pressure in the left-hand working cylinder exceeded the


safety limit.
-or-

The pressure in the right-hand working cylinder exceeded the


safety limit.
-or-

The system pressure exceeded the safety limit.

This error may be caused by a blockage in the system or by a problem with


the column. (“Right-hand” refers to the bottom pump; “left-hand” refers to the
top pump in a dual-pump module.)
To troubleshoot:
1. Check all tubing connections for signs of blockage; replace as needed (see
Section 9.3). Be careful not to overtighten fittings.
2. To determine the source of the high backpressure, isolate segments of the
flow path:
a. Remove the pump outlet tubing at the injection valve.
b. Press the POWER button on the front of the DP/SP to turn on the
pump.
c. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, set
the Flow rate to 0.01 mL/min for a capillary IC system or 1.0 mL/min
for an analytical IC system and record the backpressure.
d. Disconnect all components after the injection valve.
e. One at a time, reconnect each component of the flow path. If
reconnecting a component causes an abnormal increase in
backpressure, replace the component. Replace as many components
as necessary to resume operation at the standard operating
backpressure.
3. As columns age, their backpressure increases. It may be necessary to
compensate for this by increasing the high pressure limit. If the column is
the source of the high backpressure, clean the column. (Refer to the
column manual provided on the Thermo Scientific Reference Library
DVD (P/N 053891) for instructions.) If this does not eliminate the
problem, replace the column.

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Dionex ICS-5000 Operator’s Manual

4. Observe a run to see whether the high pressure limit is triggered when
injection occurs; if it is, the injection valve may be the source of the
blockage (i.e., the rotor seal or stator may need to be replaced). Contact
Technical Support for Dionex products for assistance.

This function cannot be adjusted by the user.

This error occurs if you attempt to change a parameter that users are not
allowed to adjust.
To troubleshoot:
Only Thermo Fisher Scientific Service Representatives can change this
parameter.

Upper pressure limit exceeded.

This error occurs if the upper pressure limit specified in the program is
exceeded. The running batch is aborted (default) and this message appears.
To troubleshoot:
1. Inspect the tubing for blockage or crimping; replace as needed (see
Section 9.3). Be careful not to overtighten fittings.
2. To determine the source of the high backpressure, isolate segments of the
flow path:
a. Remove the pump outlet tubing at the injection valve.
b. Press the POWER button on the front of the DP/SP to turn on the
pump.
c. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, set
the Flow rate to 0.01 mL/min for a capillary IC system or 1.0 mL/min
for an analytical IC system and record the backpressure.
d. Disconnect all components after the injection valve.
e. One at a time, reconnect each component of the flow path. If
reconnecting a component causes an abnormal increase in
backpressure, replace the component. Replace as many components

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8 • DP/SP Troubleshooting

as necessary to resume operation at the standard operating


backpressure.
3. As columns age, their backpressure increases. It may be necessary to
compensate for this by increasing the high pressure limit. If the column is
the source of the high backpressure, clean the column. (Refer to the
column manual provided on the Thermo Scientific Reference Library
DVD (P/N 053891) for instructions.) If this does not eliminate the
problem, replace the column.
4. Observe a run to see whether the high pressure limit is triggered when
injection occurs; if it is, the injection valve may be the source of the
blockage (i.e., the rotor seal or stator may need to be replaced). Contact
Technical Support for Dionex products for assistance.

8.13 DP/SP Does Not Start


• Power is off
Check that the main power switch on the DP/SP rear panel is turned on.
Press the POWER button on the front of the DP/SP to turn on the pump.
• Flow rate is set to zero
Select a Flow rate on the Chromeleon 7 ePanel Set or Chromeleon 6.8
panel tabset.
• While being primed, pump starts briefly and an alarm sounds
If the high pressure limit was tripped:
1. Check that the priming valve on the secondary pump head is opened
(see Figure 2-3). To open the valve, turn the knob one-half turn
counterclockwise.
2. Check fittings for overtightening. Check tubing for crimping and
replace it as necessary (see Section 9.3). Be careful not to overtighten
fittings.

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If the low pressure limit was tripped:


1. Verify that the Minimum Pressure setting is set to the correct value.
2. Make sure there are no liquid leaks in the flow system. To find and
eliminate the source of a leak, see Section 8.15.
If an Audit Trail error message is displayed, refer to the troubleshooting
steps listed for the particular message.

8.14 DP/SP Stops


• Instrument method or program (or other remote input) instructed
the pump to stop
If no error message is displayed in the Audit Trail, the DP/SP was
probably instructed to stop by the Chromeleon 7 instrument method, the
Chromeleon 6.8 program, or other remote signal source. If you do not
want the pump to stop, take the appropriate preventive action (edit the
instrument method, the program, or the settings of the other remote signal
source).
• Low pressure limit was tripped
Refer to the troubleshooting steps for the Audit Trail message “Pressure
fallen below lower limit.” on page 231.
• High pressure limit was tripped
Refer to the troubleshooting steps for the Audit Trail message “The
system pressure exceeded the safety limit.” on page 233.
• Electrical connections incorrectly installed
The electrical cables may not be properly installed. Contact Technical
Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

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8 • DP/SP Troubleshooting

8.15 DP/SP Liquid Leaks/Leak Alarm


NOTE After eliminating the source of a leak, always dry the leak
sensor thoroughly. If the leak sensor is not dry, it will remain
activated and will continue to report a leak to the Audit Trail.

• Defective piston seal


Check the pump heads for leaks. If there is any leakage, tighten the fitting
connections just enough to stop the leak. Dry the components. If the pump
head continues to leak, replace the piston seal (see Section 9.7).
• Leaking check valve
If the leaking check valve is securely tightened but allows leaks despite
this, the valve is defective. Replace both check valve cartridges (see
Section 9.6).
If the leaking check valve is loose, follow these steps to tighten it:
1. Turn off the pump.
2. Loosen the check valve enough to allow it to turn freely.
3. Tighten the check valve fingertight, and then tighten it one-quarter
turn with a 1/2-inch wrench.
4. If the check valve continues to leak, tighten it an additional one-
quarter turn with the 1/2-inch wrench.
5. If the check valve continues to leak, it is defective. Replace both
check valve cartridges (see Section 9.6).
• Eluent proportioning valve leaks (gradient pump only)
Tighten loose fittings. If there are no loose fittings, the proportioning
valve assembly should be replaced. Contact Technical Support for Dionex
products for assistance.

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• Priming valve knob leaks


If leaks occur when the priming valve knob is open, close the knob
completely and then open it one-half to three-quarters turn. If this does not
stop the leakage, replace the seal in the priming valve knob (see
Section 9.10).
If leaks occurs when the priming valve knob is closed, either the pump
head or the knob is damaged and should be replaced. Contact Technical
Support for Dionex products for assistance.
• Excessive system backpressure
If system backpressure is substantially higher than the normal operating
backpressure for the currently configured system (including the column),
tubing may be plugged or overtightened. Refer to the troubleshooting
steps for the Audit Trail message “The system pressure exceeded the
safety limit.” on page 233.

8.16 Vacuum Degassing Module Low Vacuum


• Leak in the vacuum degassing module
Check all tubing connections for leakage; tighten loose fitting
connections.

8.17 Vacuum Degassing Module Does Not Run


• Electrical connections incorrectly installed
There may be a problem with the connections from the vacuum degassing
module to the CPU board. Contact Technical Support for Dionex products
for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

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8 • DP/SP Troubleshooting

8.18 DP/SP Digital I/O Port Inoperative


• TTL input-related error
1. The TTL input mode must match the signal type output by the device
connected to the pump. Check the user’s manual for the device to
verify that the correct signal type is selected.
2. A programming error occurred in the device sending the signal. Refer
to the user’s manual for the device for troubleshooting assistance.
• TTL/Relay output-related error
1. A programming error occurred in the device sending the signal. Refer
to the user’s manual for the device for troubleshooting assistance.
2. The device being triggered may require a TTL, not a relay. Connect
the device to a pump TTL output.

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240 Doc. 065342-06 12/11


ICS-5000
EG EG Troubleshooting

8.19 Troubleshooting EG Error Messages


If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon Audit Trail.

Concentration out of range! The maximum value is %1.


-or-

Concentration out of range! The maximum value at time %1 is %2.

The allowable eluent concentration depends on the flow rate and the EGC
type. This message appears if the selected eluent concentration is out-of-range
for the flow rate. The time indicated in the message refers to the time
specified in the Chromeleon 7 instrument method or Chromeleon 6.8
program.
To troubleshoot:
Check the information in Section 4.10 to verify that the selected concentration
is within the accepted range for the cartridge type and flow rate. Adjust the
flow rate or concentration as needed.

CR-TC1 open circuit.


-or-

CR-TC2 open circuit.

To troubleshoot:
1. Check that the CR-TC is correctly plugged into the EG. Push the CR-TC
electrical cable firmly into the CR-TC 1 (or CR-TC 2) bulkhead connector.
Twist the ring on the cable connector fingertight to secure it.
2. If the error persists, the CR-TC may be faulty. Replace the CR-TC (see
Section 9.15).

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CR-TC1 over current.


-or-

CR-TC2 over current.

This error occurs when the current applied to the CR-TC exceeds the
maximum current allowed. (The CR-TC current is automatically turned off to
prevent damage to the CR-TC.) This error may also occur if liquid flow to the
CR-TC is interrupted.
To troubleshoot:
1. Check the CR-TC cable connection to the electrical bulkhead (see
Figure 2-10).
2. Refer to Section 8.23 to determine why liquid flow stopped.
3. If the error message appears again, contact Technical Support for Dionex
products for assistance. The CR-TC control electronics may have
malfunctioned.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components cannot be serviced by the
user.

CR-TC1 stopped because EGC1 OFF.


-or-

CR-TC2 stopped because EGC1 OFF.

This error occurs if you attempt to turn on the CR-TC when the EGC is turned
off. The CR-TC current is automatically turned off to prevent damage to the
CR-TC.
To troubleshoot:
Verify that the pump flow and the EGC are on before turning on the CR-TC.

242 Doc. 065342-06 12/11


8 • EG Troubleshooting

CR-TC1 stopped due to zero flow.


-or-

CR-TC2 stopped due to zero flow.

This error occurs if you turn off the pump flow while the EGC current (and
CR-TC) are on. The CR-TC current is automatically turned off to prevent
damage to the CR-TC.
To troubleshoot:
If the pump stopped unexpectedly, follow the troubleshooting steps in
Section 8.23.

The CR-TC mode is off for a virtual pump.

This error occurs when a “live” EG is linked to a virtual pump and you try to
turn on the CR-TC. The mode is automatically turned off to ensure that the
EG does not operate when there is no flow.

CR-TC mode will be turned off for invalid flow. Flow range for
analytical EGC: 0.100 – 3.000 mL/min, capillary EGC: 0.001 –
0.100 mL/min.

This error occurs when the flow to the CR-TC is out of range or there is no
pumped linked to the EGC.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.
2. Check the EGC configuration properties in the Chromeleon 7 Instrument
Controller Service or the Chromeleon 6.8 Server Configuration program
to verify that the pump and EGC are linked.

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Dionex ICS-5000 Operator’s Manual

Current linked pump is capillary. Please install a capillary EGC.


-or-

Current linked pump is analytical. Please install an analytical


EGC.

This error occurs if the type of pump linked to the EGC does not match the
EGC type. A capillary EGC can only be used with a capillary pump and an
analytical EGC can only be used with an analytical pump.
To troubleshoot:
1. Install the correct type of EGC for the pump type.
2. For a hybrid system (a dual system with both an analytical and a capillary
pump), check the EGC configuration properties in the Chromeleon 7
Instrument Controller Service or the Chromeleon 6.8 Server
Configuration program to verify that the correct pump is linked to the
EGC.

EG1 cartridge disconnected.


-or-

EG2 cartridge disconnected.

This error occurs if Chromeleon sends a command to set an EG parameter


when the EGC is disconnected.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance. The EGC control electronics may have
malfunctioned.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components cannot be serviced by the
user.

244 Doc. 065342-06 12/11


8 • EG Troubleshooting

EG1 invalid activation date.


-or-

EG2 invalid activation date.

This error occurs if the activation date for the EGC is not a valid date. This
may indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.

EG1 invalid concentration.


-or-

EG2 invalid concentration.

This error occurs if the eluent concentration is outside the range allowed by
the EG. This may indicate corrupted memory or a problem in the EG
instrument control firmware.
To troubleshoot:
Contact Technical Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components and instrument control
firmware cannot be serviced by the user.

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Dionex ICS-5000 Operator’s Manual

EG1 invalid flow.


-or-

EG2 invalid flow.

This error occurs if the flow rate is set to a value the EG does not support.
To troubleshoot:
Set the flow rate to a value within the allowed range. Refer to Appendix A for
flow rate specifications.

EG1 invalid flow rate-concentration.


-or-

EG2 invalid flow rate-concentration.

This error occurs if the selected concentration is too high for the current flow
rate.
To troubleshoot:
Set the flow rate to a value within the allowed range. The allowable eluent
concentration for a particular application depends on several factors: the flow
rate, suppressor type, EGC type, and cartridge configuration. For details, refer
to Section 4.9.

EG1 invalid ion count.


-or-

EG2 invalid ion count.

This error occurs if the ion count reported by the EGC is invalid. This may
indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.

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8 • EG Troubleshooting

EG1 invalid serial number.


-or-

EG2 invalid serial number.

This error occurs if the serial number reported by the EGC is invalid. This
may indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.

EG1 over current.


-or-

EG2 over current.

This error occurs when the current applied to the EGC exceeds the maximum
current allowed. (The EGC current is automatically turned off to prevent
damage to the cartridge.) This error may also occur if the liquid flow to the
cartridge is interrupted.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. Refer to Section 8.23 to determine why there is no flow.
3. If the error message appears again, contact Technical Support for Dionex
products for assistance. The cartridge control electronics may have
malfunctioned.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components cannot be serviced by the
user.

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EG1 over power.


-or-

EG2 over power.

This error occurs when, in order to maintain the selected current, the power
supply is required to supply a higher voltage than the EGC can support.
To troubleshoot:
Replace the EGC (see Section 9.14).

EG1 over voltage.


-or-

EG2 over voltage.

This error occurs when the current applied to the EGC exceeds the maximum
current allowed. (The EGC current is automatically turned off to prevent
damage to the cartridge.) This error may also occur if the liquid flow to the
cartridge is interrupted.
To troubleshoot:
1. Refer to Section 8.23 to determine why there is no flow.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance. The EGC control electronics may have
malfunctioned.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components cannot be serviced by the
user.

248 Doc. 065342-06 12/11


8 • EG Troubleshooting

EG1 wrong cartridge error.


-or-

EG2 wrong cartridge error.

This error occurs when an EGC is plugged into the EG that is not one of the
supported types.
To troubleshoot:
Refer to Table 2-2 for a list of the supported EGC types for capillary and
analytical IC systems.

The EG mode is off due to pump pressure alarm or leak.

This error occurs if the pump flow is turned off because of a pump pressure
alarm or leak. The EG is automatically turned off to prevent damage to the
EG.
To troubleshoot:
Check the troubleshooting information for the pump in Section 8.14 and
Section 8.15.

The EG mode is off for a virtual pump.

This error occurs when a “live” EG is linked to a virtual pump and you try to
turn on the EGC. To prevent damage to the EGC, the mode is automatically
turned off to ensure that the EG does not operate when there is no flow.

EG mode will be turned off for invalid flow.

This error occurs when the flow to the EG is out of range or there is no
pumped linked to the EG.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.

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Dionex ICS-5000 Operator’s Manual

2. Check the EGC configuration properties in the Chromeleon 7 Instrument


Controller Service or the Chromeleon 6.8 Server Configuration program
to verify that the pump and EGC are linked.

EG mode will be turned off for invalid flow. Flow range for
analytical EGC: 0.100 – 3.000 mL/min, capillary EGC: 0.001 –
0.100 mL/min.

This error occurs when the flow to the EGC is out of range or there is no
pumped linked to the EGC.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.
2. Check the EGC configuration properties in the Chromeleon 7 Instrument
Controller Service or the Chromeleon 6.8 Server Configuration program
to verify that the pump and EGC are linked.

EGC-1 is not linked to a compatible pump.


-or-

EGC-2 is not linked to a compatible pump.

This error occurs if the type of pump linked to the EGC does not match the
EGC type. A capillary EGC can only be used with a capillary pump and an
analytical EGC can only be used with an analytical pump.
To troubleshoot:
1. Install the correct type of EGC for the pump type.
2. For a hybrid system (a dual system with both an analytical and a capillary
pump), check the EGC configuration properties in the Chromeleon 7
Instrument Controller Service or the Chromeleon 6.8 Server
Configuration program to verify that the correct pump is linked to the
EGC.

250 Doc. 065342-06 12/11


8 • EG Troubleshooting

EGC cannot be used due to invalid ion count.

This error occurs if the ion count reported by the EGC is invalid. This may
indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.

EGC is either not installed or invalid cartridge number. Please


install a capillary EGC.

This error occurs if no EGC cartridge is connected to the EG or an analytical


EGC is connected to a capillary IC system.
To troubleshoot:
1. Verify that a capillary EGC is installed.
2. Verify that the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.

EGC is either not installed or invalid cartridge number. Please


install an analytical EGC.

This error occurs if no EGC cartridge is connected to the EG or a capillary


EGC is connected to an analytical IC system.
To troubleshoot:
1. Verify that an analytical EGC is installed.
2. Verify that the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.

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Dionex ICS-5000 Operator’s Manual

EGC is either not installed or invalid cartridge number. Please


install an EGC.

This error occurs if no EGC cartridge is connected to the EG or the cartridge


serial number is not valid for the type of IC system.
To troubleshoot:
1. Verify that an EGC of the correct type (capillary or analytical) is installed.
2. Verify that the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.

Leak sensor wet.

This error occurs when liquid accumulates in the drip tray in the bottom of the
EG.
To troubleshoot:
1. Locate the source of the leak by visually inspecting the tubing, fittings,
and components in the EG.
2. Tighten fittings (or replace tubing and fittings) as required (see
Section 9.12). Refer to Section 8.22 for detailed troubleshooting of
various types of leaks.
3. After fixing the leak, dry the drip tray and leak sensor thoroughly to
prevent the leak sensor from triggering additional error messages.

pH modifier must be used with a different type of cartridge.

This error occurs if you attempt to configure an EPM III Electrolytic pH


Modifier with an incompatible type of EGC.
To troubleshoot:
Verify that the EPM III is paired with an EGC III K2CO3. The EPM III cannot
be used with any other cartridge type.

252 Doc. 065342-06 12/11


8 • EG Troubleshooting

Pump is disconnected. The EG mode and CR-TC modes are


turned off.

This error occurs if the pump linked to the EG is disconnected from


Chromeleon. To prevent damage to the EGC and CR-TC, the modes are
automatically turned off to ensure that the EG does not operate when there is
no flow.

8.20 EG ALARM LED Is Lighted


• Leaking fitting
Locate the source of the leak. Tighten or replace liquid line connections as
needed (see Section 9.12).
• Blocked or improperly installed waste line
Check the EG waste lines to be sure they are not crimped or otherwise
blocked. Make sure the lines are not elevated at any point after they exit
the EG.
• EGC leaks
Replace the EGC (see Section 9.14).
• RFIC Eluent Degasser leaks
Replace the RFIC Eluent Degasser (see Section 9.16).
• EGC electrical connection is open
1. Tug gently on the EGC electrical cable; the locking connector should
hold the cable in place (see Figure 2-10).
2. If the electrical cable is fully seated but the problem persists, the
cartridge is defective and must be replaced (see Section 9.14).
• EGC input electrical connection has shorted out
Replace the EGC (see Section 9.14).

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• Electrical error
The EG current and/or voltage may have become unstable. Contact
Technical Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

8.21 EG POWER LED Fails to Light


• No power
Check that the POWER button on the front of the EG is turned on.
Check that the EG main power switch (on the rear panel) is turned on.
Check that the main power cord is plugged into both the EG rear panel
connector and the power source. Check that the wall outlet has power.
If the POWER LED still fails to light, contact Technical Support for
Dionex products for assistance.

8.22 Liquid Leaks in the EG


• Leaking fitting
Locate the source of the leak. Tighten or replace liquid line connections as
needed (see Section 9.12).
• Blocked or improperly installed waste line
Check the EG waste lines to be sure they are not crimped or otherwise
blocked. Make sure the lines are not elevated at any point after they exit
the EG.
• EGC leaks
Replace the EGC (see Section 9.14).
• (Analytical IC only) RFIC Eluent Degasser leaks
Replace the analytical IC system RFIC Eluent Degasser (see
Section 9.16).

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8 • EG Troubleshooting

8.23 No Flow
• DP/SP power is off
Turning off the DP/SP automatically turns off the EG and the suppressor.
Current to the CR-TC is automatically turned on and off when the EG
power is turned on and off.
Check that the power to the DP/SP is turned on. Prime the pump (see
Section 9.5) and resume operation.
• DP/SP pressure limit tripped
Verify that the Current Pressure reading on the Chromeleon 7 ePanel Set
or the Chromeleon 6.8 panel tabset is between the high and low limits
displayed on the panel. For details, see Section 4.8.

NOTE The analytical EGC requires at least 14 MPa


(2000 psi) of backpressure for optimal removal of
electrolysis gas from the eluent produced by the car-
tridge. A system backpressure of 16 MPa (2300 psi) is
ideal.

• (Analytical IC only) RFIC Eluent Degasser tubing is ruptured


If flow from the EG waste line is normal but there is no flow through the
columns, the tubing assembly inside the analytical IC system RFIC Eluent
Degasser has ruptured. Replace the degasser (see Section 9.16).

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8.24 EG Stops Operation


• DP/SP power is off
Turning off the DP/SP automatically turns off the EG and the suppressor.
Current to the CR-TC is automatically turned on and off when the EG
power is turned on and off.
Check that the power to the DP/SP is turned on. Prime the pump (see
Section 9.5) and resume operation.
• DP/SP pressure limit tripped
Verify that the Current Pressure reading on the Chromeleon 7 ePanel Set
or the Chromeleon 6.8 panel tabset is between the high and low limits
displayed on the panel. For details, see Section 4.8.

NOTE The analytical EGC requires at least 14 MPa (2000 psi)


of backpressure for optimal removal of electrolysis gas
from the eluent produced by the cartridge. A system
backpressure of 16 MPa (2300 psi) is ideal.

• DP/SP flow rate is too low or too high


For a capillary IC system, select a flow rate between 0.001 and
0.100 mL/min. For an analytical IC system, select a flow rate between
0.100 and 3.000 mL/min.
• Electrical error detected (ALARM LED is lighted)
To prevent damage to the EGCs, the DP/SP automatically turns off
electrical power to the cartridge when excessive current or voltage is
detected. Contact Technical Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

• EGC is expended
Replace the cartridge (see Section 9.14).
• No communication with Chromeleon
1. Check that the POWER button on the front of the EG is turned on.

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8 • EG Troubleshooting

2. Check that the EG main power switch (on the rear panel) is turned on.
3. Check that the main power cord is plugged into both the EG rear
panel connector and the power source. Check that the wall outlet has
power.
4. Check the USB connections. The EG should be connected to the
DP/SP (or other Dionex ICS-5000 module) via a USB cable
(P/N 960777). In addition, one module in the system must be
connected to the PC on which Chromeleon is installed.
5. Check that the EG is configured in Chromeleon and is assigned to an
instrument (Chromeleon 7) or timebase (Chromeleon 6.8).

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ICS-5000
DC DC Troubleshooting

8.25 Troubleshooting DC Error Messages


If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon Audit Trail.

CD cell option disconnected.

To troubleshoot:
1. Check the detector connection: An electronics connector on the back of
the detector plugs into a receptacle on the detector compartment. Push on
the upper part of the detector (see Figure 8-3) to make certain the
connector is securely connected.
2. If the error persists, there may be a problem in the detector electronics.
Contact Technical Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

Push here to
ensure the
detector’s
electrical
connection is
secure.

Figure 8-3. Conductivity Detector Connection

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CD cell over safe temperature.

This error occurs when the temperature of the conductivity detector is higher
than the maximum allowed. This error may occur if the Thermo Scientific
Dionex ICS-5000 Ion Chromatography System is operating in an
environment in which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
1. Refer to Appendix A for environmental specifications.
2. Verify that the compartment setpoint is at least 5 °C less than the CD cell
setpoint.
3. Check the suppressor current setting. Running the suppressor at a higher
current than is recommended for the application can cause heat-up of the
CD cell.

Column temperature open circuit.

This error may indicate a problem in the detector electronics. Contact


Technical Support for Dionex products for assistance.

Column over safe temperature.

This error occurs when the temperature of the column compartment exceeds
the maximum allowed. This error may occur if the Thermo Scientific Dionex
ICS-5000 Ion Chromatography System is operating in an environment in
which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.

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8 • DC Troubleshooting

Column temperature calibration error.

To troubleshoot:
Repeat the calibration procedure. Follow the instructions provided in the DC
Temperature Calibration Kit (P/N 063782). If the error appears again, contact
Technical Support for Dionex products for assistance.

Compartment temperature open circuit.

This error may indicate a problem in the detector electronics. Contact


Technical Support for Dionex products for assistance.

Compartment over safe temperature.

This error occurs when the temperature of the DC lower compartment is


higher than the maximum allowed. This error may occur if the Thermo
Scientific Dionex ICS-5000 Ion Chromatography System is operating in an
environment in which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.

Compartment temperature calibration error.

To troubleshoot:
Repeat the calibration procedure, following the instructions provided in the
DC Temperature Calibration Kit (P/N 063782). If the error appears again,
contact Technical Support for Dionex products for assistance.

ED cell current exceeds limits error.

This error can have multiple causes (for example, a cell potential that is too
high for a given salt concentration, a cell potential that is too high because the
reference mode is incorrect, injection of excessive amounts of electroactive

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analytes, a damaged or incorrectly installed cell gasket, or an electrical short


between two of the three electrodes).
To troubleshoot:
1. Turn off the cell voltage. Excessive currents can change or even damage
the working electrode.
2. Turn off the pump flow.
3. Disassemble the cell (see Section 9.28.3) and check for evidence of liquid
and salt bridges that can cause shorts. Rinse the cell surface and dry it
with a clean, lint-free towel. Replace the cell gasket.
4. Verify that the correct electrode material, waveform potentials, and
reference mode are selected for the application being run.
5. Restart the flow and select DC amperometry mode. Apply cell potential
in steps increasing toward the detection potential (the potential of the
integration period in integrated amperometric detection). If the current
becomes excessive again, try a new working electrode or another cell, if
available.

ED cell option disconnected.

This error indicates that the electrochemical detector is unplugged.


To troubleshoot:
1. Check the detector connections: Verify that the signal cable from the cell
is connected to the appropriate connector on the detector block (see
Figure 8-4). Also, push firmly on the detector to ensure the electronics

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8 • DC Troubleshooting

connector on the back of the detector is securely connected to the


receptacle on the detector compartment.

Push here to ensure


the detector’s
electrical connection
is secure.

ED Cell Cable

Figure 8-4. Electrochemical Detector Connection (Analytical Cell Shown)

2. If the error appears again, contact Technical Support for Dionex products
for assistance. The detector electronics may have malfunctioned.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chroma-


tography System electronics components cannot be
serviced by the user.

ED cell working electrode disconnected.

This error occurs when the cable on the working electrode is disconnected
from the cell electronics.
To troubleshoot:
Check the cable connection: Verify that the signal cable from the working
electrode is connected to the detector block (see Figure 8-4).

ED pH offset calibration failed.

This error occurs when the pH reading differs by more than 1.0 pH unit from
7.0, which is the value specified for offset calibration. This can be caused by
too large a change in the Ag/AgCl reference potential or by a damaged glass
membrane in the pH sensing part of the reference electrode
To troubleshoot:

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1. Check the buffer selection.


2. Verify that the electrode is properly immersed in the calibration buffer.
3. Repeat the calibration procedure (see Section 9.28.6). If the error recurs,
repeat the calibration at least one more time.
4. If the error recurs after repeating the calibration at least two times, replace
the Ag/AgCl reference electrode (see Section 9.28.5).

ED pH slope calibration failed.

This error occurs when the pH sensing glass membrane of the Ag/AgCl
reference electrode is broken or otherwise affected, causing the calibration
slope to deviate by more than ±10% from the theoretical slope of 59 mV/pH
unit at 25 C.
To troubleshoot:
1. Make sure the calibration temperature is as close as possible to 25 C.
2. Verify that the correct buffer is being used and that the electrode is
properly immersed in the calibration buffer.
3. Repeat the calibration procedure (see Section 9.28.6). If the error recurs,
repeat the calibration at least one more time.
4. If the error recurs after repeating the calibration at least two times, replace
the Ag/AgCl reference electrode (see Section 9.28.5).

ED reference electrode disconnected.

To troubleshoot:
Check the cable connection: Verify that the signal cable from the working
electrode is connected to the detector block (see Figure 8-4).

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8 • DC Troubleshooting

High pressure valve 1 error.


-or-

High pressure valve 2 error.


-or-

High pressure valve 3 error.


-or-

High pressure valve 4 error.

This error occurs if a high-pressure valve fails to switch position within


1 second of being toggled. High-pressure valves 1 and 2 are the valves
installed in the DC lower compartment (see Figure 8-5). High-pressure valves
3 and 4 are the valves installed on either the IC Cubes or the AM in the upper
compartment (see Figure 8-6).

High-Pressure
1 Valve #1

High-Pressure
1 2 2 Valve #2 (not
installed in this
system)

Figure 8-5. High-Pressure Valves #1 and #2 (In DC Lower Compartment)

High-
3 Pressure
Valve #3

High-
3 4 4 Pressure
Valve #4

Figure 8-6. High-Pressure Valves #3 and #4 (On IC Cubes)

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Dionex ICS-5000 Operator’s Manual

3 High-
4 Pressure
3
Valve #3

High-
4 Pressure
Valve #4

Figure 8-7. High-Pressure Valves #3 and #4 (On AM)

To troubleshoot:
1. If a sequence is being executed, terminate the sequence by selecting Stop
on the Chromeleon 7 ePanel or Chromeleon 6.8 Control panel.
2. Turn off the Thermo Scientific Dionex ICS-5000 Ion Chromatography
System power briefly by pressing the POWER button on the front of each
module. Then press each button again to restart the system.
3. Try to toggle the valve from Load to Inject by pressing the Load and
Inject buttons on the front of the DC.
4. If the problem persists, contact Technical Support for Dionex products for
assistance.

IC Cube 1 heater over safe temperature.


-or-

IC Cube 2 heater over safe temperature.

This error occurs when the temperature of the IC Cube heater exceeds the
maximum allowed. This error may occur if the Thermo Scientific Dionex
ICS-5000 Ion Chromatography System is operating in an environment in
which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.

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8 • DC Troubleshooting

Lower door opened.

This message occurs when the door to the lower compartment is opened
during a run.
To troubleshoot:
1. Verify that the door is fully closed.
2. Check for—and remove—any obstruction.
3. If the door is fully closed and the error persists, contact Technical Support
for Dionex products for assistance.

Lower leak sensor wet.

The leak sensor is installed in the drip tray at the bottom of the column
compartment (see Figure 9-33). If liquid accumulates in the tray, the sensor
signals the problem and this error message appears.
To troubleshoot:
1. Locate the source of the leak by visually inspecting the tubing, fittings,
and components.
2. Tighten fittings or replace tubing and fittings as required. Refer to
Section 8.26 for detailed troubleshooting of various types of leaks.
3. After fixing the leak, dry the drip tray thoroughly to prevent the leak
sensor from triggering additional error messages.

Reaction coil open circuit.

This error occurs when the reaction coil heater is unplugged from the DC.
To troubleshoot:
1. Check that the reaction coil heater is correctly plugged into the
component panel.
2. If the error persists, the heater may be faulty. Replace the heater
(P/N 061746).

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Reaction coil over safe temperature.

This error occurs when the temperature of the DC upper compartment is


higher than the maximum allowed. This error may occur if the Thermo
Scientific Dionex ICS-5000 Ion Chromatography System is operating in an
environment in which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.

Suppressor over-current.

This error may be caused by a depleted or dirty suppressor or by a


malfunction in the suppressor controller electronics.
To troubleshoot:
1. Follow the instructions in the suppressor manual to regenerate the
suppressor. Suppressor manuals are included on the Thermo Scientific
Reference Library DVD (P/N 053891).
2. Follow the instructions in the suppressor manual to clean the suppressor.
3. If you suspect a malfunction in the suppressor controller, contact
Technical Support for Dionex products for assistance.

NOTE The Thermo Scientific Dionex ICS-5000 Ion Chromatogra-


phy System electronics components cannot be serviced by the
user.

Suppressor over-power.

This error appears when, in order to maintain the selected current, the Thermo
Scientific Dionex ICS-5000 Ion Chromatography System is required to apply
a higher voltage than the suppressor can support.
To troubleshoot:
1. Reduce the flow rate.

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8 • DC Troubleshooting

2. Rehydrate the suppressor. Refer to the suppressor manual for instructions.


Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).
3. If the error persists, replace the suppressor (see Section 9.27.2).

Suppressor over-voltage.

This error appears if you turn on the suppressor and the system cannot
establish a connection with the suppressor.
To troubleshoot:
1. Check the suppressor cable connection.
2. If the error persists, replace the suppressor (see Section 9.27.2).

Suppressor stopped for flow rate.

This message occurs if the pump flow stops while the suppressor is on. The
suppressor is automatically turned off to prevent damage to the suppressor.
To troubleshoot:
If the pump stopped unexpectedly, see Section 8.14 for pump troubleshooting
information.

Upper door opened.

This message occurs when the door to the upper compartment is opened
during a run.
To troubleshoot:
1. Verify that the door is fully closed.
2. Check for—and remove—any obstruction.
3. If the door is fully closed and the error persists, contact Technical Support
for Dionex products for assistance.

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8.26 Liquid Leaks from DC Components


• Leaking fitting
Locate the source of the leak. Tighten or, if necessary, replace the liquid
line connection (see Section 9.19).
• Broken liquid line
Replace the line and fittings with the same length and internal diameter
tubing (see Section 9.19).
• Blocked or improperly installed line
Make sure the lines are not crimped or otherwise blocked. Also, if the
blocked line is a waste line, make sure it is not elevated at any point after
it exits the DC. If a line is blocked, replace it (see Section 9.19).
• Leaking injection valve
1. Make sure the liquid line connections to the transducer are tight.
Replace any damaged fittings (see Section 9.19).
2. If the leak is from behind the valve stator, the rotor seal may be
scratched. Rebuild the injection valve (see Section 9.22).
• Leaking cell
1. Check the waste lines for blockage; trapped particles can plug the
lines and cause a restriction and/or leak. If necessary, clear the waste
lines by reversing the direction of flow.
2. Make sure the plumbing downstream from the cell is clear; a
blockage may overpressurize the cell and cause it to leak. If the
problem continues, Contact Technical Support for Dionex products
for assistance.
Leaking suppressor
Refer to the suppressor manual for troubleshooting procedures.
Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).

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8 • DC Troubleshooting

8.27 VALVE Button Not Working


The VALVE 1 and VALVE 2 buttons on the front of the DC must be enabled in
Chromeleon 6.8 or Chromeleon 7 in order to use them to manually switch the
inject valves. To enable a button, open the Commands dialog box and select
the Valve1Button (or Valve2Button) command in the list of commands for
the DC.

8.28 ED Cell Troubleshooting

8.28.1 ED Cell pH Readout Always 7.0


The pH reading of the pH-Ag/AgCl reference electrode is displayed on the
Chromeleon 7 ED ePanel or the Chromeleon 6.8 EC Detector panel.
• Disconnected pH-Ag/AgCl reference electrode
Verify that the reference electrode cable is securely connected (see
Figure 8-8).

Check the
cable
connection

Figure 8-8. ED Cell Electrical Connections

• Reference electrode short circuit


Replace the reference electrode (see Section 9.28.5).
• pH-Ag/AgCl reference electrode glass membrane broken or cracked
Replace the pH-Ag/AgCl reference electrode (see Section 9.28.5).

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8.28.2 Cannot Set ED Cell pH Readout to 7.0


The pH reading of the pH-Ag/AgCl reference electrode is displayed on the
ED ePanel in Chromeleon 7 or the EC Detector Control panel in Chromeleon
6.8.
• Inaccurate calibration buffer
Use a pH meter to check the pH of the buffer.
• Dry pH-Ag/AgCl reference electrode
1. Soak the pH-Ag/AgCl reference electrode in a solution containing
1 M KCl and 1 M HCl long enough to restore the electrode potential
to within 30 mV when compared to an unexposed Ag/AgCl reference
electrode. To test the pH-Ag/AgCl reference electrode potential, see
“Using a Digital Voltmeter to Determine Reference Potential Shift”
on page 274.
2. Replace the pH-Ag/AgCl reference electrode (see Section 9.28.5).
To prevent a pH-Ag/AgCl reference electrode from drying out, make sure
that eluent is being pumped continuously through the cell. If the cell will
not be used for a short time (less than 2 days), disconnect the tubing from
the inlet and outlet fittings and all fitting plugs. For longer shutdowns,
remove the electrode from the cell and store it in its storage bottle filled
with saturated KCl solution. See Section 4.1.2 for detailed instructions.

8.28.3 Shift in ED Cell pH Readout


The pH readout is considered to have shifted if it is 0.5 pH units or more
different from the value observed when the pH-Ag/AgCl reference electrode
was new.
• Faulty pH-Ag/AgCl reference electrode
1. Check the electrode by following the instructions in Section 8.28.6.
2. Regenerate the electrode by soaking in a solution containing 1 M KCl
and 1 M HCl long enough to restore the electrode potential to within
30 mV when compared to an unexposed Ag/AgCl reference
electrode. To test the pH-Ag/AgCl reference electrode potential, see
“Using a Digital Voltmeter to Determine Reference Potential Shift”
on page 274.

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8 • DC Troubleshooting

3. If soaking does not fix the problem, replace the electrode (see
Section 9.28.5).

8.28.4 No ED Cell pH Readout or Intermittent Readout


The pH reading is displayed on the ED ePanel in Chromeleon 7 or the EC
Detector Control panel in Chromeleon 6.8.
• PdH reference electrode selected
Select the AgCl reference electrode mode on the ED ePanel in
Chromeleon 7 or the EC Detector Control panel in Chromeleon 6.8, or in
the Chromeleon 7 instrument method or the Chromeleon 6.8 program.
• Disconnected reference electrode
Verify that the reference electrode cable is securely connected (see
Figure 8-8).
• Uncalibrated pH-Ag/AgCl reference electrode
Calibrate the pH-Ag/AgCl reference electrode (see Section 9.28.6).
• Dry pH-Ag/AgCl reference electrode
1. Soak the pH-Ag/AgCl reference electrode in a solution containing
1 M KCl and 1 M HCl long enough to restore the electrode potential
to <30 mV when compared to an unexposed Ag/AgCl reference
electrode. To test the electrode potential, see “Using a Digital
Voltmeter to Determine Reference Potential Shift” on page 274.
2. If soaking the pH-Ag/AgCl reference electrode does not fix the
problem, replace the electrode (see Section 9.28.5).
To prevent a pH-Ag/AgCl reference electrode from drying out, make sure
that eluent is being pumped continuously through the cell. If the cell will
not be used for a short time (less than 2 days), disconnect the tubing from
the inlet and outlet fittings and all fitting plugs. For longer shutdowns,
remove the electrode from the cell and store it in its storage bottle filled
with saturated KCl solution. See Section 4.1.2 for detailed instructions.
• Contaminated pH-Ag/AgCl reference electrode
Replace the pH-Ag/AgCl reference electrode (see Section 9.28.5).

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8.28.5 Leak in pH-Ag/AgCl Reference Electrode Compartment


• Defective pH-Ag/AgCl reference electrode O-ring
Replace the pH-Ag/AgCl reference electrode O-ring (see Section 9.28.7).

8.28.6 Shift in Ag/AgCl Reference Potential


• Faulty pH-Ag/AgCl reference electrode
A shift in reference potential causes a shift in the effective potential
applied to the working electrode. For example, when using an electrode
with a shift of 50 mV, an applied potential of 0.1 V, is equivalent to an
applied potential of 0.15 V for a new pH-Ag/AgCl reference electrode
with no shift.
Following the steps below, measure the pH-Ag/AgCl reference electrode
potential shift by comparing it to the potential shift of an unexposed
electrode. A spare pH-Ag/AgCl reference electrode (P/N 061879) stored
in 3 M KCl can be kept on hand for this purpose.

Using a Digital Voltmeter to Determine Reference Potential Shift

1. For each pH-Ag/AgCl reference electrode (the unexposed electrode and


the electrode being tested), use a straightened paper clip or short piece of
wire of a suitable diameter to connect the voltmeter’s voltage inputs to
pin 1 on the reference electrode’s cable connector.
To identify the cable connector pins, refer to Product Information Update
for the Electrochemical Detector (PIU_ED_1). The document is included
on the Thermo Scientific Reference Library DVD (P/N 053891).
2. Immerse both electrodes in a solution of 0.1 M KCl.
3. Read the potential difference (in mV) between the unexposed electrode
and the electrode being tested. If it is greater than 30 mV, try regenerating
the electrode by soaking it in a solution containing 1 M KCl and 1 M HCl.
If this does not reduce the potential shift, replace the electrode (see
Section 9.28.7).

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ICS-5000
TC TC Troubleshooting

8.29 Troubleshooting TC Error Messages


If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon Audit Trail.

AcqOff without previous AcqOn.

This error occurs if the Chromeleon 7 instrument method or Chromeleon 6.8


program contains an AcqOff command, but no AcqOn command.
To troubleshoot:
Every program should include one AcqOn command. Enter the AcqOn
command after the first injection.

Acquisition is still on at program end.

This error occurs if a Chromeleon 7 instrument method or Chromeleon 6.8


program does not include a command that ends data acquisition.
To troubleshoot:
The AcqOn command must be paired with an AcqOff command. Enter the
AcqOff command at the appropriate point in the program.

All samples scheduled for run on timebases x need to specify the


same value for property (nominal) Temperature.
-or-

All samples scheduled for run on timebases x need to specify the


same value for property TempCtrl.
-or-

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All samples scheduled for run on timebases x need to specify the


same value for property y.

When a TC is shared by two timebases, the same values must be selected for
certain parameters. If the Chromeleon Ready Check detects a discrepancy,
this error occurs and batch processing cannot be started.
To troubleshoot:
Find and eliminate any discrepancies in the parameter settings. For example,
all samples must turn on TempCtrl or all samples must turn off TempCtrl.

Can't execute “Disconnect” command during data acquisition.


-or-

Can't execute “Standby” command during data acquisition.

Selecting the Disconnect or Standby command during data acquisition will


stop data transmission and cause data acquisition to stall. If you attempt to
issue one of these commands during data acquisition, this error occurs.
To troubleshoot:
Wait until data acquisition is completed before attempting to issue either of
these commands.

Can't find download image TC3000.HEX.

TC3000.HEX is the version of the TC instrument control firmware file that


should be available in the \Bin directory of your Chromeleon installation. This
error occurs if the file is missing.
To troubleshoot:
Select Tools > Instrument Qualification (Chromeleon 7) or Qualification >
Chromeleon 6.8 IQ (Chromeleon 6.8) to run the Chromeleon IQ and
diagnose the problem. When you eliminate the source of the error, rerun the
Setup program.

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8 • TC Troubleshooting

Can't start acquisition at negative retention times.

This error occurs if you attempt to execute the AcqOn command while
retention times are negative.
To troubleshoot:
Wait until the retention time value is positive.

Can’t start acquisition: The server configuration does not fulfill


the license conditions.

Operation of the TC requires the appropriate version of Chromeleon plus a


Timebase Class 1 license. This error occurs if you attempt to start data
acquisition when these requirements are not met.
To troubleshoot:
Contact your local Dionex products representative at Thermo Fisher
Scientific to obtain the appropriate software version and/license.

Can’t start TC firmware. A firmware download may be necessary.

-or-

Error finishing download.


-or-

TC—Firmware download failed.

If the TC firmware cannot be started after a firmware download or if


Chromeleon is unable to successfully download firmware to the TC, the
appropriate message (shown above) is displayed.
To troubleshoot:
1. Press the POWER button on the front of the TC to turn off the power; after
30 seconds, press the button again to turn on the power.
2. Download new firmware to the TC as follows:
a. Insert the CD containing the new firmware version into the CD drive.

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b. Start the Chromeleon 7 Instrument Configuration Manager or the


Chromeleon 6.8 Server Configuration program.
c. In the instrument or timebase, right-click the TC for which you want
to update the firmware and select Properties on the context menu.
d. On the General tab page in the Properties dialog box, click
Firmware Download to display a file open dialog box.
e. Select the file (the extension is .fmw) containing the new firmware
version and click Open to begin the download. Audit Trail messages
will inform you of the status of the download.
3. If the error occurs again, contact Technical Support for Dionex products
for assistance. The firmware cannot be serviced by the user.

Can't use device “x” as a source of the column pressure. Please


check the property “SystemPressure” for a valid device name.
The device must have the “Pressure” property available.
-or-

Can't use device “x” as a source of the column pressure. Please


check the property “y” for a valid device name. The device must
have the “Pressure” property available.

This error occurs if the device selected to monitor the system pressure is
ineligible to do so.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name, and select the SystemPressure
command.
4. Enter the name of the pump currently delivering flow for this column.
5. For Chromeleon 6.8, click Execute.

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Card data checksum error.

This error indicates that the column ID chip card memory is corrupted.
To troubleshoot:
Replace the column ID chip card (see Section 9.30).

Command is not available in demo mode.

This error occurs if you attempt to issue a command that is not available when
the TC is in demo (or simulation) mode.
To troubleshoot:
If a TC is present and connected, disable the demo mode:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. In the instrument or timebase, right-click the TC and select Properties.
3. On the General tab page, clear the Simulation Mode or Demo Mode
check box.
4. If the TC does not appear in the Module address box, click Browse and
select the TC. Click OK.

Communication error: x.

This error occurs if there is a communication failure between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.

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Communication time-out.

This error occurs if a TC firmware command is not executed within the time
allotted for its completion.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.

Configuration doesn’t match. X not installed.


-or-

Configuration mismatch (x - CM uses y, Column Compartment


uses z). Please use the Server Configuration program to check
the installation.

This error occurs if there is a discrepancy between the TC properties and the
actual configuration.
To troubleshoot:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. In the instrument or timebase, right-click the TC and select Properties.
3. Correct any discrepancies in the Properties dialog box.

Current flow is out of limits defined for the column.

This error occurs if the current flow rate exceeds the value specified by the
Column_x.FlowRate_UpperLimit command.
To troubleshoot:
Select a valid flow rate.

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Current pressure is out of limits defined for the column.

This error occurs if the current pressure reading is outside the range specified
by the Column_x.Pressure_UpperLimit and Column_x.Pressure_
LowerLimit commands.
To troubleshoot:
• Find and eliminate any liquid leaks or blockages in tubing connections
(see Section 8.31). Adjust the flow rate accordingly.

Current temperature is out of limits defined for the column.

This error occurs if the current temperature reading is outside the range
specified by the Column_x.Temp_UpperLimit and Column_x.Temp_
LowerLimit commands.
To troubleshoot:
Select a valid temperature setting.

Data buffer overrun.

This error occurs in Chromeleon 6.8 if the system cannot write incoming data
to disk fast enough.
To troubleshoot:
Increase the buffer size:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. Right-click the computer name and select Properties on the menu.
3. Click the Advanced tab and enter a new value (in seconds) in the Buffer
field. Click OK.
4. If the error occurs again, contact Technical Support for Dionex products
for assistance.

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Device control feature is not available! Please check key code


and CM Features (see “About Chromeleon...” on the client's Help
menu).

This error occurs if you attempt to select or define a feature that is not
available for your TC.
To troubleshoot:
Select Help > About Chromeleon... to open the About Chromeleon screen.
• For Chromeleon 7, click Details to view all license features you
purchased (devices controlled, number of timebases, and other software
options).
• For Chromeleon 6.8, the license features you purchased are listed on the
About Chromeleon screen and labeled On.
If necessary, upgrade your software by acquiring the corresponding licenses.
Contact your local Dionex products representative at Thermo Fisher
Scientific for assistance.

Device is not remote.


-or-

TC is not remote.

If you try to issue certain commands (for example, Column_x and


InjectValve_x commands) when the TC is not under Chromeleon control, the
appropriate message (shown above) is displayed.
To troubleshoot:
Select the Connect command to connect the TC to the Chromeleon server.
Check the Audit Trail for messages indicating whether the module was
successfully connected.

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Device not found on the USB.


-or-

USB/LAN communication error. Please check communication


cable and instrument’s power.

This error occurs if there is a problem with the connection between the TC
and the Chromeleon server or with the power supply.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.

Either the current date is later than the expiration date for x or the
program or batch will end later than 24 hours before the
expiration time for x.

Chromeleon compares the current date with the column expiration date during
injection or before beginning batch processing. This error occurs if the
expiration date has already passed or if batch processing is scheduled to start
less than 24 hours before the expiration date.
To troubleshoot:
Replace the column.

Error deleting flash memory.

This error occurs if, during a firmware download, the existing firmware
cannot be erased from memory.
To troubleshoot:
Flash memory cannot be serviced by the user. Contact Technical Support for
Dionex products for assistance.

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Error during storing of the card data to the chip card.

This error occurs if the column ID chip card is installed incorrectly, or is


defective.
To troubleshoot:
When the chip card is properly installed, the Dionex logo on the card faces up
and the LED on the memory slot is green. If this error occurs when the chip
card is properly installed, it indicates that the card is defective and should be
replaced (for instructions, refer to Section 9.30).

Error programming flash memory.

This error occurs if, during a firmware download, the new firmware cannot be
programmed into memory.
To troubleshoot:
Flash memory cannot be serviced by the user. Contact Technical Support for
Dionex products for assistance.

Executing this command will reset associated counter values


stored in the module.

This error occurs when you select a command (RotorSealChanged, for


example) that updates information stored in the TC. To prevent information
from being inadvertently changed, Chromeleon requests confirmation before
executing the command.
To troubleshoot:
If you want to execute this command, click Execute; otherwise, click Cancel.

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Firmware download in progress. Please wait.

This error occurs if you attempt to issue a command while firmware is being
downloaded to the TC.
To troubleshoot:
Wait until the firmware download is complete. Audit Trail messages will
inform you of the status of the download.

Gas leak detected.

This error occurs if the gas sensor detects an increased concentration of gas
inside the TC.
To troubleshoot:
1. Find and eliminate the leak.
2. If you are using Chromeleon 7: Open the Commands dialog box (press
the F8 key). Select the TC and click the Commands tab. Click the
ClearAlarmLED button.
3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door and
resuming operation.

Humidity leak detected.

This error occurs if the humidity sensor detects an increased concentration of


humidity inside the TC.
To troubleshoot:
1. Find and eliminate the leak.
2. If you are using Chromeleon 7: Open the Commands dialog box (press
the F8 key). Select the TC and click the Commands tab. Click the
ClearAlarmLED button.

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3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door and
resuming operation.

Illegal parameter.

This error occurs if you enter a parameter that is not valid for the TC.
To troubleshoot:
Select a valid parameter.

Invalid date/time format. Either use “DD MMM YYYY” or “current [


+ [Nyear[s]] [Nmonth[s]] [Nday[s]]].” Examples: “31 Dec 1999,”
“current + 1 year 6 months.”

This error occurs if you enter the date associated with an event in an invalid
format.
To troubleshoot:
Enter the date in the format specified in the message.

Invalid enumerated value.

This error occurs if you attempt to enter an invalid value for a property, rather
than selecting a value from the drop-down list box in the Commands dialog
box.
To troubleshoot:
Select a valid option from the drop-down list box available for this property.

Next qualification of this module is due in x day(s) (due date is


[date]).
-or-

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Next qualification of this module is overdue (due date was [date]).


-or-

Next qualification of this module was due on [date]. Allowing x


more grace day(s).
-or-

Next qualification of this module is overdue (due date was [date]).


Module may no longer be used.

Chromeleon monitors the date on which qualification was last performed and
displays an appropriate message (shown above) at the following times: when
the due date for the next qualification is approaching; when the due date is
overdue, but the TC can still be used; and when the due date is overdue and
the TC can no longer be used.
The Qualification.WarningPeriod property determines the number of days
before the due date that the warning is first displayed. The
Qualification.GracePeriod property determines for how many days after the
due date you can continue using the TC without performing the qualification.
To troubleshoot:
Contact Technical Support for Dionex products to schedule an Operational
Qualification and Performance Qualification.

Next service of this module is due in x day(s) (due date is [date]).


-or-

Next service of this module is overdue (due date was [date]).

Chromeleon monitors the date on which service was last performed and
display an appropriate message (shown above) at the following times: when
the due date for the next service is approaching and when the due date is
overdue. The Service.WarningPeriod property determines the number of
days before the due date that the warning is first displayed.
To troubleshoot:
Contact Technical Support for Dionex products for information about
performing annual preventive maintenance.

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No chip card in the reader for the column x.

This error occurs if a column ID chip card is not installed for the column
identified in the message.
To troubleshoot:
Install a column ID chip card for the column (see Section 9.30). Or, if you do
not want to store information about this column, follow the steps below to
disable this option.
1. In the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program, right-click the TC and
select Properties on the context menu.
2. Select the Components tab in the Properties dialog box. Clear the check
mark beside the column name and click OK.

No response from x for x seconds.


-or-

No response from x for x seconds. Device disconnected.

This error occurs if there is a communication failure between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.

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Operating columns above 70 °C could affect column


performance. Verify recommended column operating conditions
before setting temperature above 70 °C.

This error occurs if you select a TC temperature setting above 70 °C (158 °F).
To troubleshoot:
Refer to the column manual for the recommended operating conditions.
Column manuals are provided on the Thermo Scientific Reference Library
DVD (P/N 053891).

Parameter x value exceeded its allowed range. Set to closest valid


value x.
-or-

Value for [name] parameter is not within valid range. Value passed
(x) will be substituted by y.
-or-

Value x replaced by valid table entry y.

If you select a value outside the allowable range for certain parameters,
Chromeleon ignores the setting, replaces it with the closest valid setting, and
this error occurs.
To troubleshoot:
No immediate action is required. In future, specify a valid setting for the
parameter.

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Primary property “x” is already assigned and cannot be changed.

This error occurs if you attempt to change one of the primary column
properties (batch or lot number, date of manufacture, etc.) used for column
identification.
To troubleshoot:
Once a primary column property has been assigned, it cannot be changed. As
an alternative, consider changing a secondary column property. For a list of
primary and secondary properties, refer to the Chromeleon Help.

Properties cannot be changed. A chip card has not been inserted


properly. Check the CardState property for all cards and reinsert
those indicating “BusBlocked.”

This error occurs if you attempt to change column ID properties when at least
one column ID chip card is inserted incorrectly.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name and select the CardState property. If
the status is BusBlocked, remove the card from the card slot and reinsert
it.
When the card is properly installed, the Dionex logo on the card faces up and
the LED on the memory slot is green.

Properties cannot be changed if the compartment door is open.

This error occurs if you attempt to change column ID properties when the TC
door is open (or is not fully closed).
To troubleshoot:
1. Verify that the door is fully closed.
2. If the door is not fully closed, check for—and remove—any obstruction.

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3. If the door is fully closed but the error persists, contact Technical Support
for Dionex products for assistance.

Properties cannot be changed—there is no card in the card


reader.

This error occurs if you attempt to change column ID properties for a column
for which no chip card is installed.
To troubleshoot:
Insert a column ID chip card into the appropriate slot (see Section 9.30).

Raw data file x cannot be created.


-or-

Raw data file x cannot be created. Continuing with network failure


protection.
-or-

Raw data file x cannot be written.


-or-

Raw data file x cannot be written. Continuing with network failure


protection.

If a network failure prevents Chromeleon from creating or writing to a raw


data file, the corresponding error occurs.
To troubleshoot:
Wait until batch processing is complete; then, reboot the PC and restart the
Chromeleon server.

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Starting data acquisition manually will overwrite any data which


has been acquired so far.

This error occurs if you attempt to start data acquisition manually while a
batch is already running.
To troubleshoot:
To retain the data already acquired, cancel manual data acquisition; otherwise,
go ahead and start data acquisition.

The command can format only chip cards with an invalid data
structure.

This error occurs if you select the FormatChipCard command for a column
ID chip card that is not defective.
To troubleshoot:
Cancel the command. Do not attempt to reinitialize a chip card unless it
contains invalid or corrupted data.

The communication interface is closed. Reconnect the


instrument.

This error occurs if there is a communication failure between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.

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The compartment door is open; a batch or a program may need to


wait until the door has been closed. Please close the door.

This error occurs if you attempt to operate the TC when the door is open (or
not fully closed).
To troubleshoot:
1. Verify that the door is fully closed.
2. If the door is not fully closed, check for—and remove—any obstruction.
3. If the door is fully closed but the error persists, contact Technical Support
for Dionex products for assistance.

The counter [name] (value: x) has exceeded its limit (y). Module
should no longer be used. Replace the [name].

This error occurs if the number of hours a TC part has been in use exceeds the
lifetime set by the OperationTime.Limit property.
To troubleshoot:
Replace the part identified in the message before resuming operation.

The data format stored on the chip card is unsupported (format


version x).

This error occurs if the column ID chip card data is inadvertently saved in an
invalid format.
To troubleshoot:
1. To reinitialize the chip card, open the Chromeleon 7 ePanel Set or the
Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name and select the FormatChipCard
command.
4. For Chromeleon 6.8, click Execute.

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The injections limit for the column has been exceeded.


-or-

The injections limit will be exceeded for the column x.

Chromeleon monitors the number of injections done with each column and
display an appropriate message (shown above) at the following times: when
the injections limit is about to be exceeded or has been exceeded.
To troubleshoot:
Replace the column.

The nominal temperature must be set within the current limits.

This error occurs if the selected TC temperature setting is outside the range
specified by the Temperature.LowerLimit and Temperature.UpperLimit
commands.
To troubleshoot:
Select a valid temperature setting.

The nominal temperature value is out of range defined by the


active column ID.

This error occurs if the selected TC temperature setting is outside the range
specified by the Column_x.Temp_LowerLimit and Column_x.Temp_
UpperLimit commands.
To troubleshoot:
Select a valid temperature setting.

The oven is not fully operable yet. Check the values of “Standby,”
“Ready,” “Door,” and “CardState.”

Each time the TC power is turned on, the firmware runs a series of self-
diagnostics in which the status of the main components is checked. This error
occurs if a component is not ready for operation.

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To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Check the status of each property listed in the error message. The table
below indicates the status required for operation.

Command Status
CardState OK
Door Closed
Ready Ready
Standby NoStandby

4. When you identify the component that is not ready for operation, find and
eliminate the cause of the problem.

The primary column ID property “x” will be changed. The property


can't be changed in the future.

This error occurs when you modify a primary column property (batch or lot
number, date of manufacture, etc.). To prevent any unintended changes,
Chromeleon requests confirmation before saving the new property.
To troubleshoot:
If you are sure that the proposed change is correct, go ahead and save it.

The upper limit must be higher than the lower limit.

This error occurs if the value entered for a parameter’s upper limit (for
example, TC_Temp.Signal.UpperLimit) is less than the lower limit for the
parameter.
To troubleshoot:
Increase the value of the upper limit setting.

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The Warning threshold must be higher than the Limit threshold.

This error occurs if the Warning value selected for a Predictive Performance
command (for example, LeftRotorSealSwitches) is lower than the Limit
value. Chromeleon issues a warning message in the Audit Trail when the
Warning value is reached and an error message when the Limit value is
reached.
To troubleshoot:
Select a Warning value that is higher than the Limit value.

The Warning threshold must be lower than the Limit threshold.

This error occurs if the Warning value selected for a parameter is higher than
the Limit value. Chromeleon issues a warning message in the Audit Trail
when the Warning value is reached and an error message when the Limit
value is reached.
To troubleshoot:
Select a Warning value that is lower than the Limit value.

There was already an AcqOff command for this channel before.


-or-

There was already an AcqOn command for this channel before.


-or-

Two AcqOn commands for the same channel. The second


chromatogram will overwrite the first.

A Chromeleon 7 instrument method or Chromeleon 6.8 program can include


no more than one command to start or terminate data acquisition for a
channel; if multiple commands are present, the appropriate message (shown
above) appears.
To troubleshoot:
Remove the duplicate commands from the instrument method or program.

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This function cannot be adjusted by the user.

This error occurs if you attempt to change the setting for a read-only
parameter.
To troubleshoot:
Do not attempt to reset read-only parameters.

This operation may affect the oven's operation on timebase x,


which is currently running a batch.

If batch processing is in progress when you attempt to change a property


(such as Temperature or TempCtrl) that affects the entire TC, this error
occurs.
To troubleshoot:
To avoid disrupting operation, cancel the command.

Unknown error code.

This error occurs if Chromeleon does not recognize the error code sent by the
TC firmware.
To troubleshoot:
The firmware cannot be serviced by the user. Contact Technical Support for
Dionex products for assistance.

Unknown format of the card data.

This error occurs if Chromeleon does not recognize the format of data stored
on the column ID chip card.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.

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3. Under TC, select the column name and select the FormatChipCard
command.
4. For Chromeleon 6.8, click Execute.
5. If the error occurs again, insert a new column ID chip card (see
Section 9.30).

X position error.

This error occurs if a TC injection valve fails to switch position within the
time allotted.
To troubleshoot:
1. If a sequence is being executed, terminate the sequence by clicking Abort
Batch on the Sequence Control panel.
2. Press the POWER button on the front of the TC to turn off the power; after
30 seconds, press the button again to turn on the power.
3. Try to toggle the injection valve from Load to Inject by clicking the Load
and Inject buttons on the TC ePanel or Control panel.
4. If the error occurs again, contact Technical Support for Dionex products
for assistance.

You do not have the privilege to approve the module's


qualification.
-or-

You do not have the privilege to change the performance limits.


-or-

You do not have the privilege to change the qualification


intervals.

In controlled environments, users are not allowed to perform certain


operations unless they have been granted the appropriate privileges. If you
attempt to do so, the appropriate message (shown above) is displayed.

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To troubleshoot:
The Chromeleon 6.8 administrator assigns various privileges to individual
users or to user groups. Contact the administrator if you need one or more of
the above privileges assigned to you.

8.30 TC ALARM LED Is Lighted


If the ALARM LED lights (red), check the Chromeleon Audit Trail for the
cause.
• Gas leak inside the TC
1. Find and eliminate the leak.
2. If you are using Chromeleon 7: Open the Commands dialog box
(press the F8 key). Select the TC and click the Commands tab. Click
the ClearAlarmLED button.
3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door
and resuming operation.
• Humidity leak inside the TC
1. Find and eliminate the leak.
2. If you are using Chromeleon 7: Open the Commands dialog box
(press the F8 key). Select the TC and click the Commands tab. Click
the ClearAlarmLED button.
3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door
and resuming operation.
• Failure of a mechanical component
If a VALVE LED is flashing, a mechanical component in the TC injection
valve has failed. Replace the injection valve “pod” (see Section 9.32).
If you are using Chromeleon 7: Open the Commands dialog box (press
the F8 key). Select the TC and click the Commands tab. Click the

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ClearAlarmLED button. If you are using Chromeleon 6.8: On the TC


Control panel, click the Clear Alarm button.
If the OVEN LED is flashing, a mechanical component in the TC has
failed. These parts are not user-serviceable. Contact Technical Support for
Dionex products for assistance.

8.31 Liquid Leaks from TC Components


• Leaking fitting
Locate the source of the leak. Tighten or, if necessary, replace the liquid
line connection (see Section 9.29).
• Broken liquid line
Replace the line with tubing of the same length and internal diameter (see
Section 9.29).
• Blocked or improperly installed line
Make sure the lines are not crimped or otherwise blocked. Also, make
sure the waste line is not elevated at any point after it exits the TC. If a
line is blocked, replace it (see Section 9.29).
• Leaking injection valve
1. Make sure the liquid line connections to the valve are tight. Replace
any damaged fittings (see Section 9.29).
2. Liquid leaks from behind the valve stator may indicate a scratched
rotor seal. Rebuild the injection valve (see Section 9.31).
• Leaking temperature stabilizer
1. Tighten the fittings on the temperature stabilizer inlet and outlet.
2. If tightening the fittings does not eliminate the leak, excessive system
backpressure may be the source of the problem. Follow the
troubleshooting steps in Section 8.9 to reduce the backpressure.

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8.32 TC Temperature Does Not Increase


If the temperature fails to increase as expected, although the temperature set
point has not been reached, follow the troubleshooting steps below.
• Front door not closed
Verify that the TC door is fully closed. If it is, check the door seal for
signs of damage. If the seal is damaged, contact Technical Support for
Dionex products for assistance.
• Column tubing connections incorrectly oriented
Column tubing connections that are incorrectly oriented can open a small
path for ambient air into the TC. Check that the tubing connections are at
a 90-degree angle in relation to the door seal.
• Ventilation slots on TC are obstructed
Make sure the ventilation slots are not obstructed in any way. Allow at
least 6 cm (2.4 in) behind the TC for ventilation.
• Ambient temperature is too high
Reduce the ambient temperature (for example, ventilate the lab in which
the TC is installed).

8.33 TC Temperature Stabilizer Not Operating Properly


• Temperature stabilizer installed incorrectly
Remove the temperature stabilizer and install it correctly. Make sure there
is good thermal contact between the temperature stabilizer and the
thermal element. For detailed instructions, refer to Thermo Scientific
Dionex ICS-5000 Ion Chromatography System Installation Instructions
(Document No. 065343).
• TC calibration is incorrect
The TC cannot be calibrated by the user. Contact Technical Support for
Dionex products for assistance.
• Defective temperature stabilizer
Replace the temperature stabilizer (standard bore, P/N 064548;
microbore, P/N 064650).

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9 • Service

This chapter describes Thermo Scientific Dionex ICS-5000 Ion


Chromatography System service and repair procedures that users may
perform. All procedures not included here, including electronics-related repair
procedures, must be performed by Thermo Fisher Scientific personnel. For
assistance, contact Technical Support for Dionex products. In the U.S. and
Canada, call 1-800-346-6390. Outside the U.S. and Canada, call the nearest
Thermo Fisher Scientific office.
Before replacing any part, refer to the troubleshooting information in
Chapter 8 to correctly identify the cause of the problem.
Substituting non-Dionex/Thermo Fisher Scientific parts may impair a
module’s performance, thereby voiding the product warranty. Refer to
the warranty statement in the Dionex Terms and Conditions for more
information.

Capillary 9.1 Connecting Capillary Tubing


IC
When connecting precision cut 0.062 mm (0.0025 in) ID blue PEEK tubing
(capillary tubing) to a port, make sure the ferrule and fitting bolt are at least
2 mm (0.1 in) from the end of the tubing before you insert the tubing into the
port. Do not position the ferrule and fitting bolt flush with the end of the
tubing.

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Figure 9-1 illustrates the correct and incorrect placement of the ferrule and
fitting bolt on the tubing.

Correct Incorrect
2 mm

Figure 9-1. Correct and Incorrect Ferrule and Fitting Bolt Placement for
Capillary Tubing Connections (High-Pressure Fitting and Ferrule Shown)

Follow the steps below to install capillary tube fittings:


1. Install the fitting bolt and ferrule onto
the tubing. Position the ferrule at least
2 mm (0.1 in) from the end of the
tubing (see Figure 9-1).

2. Insert the tubing into the port until it


stops.

3. While maintaining pressure on the


tubing to keep it in place in the port,
tighten the fitting bolt fingertight.
4. If you are installing a high-pressure
fitting (blue bolt and ferrule), follow
the instructions below to tighten the
fitting.

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Capillary 9.2 Tightening Guidelines for High-Pressure Fittings
IC
Follow these guidelines when tightening a high-pressure fitting bolt
(P/N 074449) and high-pressure ferrule (P/N 074373):
1. First, use your fingers to tighten the fitting bolt as tight as you can. Then,
use a wrench to tighten the fitting an additional 3/4 turn (270 degrees).
2. If leaks occur, replace the fitting bolt, ferrule, and tubing.

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ICS-5000
DP/SP DP/SP Service

9.3 Replacing Tubing and Fittings


The DP/SP is plumbed with the tubing and fittings listed below.

Tubing Size and Type Color P/N Used to connect…


Pump outlet tubing Black 068658 Pulse damper outlet
assembly: 0.25 mm (capillary pumps) or static
(0.010 in) ID PEEK, valve outlet (standard bore
86 cm (34 in) analytical pumps) to EGC
inlet or injection valve
0.125 mm (0.005 in) ID Red 044221 Microbore analytical pumps
PEEK, 86 cm (34 in) (1 in) only: Static valve outlet to
EGC inlet or injection valve
0.25 mm (0.010 in) ID Black 042690 Primary and secondary
PEEK, 10 cm (4 in) (1 in) pump heads
0.51 mm (0.020 in) ID Orange 042855 Microbore systems only:
PEEK, 13 cm (5 in) (1 in) Proportioning/eluent valve to
inlet check valve
1.02 mm (0.040 in) ID Tan 054410 Standard bore systems only:
PEEK, 13 cm (5 in) (1 in) Proportioning/eluent valve to
inlet check valve
0.159 cm (0.0625 in) Yellow 063268 Peristaltic pump to primary
ID PharMed® (1 in) pump head
0.15 cm (0.060 in) ID Colorless 064079 • Peristaltic pump to seal
Tygon® 2075 tubing (1 in) wash reservoir
• Between pump heads for
seal wash
1.58 mm (0.062 in) ID Colorless 014157 • Eluent reservoirs
PTFE (1 in) • Vacuum degassing
assembly
1.58 mm (0.062 in) ID Colorless 047203 Secondary pump head to
polyurethane (1 in) waste

Table 9-1. DP/SPTubing and Fittings

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9 • DP/SP Service

Tubing Size and Type Color P/N Used to connect…


10 mm (0.39 in) ID Colorless 055075 Drip tray drain hose
polyethylene
1/16 in fitting bolt Tan 052230 Inlet check valve fitting
1/16 in ferrule Tan 062511
1/8 in fitting bolt Tan 052267 Eluent reservoir fittings
1/8 in ferrule Yellow 048949
High-pressure 10-32 Blue 074449 Capillary pumps only: Pulse
fitting bolt damper to EGC or injection
valve
High-pressure 10-32 Blue 074373 Use with high-pressure fitting
ferrule, double-cone bolts
10-32 fitting bolt Black 043275 All other tubing fittings
10-32 ferrule, double- Tan 043276
cone

Table 9-1. DP/SPTubing and Fittings (Continued)

Notes

• For tightening requirements for the 10-32 fitting bolt (P/N 043275) and
ferrule (P/N 043276), refer to Installation of Dionex Liquid Line Fittings
(Document No. 031432). The manual is on the Thermo Scientific
Reference Library DVD (P/N 053891).
• For tightening requirements for the high-pressure fitting bolt
(P/N 074449) and ferrule (P/N 074373), see Section 9.2.
• Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing and there are no nicks or burrs
on the end. A tubing cutter (P/N 049584) is included in the DC Ship Kit
(P/N 072011). Refer to the instructions provided with the cutter.

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9.4 Cleaning Eluent Reservoirs


Before preparing new eluent, all eluent reservoirs should be rinsed thoroughly
(inside and out) with ASTM Type I (18 megohm-cm) filtered and deionized
water that meets the specifications listed in Section 1.5. If a reservoir still
appears dirty, or has a slimy film on the inside, clean it as instructed below.
Capillary Clean reservoirs in a capillary IC system every 3 months, as instructed below.
IC
1. Dispose of any remaining chemicals according to municipal regulations.
2. Rinse the reservoir (inside and out) with ASTM Type I (18 megohm-cm)
filtered and deionized water.
3. Rinse the inside of the reservoir with isopropyl alcohol or methanol.
4. If algae or bacteria have left a slimy film on the reservoir, use an algicide
or disinfectant (dilute hydrogen peroxide, etc.).
5. Rinse cleaning chemicals out of the reservoir with ASTM Type I
(18 megohm-cm) filtered and deionized water.
6. Dry the reservoir with clean, particulate-free air.

9.5 Priming the DP/SP


The pump should be primed if the eluent has been changed, the eluent line is
new (empty), or the eluent line contains air. This section describes two
methods for priming the pump:
• To prime the pump with the PUMP PRIME button, see Section 9.5.1.
• To prime the pump from the Pump panel in Chromeleon, see
Section 9.5.2.
Although a 10 cc syringe (P/N 054578) can be used with either priming
procedure, using a syringe only if eluent lines are 100% empty or if the pump
is dry is recommended.

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9 • DP/SP Service

9.5.1 Priming with the PUMP PRIME Button


1. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the Pump tab.
2. Gradient pump only: Enter 100% for the channel (A, B, C, or D) to be
primed.
3. Set the priming flow rate to the desired rate. The default rate for a
capillary IC pump is 3.0 mL/min. The default rate for an analytical IC
pump is 6.0 mL/min.
4. Disconnect the DP/SP from the software by clicking Connected on the
Pump panel.

NOTE When the pump is connected to Chromeleon, the


PUMP PRIME buttons are disabled.

5. Open the priming valve on the secondary pump head (see Figure 9-2) by
turning it one-half turn counterclockwise.

NOTE If the priming valve is opened too much, air is drawn


through the valve and air bubbles can be seen exiting
the waste line.

1 Priming Valve

2 Secondary Pump Head


1
3 Priming Waste Line
2

Figure 9-2. DP/SP Priming Valve

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6. Press PUMP PRIME 1 (or PUMP PRIME 2) on the front of the DP/SP. The
pump will begin pumping at the priming flow rate selected on the
Chromeleon panel.
7. Prime the pump until all air is purged and no air bubbles can be seen
exiting the waste line.
8. Gradient pump only: To prime additional eluent lines, select another
eluent channel and repeat the priming procedure.
9. After priming all eluent lines, press PUMP PRIME 1 (or PUMP PRIME 2) to
stop priming and return to the flow rate last selected.
10. Close the priming valve by turning it clockwise. Do not overtighten the
priming valve.
Do not use any tools to tighten the priming valve! Overtightening may
destroy the cap seal. Open or close the priming valve only when the
system pressure is down.

11. Reconnect the pump to the software by clicking Connected on the Pump
panel.

9.5.2 Priming from the Chromeleon Panel


1. Open the priming valve on the secondary pump head (see Figure 9-2) by
turning it one-half turn counterclockwise.

NOTE If the priming valve is opened too much, air is drawn


through the valve and air bubbles can be seen exiting
the waste line.

2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the Pump tab.
3. Gradient pump only: Enter 100% for the channel (A, B, C, or D) to be
primed.
4. Set the priming flow rate to the desired rate. The default rate for a
capillary IC pump is 3.0 mL/min. The default rate for an analytical IC
pump is 6.0 mL/min.
5. Click the Prime button on the Pump panel. A warning message asks you
to verify that the purge (priming) valve is open. Click Execute despite
warnings (Chromeleon 7) or OK (Chromeleon 6.8). Priming starts.

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9 • DP/SP Service

6. Prime the pump until all air is purged and no air bubbles can be seen
exiting the waste line. Click the Prime button to stop priming.

NOTE Priming will stop automatically after the number of


seconds specified in the Duration box have elapsed.
You can set the duration to a preferred value.

7. Gradient pump only: To prime additional eluent lines, select another


eluent channel and repeat the priming procedure.
8. Close the priming valve by turning it clockwise. Do not overtighten the
priming valve.
Do not use any tools to tighten the priming valve! Overtightening may
destroy the cap seal. Open or close the priming valve only when the
system pressure is down.

9. Enter the flow rate required for your application.


10. Gradient pump only: Enter the required proportions of eluents A, B, C,
and D on the Pump panel.
11. Turn on the pump flow.

NOTE After starting the pump, wait at least 5 minutes (longer


for flow rates below 1.0 mL/min) before beginning an
analysis. This allows the DP/SP to stabilize the flow
rate.

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9.6 Replacing the Check Valves


A dirty check valve causes erratic flow rates and pressures; in addition, it may
cause the pump to lose prime and/or be difficult to reprime. If a check valve
leaks or is dirty, it should be replaced.
Capillary IC pumps and analytical IC pumps use different check valves.
Verify that you have the correct check valve assembly for your pump type
(see Table 9-2).

Pump Type Check Valve Assembly Part Number


Capillary IC Inlet 044541
Outlet 044540
Analytical IC Inlet 045722
Outlet 045721

Table 9-2. DP/SP Check Valve Assemblies

Before beginning, locate the 1/2-inch wrench (P/N 062336) in your pump
ship kit:

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

Additional items:
• Cleanroom gloves (lint-free, particle-free, and oil-free)
• 0.2 micron filtered, Class 10, isopropyl alcohol (IPA)
• 0.2 micron filtered, canned air duster (ITW Chemtronics Ultrajet® or
equivalent)

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9 • DP/SP Service

9.6.1 Removing the Check Valves


1. Turn off the pump flow.
2. Begin monitoring the Current Pressure reading on the Pump panel on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset. When the
system pressure reaches zero, do the following:
• Disconnect the pump from the software by clicking Connected on
the Pump panel.
• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Open the DP/SP door to access the mechanical components.
4. Five red Phillips screws are installed on the component mounting panel
before shipment from the factory. Remove these screws, if present.
5. Use the handles on the component mounting panel to pull the panel
forward until it reaches the stop.
6. To prevent contamination of pump parts, wear cleanroom gloves while
disassembling the pump head.
Never disassemble the pump head with bare hands. Even minute
particles of dust, dirt, etc., on the check valves or piston can
contaminate the inside of the pump head and result in poor pump
performance.

7. The check valves are installed in the primary pump head (see Figure 9-3).

1 Outlet Check Valve

1 2 Primary Pump Head

3 Inlet Check Valve

Figure 9-3. DP/SP Check Valves

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8. Disconnect the tubing connections from the inlet and outlet check valves.
9. Loosen both check valve assemblies using the 1/2-inch wrench
(P/N 062336).
10. Remove both check valve assemblies from the pump head.

9.6.2 Installing the New Check Valves


1. The inlet check valve assembly
housing has a 1/4-28 port. Inlet Check Valve
1/4-28 Port

Inspect the new inlet check valve Double-hole


assembly to verify that the double-
hole end of the cartridge (see Inlet Check Valve
Figure 9-4) is visible. Assembly

If the double-hole end is not visible,


remove the cartridge from the
Flow
housing and install it correctly.
Figure 9-4. Inlet Check Valve Assembly

2. The outlet check valve assembly


housing has a smaller, 10-32 port. Outlet Check Valve
10-32 Port

Inspect the new outlet check valve Single-hole


assembly to verify that the single-
Outlet Check
hole end of the cartridge is visible Valve Assembly
(see Figure 9-5).

If the single-hole end is not visible,


remove the cartridge from the
Flow
housing and install it correctly.
Figure 9-5. Outlet Check Valve Assembly

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9 • DP/SP Service

NOTE The pump cannot operate properly unless the car-


tridges are installed in their respective housings in the
correct orientation. Liquid enters through the check
valve in the large single hole and exits through the
small double holes.

3. Before installing the inlet and outlet check valves, rinse the bottom of the
check valve ports in the pump head with isopropyl alcohol and blow them
clean using a 0.2 micron filtered, canned air duster. Inspect the bottom of
each port for any particulate matter. If necessary, rinse and dry again until
they are clean.
4. Install the inlet check valve assembly on the bottom of the primary pump
head. Install the outlet check valve assembly on the top of the pump head.
5. Tighten the check valves fingertight, and then use the 1/2-inch wrench to
tighten an additional one-quarter to one-half turn.
Overtightening may damage the pump head and check valve housing
and crush the check valve seats.

6. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
7. Press the POWER button on the front of the DP/SP to turn on the pump.
8. Reconnect the pump to the software by clicking Connected on the Pump
panel.

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9.7 Replacing Piston Seals


A defective piston seal allows leakage past the piston. This may cause
unstable flow rates and baseline noise; in addition, it may make it difficult to
prime the pump.
The piston seal replacement procedure consists of:
• Removing the pump head and piston (Section 9.7.1)
• Cleaning the piston (Section 9.7.2)
• Removing the main piston seal (Section 9.7.3)
• Removing the piston seal wash seal (Section 9.7.4)
• Installing new seals (Section 9.7.5)
• Reinstalling the piston and pump head (Section 9.7.6)

NOTE Capillary IC pumps and analytical IC pumps use different


main piston seals and piston seal wash seals. Before continu-
ing, verify that you have the correct seal for your pump type.
Part numbers are shown on Figure 9-6 and Figure 9-7.

Before beginning, locate the following items in your pump ship kit:
• 3.0 mm hex key (P/N 062338)
• 10-32 fitting plugs (P/N 042772)
• 10 cc syringe (P/N 054578)
• Seal insertion tool (P/N 063675)

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

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9 • DP/SP Service

Additional items:
• Cleanroom gloves (lint-free, particle-free, and oil-free)
• Small beaker
• ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5
• Methanol (optional)
• 0.2 micron filtered, Class 10, isopropyl alcohol (IPA)
• Lint-free paper towels (KIMWIPES® or equivalent)
• Large flat-blade screwdriver
• 0.2 micron filtered, canned air duster (ITW Chemtronics Ultrajet or
equivalent)

9.7.1 Removing the Pump Head and Piston


1. Turn off the pump flow.
2. Begin monitoring the Current Pressure reading on the Pump panel on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset. When the
system pressure reaches zero, do the following:
• Disconnect the pump from the software by clicking Connected on
the Pump panel.
• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Open the DP/SP door to access the mechanical components.
4. Five red Phillips screws are installed on the component mounting panel
before shipment from the factory. Remove these screws, if present.
5. Use the handles on the component mounting panel to pull the panel
forward until it reaches the stop.

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6. To prevent contamination of pump parts, wear cleanroom gloves while


disassembling and reassembling the pump head.
Never disassemble the pump head with bare hands. Even minute
particles of dust, dirt, etc., on the check valves or piston can
contaminate the inside of the pump head and result in poor pump
performance.

7. Disconnect all tubing connections to the pump head with the defective
piston seal.
8. The primary and secondary pump heads have different components.
When disassembling a pump head, refer to Figure 9-6 for a primary pump
head or Figure 9-7 for a secondary pump head.

Note: Each check


9 valve assembly
B includes a valve
body (B) and a
8 cartridge (C).
C

7
6
4
3
2
C
1

10 B

4 Seal Wash Body


P/N 074446 (Capillary)
P/N 062064 (Analytical)
1 Piston 5 8 Primary Pump Head
P/N 068646 (Capillary) P/N 074447 (Capillary)
P/N 062082 (Analytical) P/N 062083 (Analytical)
2 Seal Retainer 6 Backup Ring 9 Outlet Check Valve Assembly
P/N 068627 (Capillary) P/N 074371 P/N 044540 (Capillary)
P/N 062092 (Analytical) (Capillary only) P/N 045721 (Analytical)
3 Piston Seal Wash Seal 7 Main Piston Seal 10 Inlet Check Valve Assembly
P/N 068628 (Capillary) P/N 075493 (Capillary) P/N 044541 (Capillary)
P/N 063382 (Analytical) P/N 064946 (Analytical) P/N 045722 (Analytical)

Figure 9-6. DP/SP Pump: Primary Pump Head Assembly

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9 • DP/SP Service

12
8 10
11

5
7
6
4
3
8 Secondary Pump Head
2 P/N 074240 (Capillary)
P/N 062079 (Analytical)
1
4 Seal Wash Body 9 Priming Valve
P/N 074446 (Capillary) P/N 063968
P/N 062064 (Analytical) (Capillary and Analytical)
1 Piston 5 10 Priming Valve Seal
P/N 068646 (Capillary) P/N 063382
P/N 062082 (Analytical) (Capillary and Analytical)

2 Seal Retainer 6 Backup Ring 11 Membrane


P/N 068627 (Capillary) P/N 074371 P/N 062081
P/N 062092 (Analytical) (Capillary only) (Capillary and Analytical)
3 Piston Seal Wash Seal 7 Main Piston Seal 12 Pressure Transducer
P/N 068628 (Capillary) P/N 075493 (Capillary) Assembly; P/N 062057
P/N 063382 (Analytical) P/N 064946 (Analytical) (Capillary and Analytical)

Figure 9-7. DP/SP: Secondary Pump Head Assembly

9. Using a 3.0 mm hex key (P/N 062338), loosen the two screws on the
pump head with the defective seal. Remove the screws, and then carefully
remove the head and place it on a clean surface.
10. Remove the seal wash body from the pump head. Or, if the seal wash
body was not removed with the pump head in Step 9, pull it straight out of
the pump mechanism now.
11. Pull the piston out of the pump mechanism.

NOTE A magnet secures the piston in place. If the magnetic


force makes the piston difficult to remove, tilt the pis-
ton to one side and then pull it out of the pump mecha-
nism.

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9.7.2 Cleaning the Piston


1. Place the piston in a beaker containing either ASTM Type I
(18 megohm-cm) filtered and deionized water or methanol. Sonicate for
several minutes.
2. After cleaning, rinse the piston thoroughly with ASTM Type I
(18 megohm-cm) filtered and deionized water. Dry it with a lint-free
paper towel.
3. Inspect the piston for signs of damage. If the piston is scratched or scored,
replace it (see Section 9.8).
Even minute scratches or particles of dust, dirt, etc. on the check
valves or piston can contaminate the inside of the pump head and
result in poor pump performance.

9.7.3 Removing the Main Piston Seal


1. If this is the primary pump head, insert a 10-32 fitting plug (P/N 042772)
into the 10-32 outlet hole of the check valve nut.
2. If this is the secondary pump head, insert a 10-32 fitting plug
(P/N 042772) into both the 10-32 inlet and outlet holes.
3. Using a 10 cc syringe (P/N 054578), inject a few drops of ASTM Type I
(18 megohm-cm) filtered and deionized water through the main piston
seal and into the piston cavity in the pump head.
4. Reinsert the piston approximately 3 mm (0.125 in) into the piston seal and
press gently. The seal should pop out of the head and onto the piston.
Do not use a sharp tool (such as tweezers) to remove the piston seal.
This will scratch the inside of the pump housing; these scratches will
prevent a proper seal and cause leakage.

5. If the piston seal was not removed in Step 4, follow these steps:
a. Verify that the 10-32 fitting plugs in the inlet and outlet holes are
tightened enough to prevent any leaks from the pump head.
b. Fill the piston cavity with water and check for bubbles.
c. If there are no bubbles, repeat Step 4.

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9.7.4 Removing the Piston Seal Wash Seal


1. Remove the O-ring (P/N 040695) from the seal wash body. If this is a
capillary pump, also remove the backup ring.
2. Follow these steps to remove the piston seal wash seal from the seal wash
body:
a. Using a large flat-blade screwdriver, remove the retainer
(P/N 062092) for the seal from the seal wash body.
b. Insert the piston into the seal wash body from the O-ring side and
gently push the seal out of the retainer.
Do not use a sharp tool (such as tweezers) to remove the piston seal
wash seal. This may scratch the seal and the inside of the pump
housing; scratches will prevent a proper seal and cause leakage.

9.7.5 Installing the Piston Seals and O-Ring


1. Follow these steps to reassemble the seal wash body:
a. Place the seal wash body on a clean work surface.
b. Slide the new seal wash seal, with the open side of the seal facing
upward, onto the seal insertion tool (P/N 063675) (see Figure 9-8).

Piston Seal Wash Seal


P/N 068628 (Capillary)
P/N 063382 (Analytical)

Seal Insertion Tool


(P/N 063675)

Figure 9-8. Piston Seal Wash Seal and Seal Insertion Tool

c. Insert this end of the tool partway into the seal wash body. Make sure
the tool is centered and does not rock back and forth. Then, press
firmly on the tool and the seal wash body until they snap together.
d. Remove the seal insertion tool from the seal wash body.

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e. The seal wash seal is now partially installed. To complete the seal
installation, place the retainer in the seal wash body and use the large
flat-blade screwdriver to tighten the retainer.
f. Place the new O-ring (P/N 040695) on the seal wash body.

NOTE When replacing a piston seal, always replace the O-


ring, also. This will prevent leaks.

g. If this is a capillary IC pump, place the new backup ring


(P/N 074371) on the seal wash body.
2. Rinse the new main piston seal (P/N 075493, for capillary pump;
P/N 064946, for analytical pump) with isopropyl alcohol (IPA) or dip it
into a container of IPA. (The seal is easier to install when it is moist.)
3. Insert the piston through the seal wash assembly, and then through the
new main piston seal.
4. Make sure the piston seal is centered.
If the piston seal is not centered, applying pressure to it in Step 7 will
damage the seal and make it unusable.

5. Place the front of the pump head, flat side down, on a clean work surface.
Make sure the open side of the piston seal faces away from the retainer for
the seal wash seal.
6. Using IPA, rinse inside the pump head cavity where the seal will be
installed. Blow inside the cavity to dry it using the 0.2 micron filtered,
canned air duster. Inspect the cavity for any particulate matter. If
necessary, rinse and dry again, until the cavity is clean. Fill the cavity
with ASTM Type I (18 megohm-cm) filtered and deionized water.
7. Place the components on the pump head and gently press the housing until
the piston seal snaps into place.
When pressing the seal in place, ensure that the piston is free to move out,
to relieve the pressure in the pump head during seal installation.
Do not use a sharp tool (such as tweezers) to install the piston seal.
This will scratch the seal and the inside of the pump housing; these
scratches will prevent a proper seal and cause leakage.

8. Remove the 10-32 fitting plugs from the pump head.

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9.7.6 Reinstalling the Piston and Pump Head


1. Slide the piston partway into the pump head; approximately 6 mm
(1/4 in) of the sapphire part of the piston should extend from the head.
2. Place the pump head back on the pump.
3. Reinstall the screws in the pump head. Using the 3.0 mm hex key
(P/N 062338), tighten the screws just until they come into contact with
the pump head. Then, tighten the screws another one-quarter to one-half
turn, one-eighth of a turn at a time.
4. Reconnect all tubing connections to the pump head. Tighten connections
fingertight, and then tighten an additional one-quarter turn only.
5. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
6. Press the POWER button on the front of the DP/SP to turn on the pump.
7. Reconnect the pump to the software by clicking Connected on the Pump
panel.
8. Turn on the pump flow.

9.8 Replacing the Piston


If a new piston seal leaks (assuming that the pump head is tight), it indicates
that the piston is dirty, scratched, or broken, and should be replaced.
The piston replacement procedure consists of:
• Removing the pump head and the old piston (see Section 9.8.1)
• Reinstalling a new piston (see Section 9.8.2)
• Reinstalling the pump head (see Section 9.8.3)

NOTE Capillary IC pumps and analytical IC pumps use different


pistons. Before continuing, verify that you have the correct
piston for your pump type: P/N 068646 (for capillary),
P/N 062082 (for analytical).

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Before beginning, locate the 3.0 mm hex key (P/N 062338) in your pump ship
kit:

Pump Ship Kit Part Number


DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

Additional items:
• Cleanroom gloves (lint-free, particle-free, and oil-free)
• ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5

9.8.1 Removing the Pump Head and Piston


When disassembling and reassembling the pump head, refer to Figure 9-6
(primary pump head) or Figure 9-7 (secondary pump head).
1. Turn off the pump flow.
2. Begin monitoring the Current Pressure reading on the Pump panel on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset. When the
system pressure reaches zero, do the following:
• Disconnect the pump from the software by clicking Connected on
the Pump panel.
• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Open the DP/SP door to access the mechanical components.
4. Five red Phillips screws are installed on the component mounting panel
before shipment from the factory. Remove these screws, if present.
5. Use the handles on the component mounting panel to pull the panel
forward until it reaches the stop.

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9 • DP/SP Service

6. To prevent contamination of pump parts, wear cleanroom gloves while


disassembling the pump head.
Never disassemble the pump head with bare hands. Even minute
particles of dust, dirt, etc., on the check valves or piston can
contaminate the inside of the pump head and result in poor pump
performance.

7. Disconnect all tubing connections to the pump head with the damaged
piston.
8. Using a 3.0 mm hex key (P/N 062338), loosen the Allen screws on the
pump head with the damaged piston. Remove the Allen screws, and then
carefully remove the head and place it on a clean surface.
9. If the piston was not removed with the pump head in Step 8, remove the
piston now by pulling it straight out of the pump mechanism.

NOTE A magnet secures the piston in place. If the magnetic


force makes the piston difficult to remove, tilt the pis-
ton to one side and then pull it out of the pump mecha-
nism.

10. If the piston is broken, be sure to remove all broken pieces. If necessary,
flush the pump head with ASTM Type I (18 megohm-cm) filtered and
deionized water.

9.8.2 Reinstalling the New Piston


Slide the new piston (P/N 068646, for capillary; P/N 062082, for analytical)
partway into the pump head; approximately 6 mm (1/4 in) of the sapphire part
of the piston should extend from the head.

9.8.3 Reinstalling the Pump Head


1. Place the pump head back on the pump.
2. Reinstall the screws in the pump head. Using the 3.0 mm hex key
(P/N 062338), tighten the screws just until they come into contact with
the pump head. Then, tighten the screws another one-quarter to one-half
turn, one-eighth of a turn at a time.

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3. Reconnect all tubing connections to the pump head. Tighten connections


fingertight, and then tighten an additional one-quarter turn only.
4. Push the component mounting panel back into the enclosure, using the
handle in the center of the panel. Close the DP/SP door.
5. Press the POWER button on the front of the DP/SP to turn on the pump.
6. Reconnect the pump to the software by clicking Connected on the Pump
panel.
7. Turn on the pump flow.

9.9 Replacing the Piston Seal Wash Tubing


Check the piston seal wash tubing weekly for crimping or blockage and
replace as needed.
1. Turn off the pump flow.
2. Five red Phillips screws are installed on the component mounting panel
before shipment from the factory. Remove these screws, if present.
3. Open the DP/SP door and then use the handles on the component
mounting panel to pull the panel forward until it reaches the stop.
4. Remove the old tubing from the peristaltic pump (see Figure 9-9) as
follows:
a. Lift the lever up and to the right and hold it in that position with one
hand.
b. With your other hand, pull the PharMed tubing away from the rotor
and out of the lower notch on the left side of the mounting plate.
c. Release the lever.

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9 • DP/SP Service

d. Pull on the fitting slightly to remove the PharMed tubing from the
upper notch on the pump mounting plate.

PharMed Tubing
1 (P/N 063268)

2 Rotor

6 1 3 Lever

4 Mounting Plate
2
5 Tygon 2075 Tubing
3 5 (P/N 064079)

4 6 Fitting

Figure 9-9. Peristaltic Pump for Seal Wash System

5. Pull off the PharMed and Tygon 2075 tubing from the fitting. Save the
fitting.
6. Pull off all seal wash tubing from the seal wash reservoir and the primary
and secondary pump heads(see Figure 9-10).
7. Cut three new pieces of Tygon 2075 tubing (0.15 cm (0.060 in) ID;
P/N 064079) and one piece of PharMed tubing (0.159 cm (0.0625 in) ID;
P/N 063268) to the same lengths as the tubing just removed. The tubing is
included in the pump ship kit:
Pump Ship Kit Part Number
DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342

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8. Connect the new tubing pieces


to the seal wash reservoir and
pump heads (see Figure 9-10).
PharMed
9. Push the tubing onto the fitting Tubing
that was removed in Step 5.
10. Connect the PharMed tubing to
the peristaltic pump as follows: Tygon 2075
Tubing
a. Push the tubing into the
lower notch on the pump
mounting plate.
b. Lift the lever to the right and
hold it in that position with Seal
one hand. Wash
Reservoir
c. With your other hand, wind
the tubing around the rotor. Secondary Primary
Head Head
d. Release the lever.

Figure 9-10. Piston Seal Wash Tubing Connections

e. Pull on the fitting slightly to slide the tubing into the upper notch.
f. Make sure there is no slack in the tubing. If necessary, lift the lever
again, adjust the tubing around the rotor and through the lower notch
to remove any slack, and release the lever.
11. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
12. Turn on the pump flow.

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9 • DP/SP Service

9.10 Replacing the DP/SP Priming Valve Knob Seal


Replace the seal in the priming valve knob if there is leakage around the valve
threads when the valve is open or if the waste port leaks when the valve is
closed.
1. Turn off the pump flow.
2. Begin monitoring the Current Pressure reading on the Pump panel on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset. When the
system pressure reaches zero, do the following:
• Disconnect the pump from the software by clicking Connected on
the Pump panel.
• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Open the front door of the DP/SP.
4. Five red Phillips screws are installed on the component mounting panel
before shipment from the factory. Remove these screws, if present.
5. Use the handles on the component mounting panel to pull the panel
forward until it reaches the stop.
6. The priming valve knob is located on the secondary pump head (see
Figure 9-11). To remove the knob, turn it counterclockwise all the way
and then pull it straight off the pump head.

1 Priming Valve

Secondary
1 2
Pump Head

Figure 9-11. DP/SP Priming Valve

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7. Pull the old seal off the end of the priming valve knob.
8. Hold the new seal (P/N 063382) with the groove in the priming valve seal
facing away from the knob (see Figure 9-12). Carefully slide the seal onto
the knob; avoid scratching or nicking the sides.
Do not use a sharp tool (such as tweezers) to install the seal. This may
scratch the seal and the surface of the priming valve knob. These
scratches will prevent a proper seal and cause leakage.

Priming Valve Seal


(P/N 063382)

Insert seal with


groove facing
away from knob

Figure 9-12. Replacing the Priming Valve Seal

9. Insert the priming valve knob into the secondary pump head, turn the
knob clockwise, and tighten fingertight.
10. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
11. Press the POWER button on the front of the DP/SP to turn on the pump.
12. Reconnect the pump to the software by clicking Connected on the Pump
panel.
13. Turn on the pump flow.

9.11 Changing the DP/SP Main Power Fuses


1. Turn off the pump flow.
2. Begin monitoring the Current Pressure reading on the Pump panel on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset. When the
system pressure reaches zero, do the following:
• Disconnect the pump from the software by clicking Connected on
the Pump panel.

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9 • DP/SP Service

• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Turn off the main power switch on the rear panel of the pump (see
Figure 2-7).
4. Disconnect the main power cord from both its source and from the rear
panel of the pump.

HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the pump.

HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa


source et du panneau arrière du pump.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und


der Netzbuchse auf der Rückseite der Pumpe.

5. The fuse cartridge is located next to the


main power switch (see Figure 9-13).
Use a small screwdriver to remove the
fuse cartridge.
6. Replace the two fuses with new 2 A IEC
60127-2 slow-blow fuses (P/N 954773).
Fuse
Thermo Fisher Scientific recommends Cartridge
always replacing both fuses.
7. Reinstall the fuse cartridge.
8. Reconnect the main power cord to its
source and to the DP/SP.
Figure 9-13. DP/SP Fuse Cartridge

9. Turn on the main power switch.


10. Press the POWER button on the front of the DP/SP to turn on the pump.
11. Reconnect the pump to the software by clicking Connected on the Pump
panel.
12. Turn on the pump flow.

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ICS-5000
EG EG Service

9.12 Replacing Tubing and Fittings

Capillary 9.12.1 Tubing and Fittings for Capillary IC EG Channels


IC
Table 9-4 lists the tubing and fittings used to plumb an EG channel for
capillary IC.

Tubing/Fitting Size Color P/N Use to connect…


and Type
Tubing assembly, Blue 072203 CR-TC ELUENT OUT to EG
precision cut, degas ELUENT IN
0.062 mm (0.0025 in)
ID PEEK, 61 cm (24 in)
Tubing assembly, Blue 072204 CR-TC ELUENT IN to EGC
precision cut, OUT
0.062 mm (0.0025 in)
ID PEEK, 18 cm (7 in)
Tubing assembly, Black 072224 EG degas REGEN OUT to
0.25 m (0.010 in) ID CR-TC REGEN IN
PEEK, 64 cm (25 in)
Tubing assembly, Clear 072225 CR-TC REGEN OUT to waste
1.58 mm (0.062 in) ID
ETFE, 2.1 m (7 ft)
10 mm (0.39 in) ID Colorless 055075 Drip tray drain hose
polyethylene
High-pressure 10-32 Blue 074449 Use high-pressure fittings for:
fitting bolt • Pump outlet to EGC IN
• EGC OUT to CR-TC
ELUENT IN
• CR-TC ELUENT OUT to
EG degas ELUENT IN
High-pressure 10-32 Blue 074372 Use with high-pressure fitting
ferrule, double-cone bolts

Table 9-3. Tubing and Fittings for a Capillary IC EG Channel

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Tubing/Fitting Size Color P/N Use to connect…


and Type
10-32 fitting bolt Black 043275 All other tubing connections
10-32 ferrule, double- 043276
cone

Table 9-3. Tubing and Fittings for a Capillary IC EG Channel

Capillary Notes for capillary IC channels:


IC
• Do not cut the 0.062 mm (0.0025 in) ID blue PEEK tubing used for
capillary IC connections. This tubing must be cut at the factory using a
specialized precision cutter. This ensures good chromatographic results. If
you need to replace any tubing of this type, order the appropriate
precision cut tubing assembly listed in Table 9-3.
• When replacing capillary tubing, make sure the ferrule and fitting bolt are
at least 2 mm (0.1 in) from the end of the tubing before you insert the
tubing into the port. Do not position the ferrule and fitting bolt flush with
the end of the tubing. For detailed connection instructions, see
Section 9.1.
• For tightening requirements for the high-pressure fitting bolt
(P/N 074449) and ferrule (P/N 074373), see Section 9.2.
• For tightening requirements for the 10-32 fitting bolt (P/N 043275) and
ferrule (P/N 043276), refer to Installation of Dionex Liquid Line Fittings
(Document No. 031432). The manual is on the Thermo Scientific
Reference Library DVD (P/N 053891).

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9 • EG Service

9.12.2 Tubing and Fittings for Analytical IC EG Channels


Table 9-4 lists the tubing and fittings used to plumb an EG channel for
analytical IC.

Tubing/Fitting Size Color P/N Used to connect…


and Type
0.25 mm (0.010 in) ID Black 042690 • EGC to pump
PEEK tubing (1 in) • EGC to CR-TC
• RFIC Eluent Degasser to
injection valve
• RFIC Eluent Degasser to
eluent reservoir
1.6 mm (0.062 in) ID Colorless 014157 • RFIC Eluent Degasser
PTFE tubing (1 in) REGEN IN to CR-TC
• RFIC Eluent Degasser
REGEN OUT to waste
1.58 mm (0.062 in) ID Colorless 047203 EGC gas vent line
polyurethane tubing
10 mm (0.39 in) ID Colorless 055075 Drip tray drain hose
polyethylene tubing
1/8 in fitting bolt Tan 052267 The suppressor REGEN OUT
1/8 in ferrule Yellow 048949 port and the eluent reservoirs
10-32 fitting bolt Black 043275 All other tubing connections
10-32 ferrule, double- Tan 043276
cone

Table 9-4. Tubing and Fittings for an Analytical IC EG Channel

Notes for analytical IC channels:

• For ferrule fitting tightening requirements, refer to Installation of Dionex


Liquid Line Fittings (Document No. 031432). The manual is on the
Thermo Scientific Reference Library DVD (P/N 053891).
• For an analytical IC channel, use a tubing cutter to cut tubing to the
required length. Make sure the cut is at a right angle to the length of the
tubing and there are no nicks or burrs on the end. A tubing cutter
(P/N 049584) is included in the DC Ship Kit (P/N 072011). Refer to the
instructions provided with the cutter.

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9.13 Isolating a Restriction in the Liquid Lines


A restriction in the liquid plumbing will cause excessive system backpressure.
1. Begin pumping eluent through the system (including the columns) at the
flow rate normally used.
2. Work backward through the system, beginning at the flow cell exit. One
at a time, loosen each fitting and observe the pressure. The connection at
which the pressure drops abnormally indicates the point of restriction. If
the EGC is the source of the high backpressure, replace the outlet frit as
instructed in the EGC manual. The manual is included on the Thermo
Scientific Reference Library DVD (P/N 053891).
3. If the restriction has caused such high pressure that the system cannot be
operated, you must work forward through the system, adding parts one at
a time, until an abnormal pressure increase (and hence, the restriction) is
found.

9.14 Replacing the EGC


Replace the EGC when the cartridge is expended or when it leaks. Refer to
Table 2-2 for a list of the EGC models that can be used with the Dionex ICS-
5000 Eluent Generator.
Analytical IC systems require EGC III cartridges. Previous versions of EGC
are not compatible with the Dionex ICS-5000 Eluent Generator.
The EGC replacement procedure consists of:
• Removing the old EGC (see Section 9.14.1)
• Disposing of the old EGC (see Section 9.14.2)
• Installing and conditioning a new capillary EGC (see Section 9.14.4)
–or–
• Installing and conditioning a new analytical EGC (see Section 9.14.5)

The EGC contains one of the following: a corrosive base (KOH, LiOH, or
NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear
protective eyewear and gloves when handling the cartridge.

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9 • EG Service

La cartouche d'EGC contient un de ce qui suit: une base corrosive


(KOH, LiOH, ou NaOH), un acide corrosif (MSA), ou une solution
concentrée de K2CO3. Porter des lunettes et des gants protectives en
manipulant la cartouche.
Die EGC-Kartusche enthält eine korrodierende Base (KOH, LiOH oder
NaOH), eine korrodierende Säure (MSA) oder eine konzentrierte K2CO3-
Lösung. Tragen Sie daher beim Umgang mit Kartusche eine
Schutzbrille und Handschuhe.

9.14.1 Removing the Old EGC


1. Turn off the pump flow. (This turns off the power to the EGC and the
suppressor, also.)
2. Open the front door of the EG.
3. Pull the tray forward until it reaches the stop.
4. Twist the ring on the EGC
electrical cable counter-
clockwise to loosen it, and
then pull the cable straight out
of the EGC 1 (or EGC 2) EGC
bulkhead connector (see Cables
Figure 9-14).

Figure 9-14. EGC Cables

5. Close or cap the EGC vent opening to prevent leakage when you turn over
the cartridge in Step 7.
Capillary EGC
Capillary If you are removing a Vent Fitting
IC capillary EGC, tighten the Vent Fitting
vent fitting on the top of the
EGC (see Figure 9-15).

Figure 9-15. Capillary EGC Vent Fitting

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If you are removing an analytical EGC:


a. Remove the VENT line EGC
from the EGC by Vent Line
unscrewing the 10-32 luer Luer
adapter (see Figure 9-16). Adapter

NOTE If necessary, use a


wrench to hold the
luer adapter in place
while unscrewing the
vent line.

Figure 9-16. Analytical EGC Vent Line

b. Locate the 10-32 plug (P/N 053981) removed from the EGC vent
opening during installation. Install the plug into the vent opening.
6. Lift the EGC straight up and off the cartridge holder.
7. Turn the EGC upside
down and place it on the
EG drip tray (see Generation
Figure 9-17). This is the Chamber
“service position” for the
cartridge.

Electrolyte
Reservoir

Drip Tray

Figure 9-17. EGC in the Service Position


(Analytical Version Shown)

8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET
ports on the EGC.

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9 • EG Service

9.14.2 Disposing of the Old EGC


If the EGC is expended, follow these steps to dispose of it:
1. Hold the cartridge with the eluent generation chamber on top. Unscrew
the eluent generation chamber from the electrolyte reservoir and pour the
remaining electrolyte solution into an appropriate hazardous waste
container.

NOTE Refer to the Material Safety Data Sheet (MSDS)


shipped with the EGC for the chemical description.

2. Rinse the electrolyte reservoir and membranes three times with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Rinsing should render the reservoir
and membranes nonhazardous; however, check your local, state, and
federal regulatory agency regulations for proper disposal.

9.14.3 Storing an Old EGC


If the EGC is not expended, follow these steps to prepare the cartridge for
storage:
1. Plug all fittings. Tighten the vent fitting (capillary EGC) or cap the vent
port (analytical EGC). This will prevent the evaporation of water in the
electrolyte reservoir.
2. Store the cartridge in an upright position (with the electrolyte reservoir at
top) at 4 to 40°C (39 to 104°F) until its next use. The original shipping
container is ideal for storage. Before resuming operation, condition the
cartridge. For instructions, see Section 9.14.4 (for a capillary EGC) or
Section 9.14.5 (for an analytical EGC).

Capillary If you are replacing a capillary EGC, go on to Section 9.14.4.


IC

If you are replacing an analytical EGC, go on to Section 9.14.5.

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Capillary 9.14.4 Installing and Conditioning a New Capillary EGC


IC
Figure 9-18 shows the EG flow schematic for a capillary IC system. Refer to
this figure when performing EGC and CR-TC service procedures in a
capillary IC system.

Tubing Assembly Key


0.25 mm (0.010 in) ID Black
1
PEEK, 86 cm (34 in) (P/N 068658)
0.062 mm (0.0025 in) ID Blue Vent
2
PEEK, 18 cm (7 in) (P/N 072204)
EGC
0.062 mm (0.0025 in) ID Blue (Capillary)
3
PEEK, 61 cm (24 in) (P/N 072203)
0.25 mm (0.010 in) ID Black
4
PEEK, 64 cm (25 in) (P/N 072224)
1.58 mm (0.062 in) ID Clear
5
ETFE, 2.1 m (7 ft) (P/N 072225) EGC
IN
1
EGC
2 OUT
TO PUMP/DAMPER

5 WASTE, GAS
SEPARATOR
EG To CR-TC
Degas Regen Out
Cartridge (blue label)
(inside DC)

To CR-TC To CR-TC
ELUENT OUT
REGEN IN

REGEN OUT

Eluent In Eluent Out


(red label) (yellow label)
To EG Degas
Regen Out To CR-TC
ELUENT OUT
(blue label) Regen In
(orange label)

4 3
To Inject ELUENT IN To EG Degas
Valve Eluent In
(red label)

Figure 9-18. EG Flow Schematic Example for Capillary IC Systems

Capillary Flushing the Capillary EGC


IC
1. Remove the new EGC from the shipping container.

NOTE Save the shipping container; it may be required for


storage or disposal of the EGC.

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9 • EG Service

2. Verify that the vent fitting on top of the EGC is tightened.


3. Turn the cartridge upside down and place it on the EG drip tray.
4. Remove the plugs from the INLET and OUTLET fittings on the eluent
generation chamber.
5. Locate the 38 cm (15 in) piece of 0.025 mm (0.001 in) ID tan PEEK
tubing (P/N 074582) in the EG Ship Kit (P/N 072047).
6. Connect this line to the EGC INLET port and connect the other end to the
EGC IN line from the pump pulse damper (see Figure 9-19). This is a
temporary connection, to provide backpressure during the EGC setup
procedure.
7. Connect a piece of 0.25 mm (0.010 in) ID black PEEK tubing to the EGC
OUTLET port. Direct the other end of the tubing to waste. This is a
temporary connection.

Capillary EGC Flushing:


Pump at 0.02 mL/min for 20 min
EGC
(Capillary)

Electrolyte Reservoir

EGC
Electrolyte Generation IN 38 cm (15 in) of 0.025 mm
Chamber (0.001 in) ID tan
PEEK tubing
(Temporary connection
for backpressure)
EGC
0.25 mm (0.010 in) ID OUT
Pump Outlet
PEEK tubing
Tubing Assembly
(Temporary
connection) (P/N 068658)

To Waste TO PUMP/DAMPER

Figure 9-19. Flow Schematic for Flushing the Capillary EGC

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8. Slide the EGC (with the electrolyte


reservoir on top) into the cartridge
holder (see Figure 9-20).

Figure 9-20. Capillary EGC Installed on Holder

9. Push the EGC electrical cable firmly into the EGC 1 (or EGC 2) bulkhead
connector (see Figure 9-14). Twist the ring on the cable connector
fingertight to secure it.
10. Unscrew the fitting on the top of the EGC a few turns to vent the EGC.
To ensure proper ventilation, always loosen the fitting on the top of the
capillary EGC before operation.

11. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. DC panel: Verify that the suppressor Mode is off.
b. EG panel: Verify that the CR-TC is off.
To avoid damaging the suppressor and CR-TC, always turn them off
before flushing the EGC. The pump flow is on during flushing; however,
no flow reaches the suppressor or CR-TC.

c. Pump panel: Set the flow rate to 0.02 mL/min. This turns on the
pump flow, also.
12. Flush the capillary EGC for 20 minutes and then turn off the pump flow.
13. Disconnect the temporary tubing from the EGC OUTLET port.

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9 • EG Service

Capillary Conditioning the Capillary EGC


IC
1. Use a high-pressure (blue) fitting bolt and ferrule to connect the EGC OUT
line from the ELUENT IN port of the CR-TC to the EGC OUTLET port (see
Figure 9-21).
2. Disconnect the lines from the ELUENT OUT and REGEN IN port of the CR-
TC.
3. Connect a piece of 0.25 mm (0.010 in) ID PEEK tubing between the
ports. This is a temporary connection.

Capillary EGC Conditioning:


EGC
(Capillary) Pump at 0.02 mL/min for 15 min
EGC concentration at 50 mM

EGC
IN

0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly EGC
(P/N 072204) OUT ELUENT
IN
TO PUMP/DAMPER

To CR-TC
Regen Out
(blue label)

1.58 mm (0.062 in) ID


To CR-TC To CR-TC Tefzel Tubing
ELUENT OUT
REGEN IN

Eluent In Eluent Out Assembly (P/N 072225)


(red label) (yellow label)

To CR-TC 0.25 mm (0.010 in) ID


Regen In PEEK Tubing
(orange label) (Temporary
connection)

Figure 9-21. Flow Schematic for Conditioning the Capillary EGC

4. Verify that the suppressor Mode is off.

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5. Set the pump flow rate to 0.02 mL/min.

To avoid damaging the suppressor, always turn it off before


conditioning the EGC. The pump flow is on during conditioning;
however, no flow reaches the suppressor.

6. Set the EGC concentration to 50 mM and turn on the EGC and CR-TC
power.
7. Condition the EGC for 15 minutes.
8. Turn off the EGC and CR-TC power.
9. Turn off the pump flow.
10. Remove the backpressure tubing from the EGC IN line.
11. Use a high-pressure (blue) fitting to connect the EGC IN line to the EGC
INLET port.

12. Disconnect the temporary tubing from the ELUENT OUT and REGEN IN
ports of the CR-TC.
13. Reconnect the lines to the ELUENT OUT and REGEN IN ports of the CR-TC
that were disconnected in Step 2.

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9 • EG Service

9.14.5 Installing and Conditioning a New Analytical EGC


Figure 9-22 shows the EG flow schematic for an analytical IC system. Refer
to this figure when performing EGC and CR-TC service procedures in an
analytical IC system.

EGC VENT

EGC RFIC
Eluent
Degasser

Regen Regen
To Waste Out In

Eluent Eluent
Out In
Inlet Outlet
EGC
IN
EGC
TO PUMP OUT
Coupler
TO INJ VALVE - P

Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Regen In
TO CR -TC (orange label)
WASTE, GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
ELUENT OUT

To CR-TC
REGEN IN

Eluent In
(red label)

CR-TC

Figure 9-22. EG Flow Schematic Example for Analytical IC Systems

Installing the Analytical EGC

1. Remove the new EGC from the shipping container.

NOTE Save the shipping container; it may be required for


storage or disposal of the EGC.

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2. Verify that a plug is installed in the vent port. This will prevent leakage
from the vent opening when you turn over the cartridge.
3. Turn the cartridge upside down and place it on the EG drip tray in the
service position (see Figure 9-17).
4. Remove the plugs from the INLET and OUTLET fittings on the eluent
generation chamber.
5. Connect the EGC IN line from the pump to the EGC INLET port.
6. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil
(P/N 053765) in the EG Ship Kit (P/N 072047).
7. Connect one end of the
backpressure coil to the EGC Backpressure
OUTLET port (see Figure 9-23); Coil

leave the other end of the coil


unconnected. This is a
temporary connection. EGC
Outlet
Port

Figure 9-23. Analytical EGC Outlet Connection


for Conditioning Procedure

8. While holding the EGC right-side up (with the electrolyte reservoir on


top), shake the cartridge vigorously and tap it with the palm of your hand
10 to 15 times. Make sure any bubbles trapped in the eluent generation
chamber are dislodged.

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9 • EG Service

9. Slide the EGC (with the


electrolyte reservoir on top)
into the holder in the EG
(see Figure 9-24).

Figure 9-24. Analytical EGC Installed on Holder

10. Push the EGC electrical cable firmly into the EGC 1 (or EGC 2) bulkhead
connector (see Figure 9-14). Twist the ring on the cable connector
fingertight to secure it.
11. Remove the 10-32 plug from the EGC vent opening. Install a 10-32 luer
adapter in the vent opening.
12. Connect the luer adapter and VENT line removed from the old cartridge to
the vent opening in the new cartridge (see Figure 9-16).
13. Place the 10-32 plug removed from the vent opening in a safe place for
storage. The 10-32 plug is required for shipping or storing the cartridge.
To ensure proper ventilation, always connect the vent line to the
analytical EGC before operation.

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Conditioning the Analytical EGC

EGC VENT Analytical EGC Conditioning:


EGC Pump at 1.0 mL/min for 30 min
EGC concentration at 50 mM

To Waste 0.5 mL/min, 7 MPa (1000 psi)


backpressure coil
Inlet Outlet
(P/N 053765)
EGC
(Temporary connection)
IN

TO PUMP

To Waste

Figure 9-25. Flow Schematic for Conditioning an Analytical EGC

1. Set a small temporary waste container (for example, a beaker) next to the
EG. Direct the yellow backpressure coil from the EGC OUTLET port to
the waste container. The backpressure must be at least 1.4 MPa (200 psi).
2. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. DC panel: Verify that the suppressor Mode is off.
b. EG panel: Verify that the CR-TC is off.
To avoid damaging the suppressor and CR-TC, always turn them off
before conditioning the EGC. The pump flow is on during conditioning;
however, no flow reaches the suppressor or CR-TC.

c. Pump panel:
• Gradient pump only: Select the correct eluent channel (A, B, C,
or D).
• All pumps: Set the flow rate to 1.0 mL/min. This turns on the
pump flow, also.

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9 • EG Service

d. EG panel: Enter 50 mM in the Target Concentration field. This


turns on the power to the EGC, also.
e. Condition the analytical EGC for 30 minutes.
3. Turn off the EGC and CR-TC power.
4. Turn off the pump flow.

Completing the Analytical EGC Installation

1. Twist the ring on the EGC electrical cable counterclockwise to loosen it,
and then pull the cable straight out of the EGC 1 (or EGC 2) bulkhead
connector.
2. Remove the backpressure tubing from the waste container and remove the
waste container.
3. Replace the 10-32 plug in the EGC vent opening.
4. Lift the EGC out of the holder, turn it upside down, and place it on the
drip tray in the service position (see Figure 9-17).
5. Disconnect the backpressure coil from the EGC OUTLET port.
6. Connect the EGC OUT line to the OUTLET port.
7. Turn the EGC right-side up, and check for bubbles in the eluent
generation chamber. If necessary, shake and tap the cartridge to remove
bubbles.
8. Install the EGC in the holder. Remove the 10-32 plug from the vent
opening and reinstall the luer adapter and vent line.
9. Reconnect the EGC electrical cable.

9.15 Replacing the CR-TC


The CR-TC replacement procedure consists of:
• Removing the old CR-TC (see Section 9.14.1)
• Installing and hydrating the new CR-TC (see Section 9.15.2)
• Completing the plumbing for the new CR-TC (see Section 9.15.3)

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Refer to Figure 9-18 for a flow schematic of the EG and CR-TC for capillary
IC and to Figure 9-22 for analytical IC.

9.15.1 Removing the Old CR-TC


1. Turn off the pump flow. (This turns off the power to the EGC and the
suppressor, also.)
2. Open the front door of the EG.
3. Push down on the slide release latch and pull the tray forward until it
reaches the stop.
4. Pull the CR-TC off the ball studs on the component mounting panel.
5. Disconnect the liquid lines from the four ports on the CR-TC.
6. Twist the ring on the CR-TC electrical cable counterclockwise to loosen
it, and then pull the cable straight out of the CR-TC 1 (or CR-TC 2)
bulkhead connector.
7. Remove the CR-TC from the EG.

9.15.2 Installing and Flushing the New CR-TC


1. Remove the plugs from the ports on the new CR-TC.
Capillary 2. If you are installing a CR-TC in a capillary IC system:
IC
a. Connect a piece of 0.25 mm (0.010 in) ID PEEK tubing between the
ELUENT OUT and REGEN IN ports of the CR-TC (see Figure 9-26).
This is a temporary connection.
b. Locate the 38 cm (15 in) piece of 0.025 mm (0.001 in) ID tan PEEK
tubing (P/N 074582) in the EG Ship Kit (P/N 072047).
c. Connect this line to the EGC INLET port and connect the other end to
the EGC IN line from the pump pulse damper (see Figure 9-19). This
is a temporary connection, to provide backpressure.

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9 • EG Service

d. Connect the EGC OUT line to the CR-TC ELUENT IN port and connect
the waste line to the CR-TC REGEN OUT port.

Capillary CR-TC Flushing:


EGC Pump at 0.02 mL/min for 15 min
(Capillary)

EGC
IN

0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly EGC
(P/N 072204) OUT ELUENT
IN
TO PUMP/DAMPER

To CR-TC
Regen Out
(blue label)

1.58 mm (0.062 in) ID


To CR-TC To CR-TC Tefzel Tubing
ELUENT OUT
REGEN IN

Eluent In Eluent Out Assembly (P/N 072225)


(red label) (yellow label)

To CR-TC 0.25 mm (0.010 in) ID


Regen In PEEK Tubing
(orange label) (Temporary
connection)

Figure 9-26. Plumbing for Hydrating a Capillary CR-TC

3. If you are installing a CR-TC in an analytical IC system:


a. Locate the CR-TC Hydration Tubing Kit (P/N 063487) provided in
the EG Ship Kit.

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b. Refer to Figure 9-27 to plumb the four ports on the CR-TC.

To RFIC Eluent Degasser


Analytical CR-TC Flushing:
From EGC Out Port Regen In Port
Pump at application flow rate
for 10 min

TO CR -TC
REGEN OUT
(blue label)
Eluent Out
(yellow label)
To CR-TC

ELUENT OUT
REGEN IN
Eluent In
(red label)

Regen In
(orange label)
CR-TC Hydration Kit
Tubing Assembly
(P/N 063487)
(Temporary connection)

Figure 9-27. Plumbing for Hydrating an Analytical CR-TC

4. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select


the following settings:
a. DC panel: Verify that the suppressor Mode is off.
To avoid damaging the suppressor, always turn off the suppressor
before hydrating the CR-TC. The pump flow is on during conditioning;
however, no flow reaches the suppressor.

b. Pump panel:
• Gradient pump only: Select the correct eluent channel (A, B, C,
or D).
• Analytical pumps: Set the flow rate recommended for your
application. This turns on the pump flow, also. Allow the pump to
run for at least 10 minutes.
• Capillary pumps: Set the flow rate to 0.02 mL/min. This turns
on the pump flow, also. Allow the pump to run for 15 minutes.

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9 • EG Service

5. Turn off the pump flow.


6. Disconnect the temporary tubing from the ELUENT OUT and REGEN IN
ports on the CR-TC.
Capillary 7. If you are installing a CR-TC in an analytical IC system, remove the
IC backpressure tubing from the EGC IN line and use a high-pressure (blue)
fitting to connect the EGC IN line to the EGC INLET port.

9.15.3 Completing the New CR-TC Plumbing


1. Connect the regen out and eluent in lines from the eluent degasser to their
respective ports on the CR-TC. Refer to Figure 9-28 for a capillary IC
system or Figure 9-29 for an analytical IC system.

To EGC
OUTLET Port

WASTE , GAS
SEPARATOR
To CR-TC
Regen Out
(blue label)

To CR-TC To CR-TC
ELUENT OUT
REGEN IN

Eluent In Eluent Out


(red label) (yellow label)

To CR-TC
Regen In
(orange label)
To EG Degas
Cartridge
Regen Out

To EG Degas
Cartridge
Eluent In

Figure 9-28. Capillary CR-TC Plumbing Diagram: Installation Completed

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To EGC To RFIC Eluent To RFIC Eluent


OUTLET Port Degasser Degasser
REGEN OUT Port ELUENT IN Port

To CR-TC
To Gas Separator Regen In
Waste Tube (orange label)
TO CR -TC
WASTE , GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
To CR-TC

ELUENT O UT
REGEN IN
Eluent In
(red label)
CR-TC

Figure 9-29. Analytical CR-TC Plumbing Diagram:


Installation Completed

2. Check that no liquid lines are caught under the CR-TC. Align the two
mounting holes on the CR-TC back plate with the ball studs on the
mounting plate, and then push the CR-TC firmly onto the mounting ball
studs. The CR-TC clicks into place when properly installed.
3. Push the CR-TC electrical cable firmly into the CR-TC 1 (or CR-TC 2)
bulkhead connector. Twist the ring on the cable connector fingertight to
secure it.
4. Push the tray into the module until it locks into place. Close the EG door.

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9 • EG Service

9.16 Replacing the RFIC Eluent Degasser


1. Turn off the pump flow.
2. Open the front door of the EG.
3. Push down on the slide release latch and pull the tray forward until it
reaches the stop.
4. Grasp the degasser by the sides and pull it straight off the ball studs that
secure it to the component mounting panel. Dispose of the degasser.
5. Disconnect the four lines connected to the RFIC Eluent Degasser fittings
(ELUENT OUT, REGEN OUT, REGEN IN, and ELUENT IN).
6. Connect the four lines that were disconnected in Step 5 to the new RFIC
Eluent Degasser (P/N 062137).
7. Align the two mounting holes on the back plate of the new RFIC Eluent
Degasser with the ball studs on the component mounting panel. Push the
degasser firmly onto the mounting ball studs. The degasser clicks into
place when properly installed.
8. Push the tray into the module until it locks into place. Close the EG door.

9.17 Installing a Backpressure Coil


In an analytical IC system, the EGC requires at least 14 MPa (2000 psi) of
system backpressure; this ensures optimal removal of electrolysis gas from
the eluent produced by the cartridge.
During system equilibration, monitor the pressure and verify that it is between
14 and 21 MPa (2000 and 3000 psi). A system backpressure of 16 MPa
(2300 psi) is optimal.
If the backpressure is too low, install a backpressure coil (see Table 9-5)
between the injection valve and the OUTLET port on the EGC. Connect one
end of the backpressure coil to Port P (2) on the injection valve; connect the
other end to the TO INJ VALVE IN - P line.

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The EG Ship Kit (P/N 072047) includes four backpressure coils (see
Table 9-5).

Part Backpressure Flow Rate Approximate


Number Coil Description Backpressure Added
053762 4 mm ID 2.0 mL/min 3.5 MPa (500 psi)
1.0 mL/min 1.75 MPa (250 psi)
053763 4 mm ID 2.0 mL/min 7 MPa (1000 psi)
1.0 mL/min 3.5 MPa (500 psi)
053764 2 mm ID 0.50 mL/min 3.5 MPa (500 psi)
0.25 mL/min 1.75 MPa (250 psi)
053765 2 mm ID 0.50 mL/min 7 MPa (1000 psi)
0.25 mL/min 3.5 MPa (500 psi)

Table 9-5. EG Backpressure Coils

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9 • EG Service

9.18 Changing the EG Main Power Fuses


1. Press the POWER button on the front of the EG for 2 seconds to turn off
the power.
2. Turn off the main power switch on the EG rear panel (see Figure 2-12).
3. Disconnect the main power cord from both its source and from the EG
rear panel.
.

HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the EG.

HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa


source et du panneau arrière du EG.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und


der Netzbuchse auf der Rückseite des EG.

4. The fuse drawer is located above the main


power switch (see Figure 9-30). A small Fuse
tab locks the fuse drawer in place. Using a Drawer
small screwdriver, press the tab in and then Tab
up to release the fuse drawer.
5. Pull the fuse drawer out of the rear panel
and remove the old fuses.
6. Replace the two fuses with new 2 A IEC
60127-2 slow-blow fuses (P/N 954773).
Thermo Fisher Scientific recommends
always replacing both fuses.

Figure 9-30. EG Fuse Drawer

7. Insert the fuse drawer into the rear panel and press until the drawer snaps
into place.
8. Reconnect the main power cord and turn on the power.

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DC DC Service

9.19 Replacing Tubing and Fittings

Capillary 9.19.1 Tubing and Fittings for Capillary IC Systems


IC
Table 9-6 lists tubing and fittings used to plumb a DC system for capillary IC.

Tubing Size and Type Color P/N Used to connect…


IC Cube Tubing Kit N/A 072186 See Table 9-7
AS needle seal White 057301 AS normal and
assembly, 46 cm (18 in), concentrate modes only:
with 10-32 ferrule fitting Injection valve to the AS
inject port
0.25 mm (0.010 in) ID Black 042690 AS sequential modes only:
PEEK tubing, 50 cm (1 in) Injection valve to AS
(20 in) diverter valve
ED Cell Inlet Tubing Kit N/A 074221 ED cell inlet to column
outlet
10-32 fitting bolt Black 043275 • Suppressor eluent out
10-32 ferrule, double- Tan 043276 CRD eluent in
cone • CD cell inlet and outlet
• ED cell outlet
• Injection valve sample in
and sample out

Table 9-6. Tubing and Fittings for a Capillary IC DC System

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Capillary Table 9-7 lists the tubing and fittings in the IC Cube Tubing Kit (P/N 072186)
IC

Part Length/ Part Used To Connect…


Quantity Number
Precision cut 0.062 mm 65 mm 072188 50 mm guard column
(0.0025 in) ID PEEK (2.56 in) outlet to 250 mm
tubing, blue separator column inlet
Precision cut 0.062 mm 115 mm 072189 Guard column inlet to
(0.0025 in) ID PEEK (4.53 in) injection valve
tubing, blue, labeled
VALVE PORT 3
Precision cut 0.062 mm 75 mm 074603 35 mm guard column
(0.0025 in) ID PEEK (2.93 in) outlet to 150 mm
tubing, blue separator column inlet
Precision cut 0.062 mm 210 mm 072187 Separator column inlet to
(0.0025 in) ID PEEK (8.27 in) injection valve (if a guard
tubing, blue, labeled column is not present)
VALVE PORT 3
0.25 mm (0.010 in) ID 610 mm 042690 EG degas cartridge
PEEK tubing, black (24 in) REGEN OUT to waste (if
an EG is not present)
0.125 mm (0.005 in) ID 610 mm 044221 Inject valve waste to AS
PEEK tubing, red (24 in) waste
High-pressure 10-32 7 074449 • EG degas cartridge
fitting bolt, blue ELUENT OUT to
injection valve
• Injection valve to guard
or separator column
• Guard column to
separator column
• Separator column to
suppressor
High-pressure 10-32 7 074373 Use with high-pressure
ferrule, double-cone, fitting bolts
blue

Table 9-7. Contents of the IC Cube Tubing Kit (P/N 072186)

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9 • DC Service

Capillary Notes for Capillary IC systems:


IC
• The 0.062 mm (0.0025 in) ID blue PEEK tubing (capillary tubing) used
for IC Cube connections is cut at the factory using a specialized precision
cutter. If you need to replace any of this type of tubing, order an IC Cube
Tubing Kit (P/N 072186) or the individual tubing listed in Table 9-7.
• When replacing capillary tubing, make sure the ferrule and fitting bolt are
at least 2 mm (0.1 in) from the end of the tubing before you insert the
tubing into the port. Do not position the ferrule and fitting bolt flush with
the end of the tubing. For detailed connection instructions, see Section 9.1
• Except for capillary tubing, you can use a tubing cutter to cut tubing to the
required length. Make sure the cut is at a right angle to the length of the
tubing and there are no nicks or burrs on the end. A tubing cutter
(P/N 049584) is included in the DC Ship Kit (P/N 072011). Refer to the
instructions provided with the cutter.
• For tightening requirements for the high-pressure fitting bolt
(P/N 074449) and ferrule (P/N 074373), see Section 9.2.
• For tightening requirements for the 10-32 fitting bolt (P/N 043275) and
ferrule (P/N 043276), refer to Installation of Dionex Liquid Line Fittings
(Document No. 031432). The manual is on the Thermo Scientific
Reference Library DVD (P/N 053891).

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9.19.2 Tubing and Fittings for Analytical IC Systems


Table 9-8 lists the tubing and fittings used to plumb a DC system for
analytical IC.

Tubing Size and Type Color P/N Used to connect…


0.75 mm (0.030 in) ID Green 044777 Injection valve to waste
PEEK (1 in)
AS needle seal White 057301 AS normal and
assembly, 46 cm (18 in), (1 in) concentrate modes only:
with 10-32 ferrule fitting Injection valve to the AS
inject port
0.33 mm (0.013 in) ID, Light Blue 049714 AS sequential modes only:
PEEK (1 in) Injection valve to AS
diverter valve
0.51 mm (0.020 in) ID, Orange 042855 AS simultaneous mode
PEEK (1 in) only: Each injection valve
to the AS simultaneous
injection tee
1.58 mm (0.062 in) ID Colorless 014157 Suppressor REGEN OUT
PTFE (1 in)
0.125 mm (0.005 in) ID Red 044221 Microbore systems:
PEEK (1 in) Connections between
other system components
0.25 mm (0.010 in) ID Black 042690 Standard bore systems:
PEEK (1 in) Connections between
other system components
1/8 in fitting bolt Tan 052267 Suppressor REGEN OUT
1/8 in ferrule Yellow 048949 fitting
10-32 Fitting bolt Black 043275 All other tubing fittings
10-32 Ferrule, double- Tan 043276
cone

Table 9-8. Tubing and Fittings for an Analytical IC DC System

Notes for analytical IC systems:


• Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing and there are no nicks or burrs

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9 • DC Service

on the end. A tubing cutter (P/N 049584) is included in the DC Ship Kit
(P/N 072011). Refer to the instructions provided with the cutter.
• For tightening requirements, refer to Installation of Dionex Liquid Line
Fittings (Document No. 031432). The manual is on the Thermo Scientific
Reference Library DVD (P/N 053891).

9.20 Connecting a Sample Loading Port to the Injection


Valve
1. For each sample loading port to be connected, locate the following items
in the DC Ship Kit (P/N 072011):
• One 1/4-28 fitting (P/N 052230) and ferrule (P/N 052231)
• One 10-32 fitting (P/N 062980) and ferrule (P/N 062978)
• 0.75 mm (0.030 in) ID green PEEK tubing (P/N 052304)
• One luer adapter fitting (P/N 024305)
2. Locate the metal release tab under the sample loading port on the front of
the DC (see Figure 9-31). Press up on the tab to release the port and pull
the port out the front of the DC.

Sample Loading
1
Ports

1 1 2 Release Tabs
2 2

Figure 9-31. DC Sample Loading Ports and Release Tabs

3. Remove the fitting plug from the rear of the port.

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4. Attach the luer adapter fitting to the front of the port (see Figure 9-32).

1 Luer Adapter Fitting

4 2 Sample Loading Port


3
3 1/4-28 Fitting and Ferrule
2
1 Green, 0.75 mm (0.030 in)
4 ID PEEK Tubing

Figure 9-32. Sample Loading Port Connection

5. Cut a length of green, 0.75 mm (0.030 in) ID PEEK tubing. The tubing
will be used to connect the sample loading port and the sample port on the
valve.
6. Attach a 1/4-28 fitting and ferrule to one end of this tubing and connect it
to the rear of the sample loading port.
7. Thread the free end of the tubing through the sample loading port opening
on the DC. Insert the port into the opening and turn it until it snaps into
place.
8. Attach a 10-32 fitting and ferrule to the free end of the tubing and connect
it to sample port S (5) on the injection valve.

9.21 Replacing the Leak Sensor


1. Turn off the pump flow from the ePanel in Chromeleon 7 or the Control
panel in Chromeleon 6.8, or press PUMP FLOW on the front of the pump.
2. Press the POWER button on the front of the DC to turn off the DC.

To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le DC avant d'ouvrir la porte


ou d'effectuer des opérations de maintenance.

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Um Verletzungen zu vermeiden, warten Sie bitte, bis der DC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

3. Open the DC lower door.


4. Loosen the screw on the front of the leak sensor (P/N 062437) (see
Figure 9-33). Note: The screw remains attached to the sensor.

Leak
Sensor

Loosen
this
screw

Figure 9-33. Leak Sensor

5. Pull out the leak sensor from the


component panel and continue
pulling until the attached cable
is also out of the opening.
Disconnect
6. The cable attached to the leak cables
sensor connects to a cable
inside the DC. Continue pulling
the cable until the connectors
for the two cables are outside
the panel (see Figure 9-34).
7. Disconnect the two cables.
Figure 9-34. Leak Sensor Cable

8. Connect the cable from the new leak sensor to the DC cable.
9. Feed the cables back inside the DC. Align the leak sensor with the
component panel opening and fingertighten the screw.
10. Make sure the leak sensor does not touch the bottom of the drip tray.

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9.22 Rebuilding a High-Pressure (Injection) Valve


Thermo Fisher Scientific recommends rebuilding the injection valve annually.
The Injection Valve Rebuild Kit (P/N 074698; 4-port valve; P/N 057896, 6-
port valve; P/N 061759, 10-port valve) contains all required replacement
parts. This procedure also applies to high-pressure valves installed in a
Dionex ICS-5000 Automation Manager.

NOTE Substitution of non-Dionex/Thermo Fisher Scientific parts


may impair valve performance and void the product war-
ranty.

NOTE If you prefer, you can replace the high-pressure valve “pod,”
instead of rebuilding the valve. Replacing the pod is easier
and faster than rebuilding the valve.

1. Turn off the pump flow.


2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.

To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le DC avant d'ouvrir la porte


ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der DC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

3. Open the DC door.


4. Disconnect each liquid line connected to the valve.
5. Follow the instructions provided in the Rebuild Kit to replace the rotor
seal, isolation seal, and stator face.
6. Reconnect all liquid lines to the injection valve.

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9 • DC Service

7. Turn on the power to the DC.


8. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required. For tightening requirements, refer to Installation of Dionex
Liquid Line Fittings (Document No. 031432). The manual is on the
Thermo Scientific Reference Library DVD (P/N 053891).
9. Close the door.

9.23 Replacing a High-Pressure (Injection) Valve Pod


This procedure describes how to replace the mechanical parts (the “pod”) of a
high-pressure valve (P/N 074699, 4-port; P/N 061947, 6-port; P/N 061948,
10-port).

NOTE If the valve electronics require service, contact


Thermo Fisher Scientific. Electronics-related repair
procedures must be performed by Thermo Fisher Sci-
entific personnel.

NOTE Substitution of non-Dionex/Thermo Fisher Scientific


parts may impair valve performance and void the
product warranty.

1. Turn off the pump flow.

To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le DC avant d'ouvrir la porte


ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der DC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.
3. Open the DC door.

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4. Disconnect each liquid line connected to the valve.


5. Unscrew the locking ring on the outside of the valve (see Figure 9-35)
and remove the ring.

Locking Ring

Figure 9-35. Unscrew the Locking Ring (Valve in IC Cube Shown)

6. Grasp the front of the valve pod and pull out firmly to remove it from the
DC or AM.
7. Align the slots in the new pod with the runner in the valve holder on the
DC or AM (see Figure 9-36). Valve pods are keyed to fit only one way
(one slot is narrower than the other). Verify that the slots are aligned with
their matching runners.

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8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-36). If necessary, twist the end of the
pod to adjust the position of the splines.

Valve Pod Valve Holder

Slot (larger)
Runner (larger)

Splines

Figure 9-36. High-Pressure Valve Pod and Pod Holder

9. Push the pod into the holder until it clicks into place. Replace the black
locking ring.
10. Reconnect all liquid lines to the valve.
11. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required. For tightening requirements, refer to Installation of Dionex
Liquid Line Fittings (Document No. 031432). The manual is on the
Thermo Scientific Reference Library DVD (P/N 053891).
12. Close the door.

9.24 Installing or Replacing an I/O Option Board


1. Press the POWER button on the front of the DC for 2 seconds to turn off
the power.
2. Turn off the main power switch on the DC rear panel (see Figure 2-31).

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3. Disconnect the main power cord from both its source and from the DC
rear panel.

HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the DC.

HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa


source et du panneau arrière du DC.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und


der Netzbuchse auf der Rückseite des DC.

4. On the DC rear panel, remove the two screws that attach the I/O option
cover plate or the existing I/O option board to the rear panel (see
Figure 9-37). Save the screws.

Remove two
screws

Figure 9-37. DC Rear Panel: Removing the I/O Option Cover Plate

5. Slide the new I/O option board (P/N 062201) into the rear panel opening
and press firmly to connect the board to the DC motherboard.
6. Replace the two screws.

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9 • DC Service

Figure 9-38 shows the I/O option installed.

I/O
Option

Figure 9-38. DC Rear Panel: I/O Option Installed

7. Reconnect the main power cord and turn on the power.

9.25 Changing the DC Main Power Fuses


1. Press the POWER button on the front of the DC for 2 seconds to turn off
the power.
2. Turn off the main power switch on the DC rear panel (see Figure 2-31).
3. Disconnect the main power cord from both its source and from the DC
rear panel.

HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the DC.

HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa


source et du panneau arrière du DC.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und


der Netzbuchse auf der Rückseite des DC.

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4. The fuse drawer is located above the


main power switch (see Figure 9-39). Fuse
Drawer
A small tab locks the fuse drawer in
place. Using a small screwdriver, Tab
press the tab in and then up to release
the fuse drawer.
5. Pull the fuse drawer out of the rear
panel and remove the old fuses.
6. Replace the two fuses with new 10 A
IEC 60127-2 slow-blow fuses
(P/N 954772). Thermo Fisher
Scientific recommends always
replacing both fuses.
Figure 9-39. DC Fuse Drawer

7. Insert the fuse drawer into the rear panel and press until the drawer snaps
into place.
8. Reconnect the main power cord and turn on the power.

9.26 IC Cube Service Procedures

9.26.1 Replacing an IC Cube Cartridge


1. Turn off the pump flow.
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC power.

To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le DC avant d'ouvrir la porte


ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der DC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs-oder Servicearbeiten
durchführen.

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9 • DC Service

3. Open the DC upper door.


4. Disconnect each liquid line connected to the IC Cube cartridge to be
replaced.
5. Loosen the two thumbscrews on the cartridge
(see Figure 9-40) and pull the cartridge out of
the IC Cube.
6. Slide the new cartridge into the IC Cube. Cartridge
Push the cartridge firmly into the IC Cube Thumb-
and then tighten the thumbscrews. screws

Figure 9-40. Capillary Cartridge Thumbscrews


(EG Degas Cartridge Shown)

7. If you are installing a suppressor or CRD cartridge, hydrate them before


use. Refer to the instructions in the suppressor or CRD manual. The
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891)
8. Reconnect the liquid lines that were disconnected in Step 4.

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9.26.2 Replacing Capillary Columns


1. Turn off the pump flow.
2. Open the DC upper door.
3. Disconnect the line from the ELUENT OUT port of the injection valve and
the line from the ELUENT OUT fitting on the column cartridge (see
Figure 9-41).

Disconnect
these two lines

Figure 9-41. Disconnect Capillary Cartridge Eluent Lines

4. Loosen the two thumbscrews on the column cartridge and pull the
cartridge out of the IC Cube.

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5. Lift the lid of the column cartridge to open it. Figure 9-42 shows the
column cartridge when a capillary guard column and a capillary separator
column are installed.

Separator
1 Column Outlet

Separator
8 2 Column
1
Separator
3 7 3 Column Inlet
4
2 4 Precision Cut
5 Tubing
Guard Column
5 Outlet
6
6 Guard Column

7 Guard Column
Inlet
8 Precision Cut
Tubing

Figure 9-42. Separator and Guard Columns Installed in Column Cartridge

Figure 9-43 shows the column cartridge when only a capillary separator
column is installed

Separator
1 Column Outlet
1
3 4
Separator
2 Column
2
Separator
3 Column Inlet

4 Precision Cut
Tubing

Figure 9-43. Separator Column Only Installed in Column Cartridge

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6. Remove the guard column (if present)


and separator column from the column
clips. Lift up the separator column
outlet fitting (see Figure 9-44) slightly
to free it from the clips and then slide it
out of the cartridge.
7. Remove the columns from the cartridge.
8. Disconnect the tubing from the
columns. Save the tubing.
Figure 9-44. Separator Column Outlet Fitting

NOTE Do not cut the tubing that you removed from the col-
umns and do not substitute different tubing. To ensure
good chromatographic results, capillary tubing is cut
at the factory using a specialized precision cutter. If
you need to replace the tubing or to install a different
length tubing (to accommodate a new column configu-
ration), order an IC Cube Tubing Kit (P/N 072186).

9. Before installing the new separator column, tear off the column label and
slide it into the holder on the front of the cartridge (see Figure 9-48).
10. If the new column configuration is the same as the previous, connect the
precision cut tubing that you removed in Step 8 to the new columns.

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9 • DC Service

If you are changing the column configuration, refer to the following


figures for the precision cut tubing required for your configuration:

3 250 mm Separator
2 1 Column
65 mm (2.5 in)
2 Precision Cut Tubing
4 (P/N 072188)
50 mm Guard
3 Column

115 mm (4.5 in)


1 4 Precision Cut Tubing
(P/N 072189)

Figure 9-45. Tubing Connections for 250 mm Separator Column and


50 mm Guard Column

3 150 mm Separator
1 Column

75 mm (3 in)
2 4 2 Precision Cut Tubing
(P/N 074603)
35 mm Guard
3 Column
1
115 mm (4.5 in)
4 Precision Cut Tubing
(P/N 072189)

Figure 9-46. Tubing Connections for 150 mm Separator Column and


35 mm Guard Column

Separator
1 Column

2 210 mm (8.3 in)


2 Precision Cut Tubing
(P/N 072187)
1 (use with any
length separator
column)

Figure 9-47. Tubing Connections for Separator Column Only

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11. Remove the fitting plug from the outlet fitting on the separator column.
Orient the fitting with a flat side up and push the fitting into the opening at
the front of the column cartridge until it stops (see Figure 9-44).
12. Coil the separator column tubing inside the cartridge as shown in
Figure 9-42 or Figure 9-43. Secure the column and the inlet fitting in the
clips on the column cartridge.
13. Secure the inlet and outlet fittings on the guard column (if used) in the
column clips on the lid of the column cartridge.
14. Route the column inlet tubing from the guard column (if used) or the
separator column through the clip on the top edge of the cartridge lid.
15. Close the lid (you should hear a click) and route the tubing into the slot on
the front of the column cartridge (see Figure 9-48).

NOTE If the columns are installed correctly, the cartridge lid


snaps closed easily. If the lid does not close easily, do
not force it. Open the lid and verify that the columns
and tubing are installed correctly and secured in the
clips.

Separator Column
1
Outlet
2
2 Column Label

3 Column Inlet Tubing


1

Figure 9-48. Column Cartridge Closed

16. Slide the column cartridge into the IC Cube column oven and tighten the
two thumbscrews.
17. Turn on the pump flow.
18. Wait until liquid is flowing out of the Eluent Out port (3) of the injection
valve.

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19. Connect the tubing from the Eluent In port of the column cartridge to the
Eluent Out port (3) of the injection valve.

20. Wait until liquid is flowing out of the Eluent Out port of the column
cartridge.
21. Reconnect the line to the Eluent Out fitting on the column cartridge that
was disconnected in Step 3 (see Figure 9-41).
22. Close the DC upper door.

9.27 CD Service Procedures

9.27.1 Calibrating the CD Cell


NOTE Do not use this procedure to calibrate a new cell. New
cells are calibrated at the factory.

Items Needed Description


1.0 mM KCl solution Prepare by dissolving 0.07456 g of
reagent-grade KCl in 1 liter of 18 megohm-
cm DI water.
Backpressure tubing to Use 0.25 mm (0.010 in) ID black PEEK
provide at least 7 MPa tubing (P/N 042690).
(1000 psi)

1. On the Chromeleon 7 ePanel Set, click the CD tab. On the Chromeleon


6.8 panel tabset, click the CD tab.

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2. Under Detector Settings, click Calibration. The Wellness panel opens


(see Figure 9-49).

Figure 9-49. Wellness Panel: Dionex ICS-5000 Conductivity Detector


(Chromeleon 6.8 Version Shown)

3. On the Wellness panel under External Conductivity Cell Calibration,


click Instructions for a summary of the procedure (described in detail in
this section).
4. Disconnect the pump output line from the injection valve.
5. Disconnect the line from the suppressor ELUENT OUT port to the cell inlet
and connect the pump output line directly to the cell inlet.
6. Verify that backpressure at the pump is at least 7 MPa (1000 psi) at
0.01 mL/min (for capillary) or 1.00 mL/min (for analytical).
7. Set the cell heater to 35 °C. Allow the cell to reach this temperature (the
LED stops blinking).
8. Begin pumping 1.0 mM KCl through the cell at 0.01 mL/min (for
capillary) or 1.0 mL/min (for analytical).
9. Wait until the total conductivity reading stabilizes (15 to 30 minutes).
10. On the Wellness panel, click Calibrate.
After calibration, the conductivity reading should be 147.00 ± 2 S. If this
is not the case, repeat the calibration.
11. To record the new calibration value in the Audit Trail, click Log.

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12. Flush the KCl solution from the system by pumping ASTM Type I
(18 megohm-cm) filtered and deionized water through the cell. When the
conductivity drops to less than 1 S/cm, stop the pump.
13. Reconnect the pump to the injection valve and reconnect the line from the
suppressor to the cell inlet.

9.27.2 Replacing an Analytical Suppressor


Refer to the suppressor manual for guidance about when to replace a
suppressor and for instructions on preparing a new suppressor before initial
use. Suppressor manuals are included on the Thermo Scientific Reference
Library DVD (P/N 053891).
1. Stop the pump flow.
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.

To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le DC avant d'ouvrir la porte


ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der DC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

3. Open the DC upper door.


4. Disconnect the four liquid lines from the suppressor (see Figure 9-50).

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5. Unplug the suppressor cable from the detector.

Unplug cable

Disconnect lines

Figure 9-50. Disconnecting the Suppressor Liquid Lines and Cable

6. Remove the suppressor from the detector by sliding it to the left a few
millimeters to detach it from the mounting tabs on the detector. Then, pull
the suppressor toward you.
7. Orient the new suppressor with the ELUENT IN and REGEN OUT ports on
the bottom (see Figure 9-50). Press the suppressor against the back of the
detector and then slide it to the right to secure it onto the mounting tabs.
Pull out slightly on the center of the suppressor to verify that it is securely
fastened.
8. Reconnect the four liquid lines to the new suppressor.
9. Plug in the suppressor cable.
10. Close the DC door.
11. Turn on the DC power and restart the pump flow.

9.27.3 Replacing a CD
1. Stop the pump flow.
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.

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9 • DC Service

3. Open the DC upper door and disconnect the tubing from the CD CELL IN
and CELL OUT ports (see Figure 9-51).

Disconnect tubing

Release Lever

Figure 9-51. Disconnecting the CD Liquid Lines (Capillary CD shown)

4. For an analytical CD, remove the suppressor from the detector. For
instructions, refer to Section 9.27.2.
5. Press the release lever located below the detector (see Figure 9-51). The
detector pops out slightly from the DC compartment. Grasp the top of the
detector and pull outward to remove the detector from the compartment.
Do not pull from the CELL IN and CELL OUT fittings.
6. Note the electrical plug on the back of the detector and the receptacle on
the inside of the DC.
7. Push the new detector into the opening in the DC and press firmly to
ensure the electrical connection is secure.
8. Reconnect the cell inlet and outlet lines.
9. Reinstall the suppressor (see Section 9.27.2).
10. Turn on the DC power and restart the pump flow.

9.27.4 Removing Trapped Air from the Conductivity Cell


Air bubbles in the cell can cause pulsations of the baseline, random noise, and
low readings. Air may result from outgassing of the eluent. In an analytical IC
system follow the steps below to remove trapped air from the cell. These steps
are not required for a conductivity cell in a capillary IC system.

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1. Connect enough backpressure tubing to the cell outlet to shrink bubbles


and allow them to pass more easily through the cell. Refer to Table 9-9 for
the appropriate type and number of backpressure tubing coils required.

Suppressor Column Flow Rate Backpressure


Type Format (mL/min) Coils
Dionex AES 2 mm 0.25 to 0.50 2 red*
3 mm 0.50 to 1.00 2 red
4 mm 1.00 to 2.00 1 red
Dionex SRS or 2 mm or 3 mm <0.25 2 red
Dionex MMS
2 mm or 3 mm 0.25 to 0.50 1 red
*The red coil (P/N 045878) consists of 0.125 mm (0.005 in) ID PEEK tubing
with fittings.

Table 9-9. Backpressure Coil Requirements

Table 9-10 lists the correct pressure range for each type of suppressor.

Suppressor Type Pressure Range


Dionex AES 0.14 to 0.70 MPa (20 to 100 psi)
Dionex SRS or Dionex MMS 0.28 MPa (40 psi)
Table 9-10. Suppressor Operating Pressure Ranges

2. To verify that the required amount of backpressure is being generated,


follow the instructions in Backpressure Coil Pressure Test for Dionex
Suppressors (Document No. 031759), the flier shipped with the
suppressor. The instructions are also in the suppressor manual on the
Thermo Scientific Reference Library DVD (P/N 053891).
3. If a bubble is still trapped in the cell, try these techniques to remove it:
• Loosen and then tighten the cell outlet fitting.
• Temporarily disconnect the backpressure coil from the suppressor
REGEN IN port and then plug and unplug the end of the tubing with
your fingertip two or three times to create a pressure difference.

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9 • DC Service

9.28 ED Service Procedures

9.28.1 Disconnecting the ED Cell


Before performing an ED cell service procedure, follow these instructions to
disconnect the cell.
1. Turn off the cell voltage from the Chromeleon 7 ePanel Set or
Chromeleon 6.8 panel tabset.
2. Stop the pump flow.
3. Disconnect the cell inlet and outlet lines from the ED cell and disconnect
the two electrical cables (see Figure 9-52).

NOTE For a capillary IC system, disconnect the cell inlet line from
the ELUENT OUT port of the IC Cube column cartridge.

Cables

Inlet line

Outlet line

Figure 9-52. Disconnecting the ED Cell


(Cell Configured for Analytical IC Shown)

4. Grasp the cell by the cell body and pull straight out to remove it from the
detector.

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9.28.2 Replacing an ED Cell Disposable Working Electrode Gasket


For installation instructions for disposable working electrodes, refer to the
installation guide shipped with the electrodes (see below) or to Product
Manual for Disposable Electrodes (Document No. 065040), which is
included on the Thermo Scientific Reference Library DVD (P/N 053891).
• Disposable Silver Electrode Installation Guide for ED (Document
No. 065137)
• Disposable Platinum Electrode Installation Guide for ED (Document
No. 065139)
• Disposable Gold Electrode Installation Guide (Document No. 065191)
When you install a disposable electrode, make sure that you install
the correct gasket for your system.
• For a capillary system, use a 0.001-in PTFE gasket (P/N 072117,
Pkg. of 2).
• For an analytical system with a gold, silver, or platinum
disposable electrode, use a 0.002-in PTFE gasket (P/N 069141,
Pkg. of 4).
• For an analytical system with a carbon disposable electrode, use
a 0.001-in Ultem gasket (P/N 069339).

9.28.3 Replacing an ED Cell Conventional Working Electrode


Gasket
When to Replace the Gasket

Replace the gasket if there is a leak between the gasket and electrode, or
between the gasket and cell body.

Items Needed

• ED cell gasket for conventional working electrodes (P/N 045972)


• Gloves
• Blunt-end tweezers

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9 • DC Service

ED Cell Gasket Replacement Procedure

NOTE Always wear gloves when handling the ED cell. Never touch
the electrode surface.

1. Follow the instructions in Section 9.28.1, to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.
2. Loosen the yoke knob on the yoke block by unscrewing it two to three
turns (see Figure 9-53).

First, loosen the


yoke knob

Then, squeeze
the tabs on
the yoke block
and pull to
remove it

Figure 9-53. Disassembling the ED Cell


(Cell Configured for Analytical IC Shown)

3. Squeeze the tabs on the sides of the yoke block and pull the block and
knob off the working electrode (see Figure 9-53).

NOTE Handle the cell gasket and the inside surfaces of the
cell carefully to prevent scratches which may subse-
quently cause leaks.

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4. Carefully separate the parts (see Figure 9-54).

Conventional
Working
Electrode Block
Yoke
Block

Cell
Body
Cell
Gasket

Figure 9-54. ED Cell Components

5. Use tweezers to remove the old cell gasket from the cell body (see
Figure 9-55).

Alignment
Conventional
Pins
Working Electrode
Gasket

Figure 9-55. ED Cell Gasket for Conventional Working Electrodes

6. Rinse the surface of the cell with ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5.
7. Clean the polished surface of the cell with a clean, damp lint-free tissue.
8. Install the new gasket over the alignment pins on the cell body. When
correctly installed, one end of the gasket extends beyond the cell body, to
facilitate gasket installation and removal.
9. Verify that the gasket is flat against the cell body and is not wrinkled.

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10. Reinstall the working electrode block and the yoke knob and block.
Fingertighten the yoke knob by turning it a full 360 degrees.

NOTE It is not possible to overtighten the yoke knob. Once


the knob clicks into place, it does not tighten any fur-
ther. The yoke knob ensures constant pressure is
applied to the cell.

11. Orient the cell assembly with the yoke knob on the left and push the cell
onto its mounting location in the DC compartment.
12. Reconnect the cell’s inlet and outlet lines.
13. Reconnect the electrical cables.
14. Start the pump flow.
15. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.

9.28.4 Polishing an ED Cell Conventional Working Electrode


These instructions are for conventional (nondisposable) working electrodes
only. Do not polish disposable electrodes.

When to Polish the Working Electrode

• Do not polish new conventional working electrodes before


installation.
• After an electrode has been used for a period of time, a layer of
contamination may build up. When this occurs, the electrode must be
polished.
• After the working electrode is polished and installed, background signal
and analyte sensitivity require several hours to stabilize. Once stabilized,
do not polish the electrode unless you observe a loss of signal or severe
electrode recession.

Items Needed

• Polishing kit (P/N 036313) shipped with the electrode. The kit contains
polishing pads (P/N 036321), a bottle of fine polishing compound
(P/N 036318), and a bottle of coarse polishing compound (P/N 036319).

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• Gloves
• Tweezers

Working Electrode Polishing Procedure

NOTE To avoid electrode fouling, always wear gloves when han-


dling electrodes.

1. Follow the instructions in Section 9.28.3, Step 1 through Step 4, to


remove the working electrode from the cell.
2. Prepare the polishing pads:
a. Designate a pad for use with the coarse polishing compound.
b. Designate another pad for fine polishing compound; also designate
the working electrode type with which it will be used.

NOTE Do not use the same fine polishing pad to polish more
than one type of working electrode; this can contami-
nate the electrode surface with microparticles from the
other working electrodes.

c. Designate a pad that will not be used with polishing compound. This
pad is for removal of particles after polishing (see Step 5).
d. Moisten the suede side of the polishing pad slightly with water and
place the pad on a smooth, flat surface, with the suede side facing up.
3. Polish the electrode:
• If you are polishing the electrode before initial installation, use only
the fine polishing compound.
• If you are polishing the electrode because of degradation of
performance, such as increased baseline noise or tailing peaks, first
use the coarse polishing compound. Then, repeat with the fine
compound.
a. Sprinkle about one-half gram of polishing compound in the center of
the suede side of the polishing pad. Add enough ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5 to make a thick paste.

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9 • DC Service

b. Using the working electrode block, spread the paste evenly over the
pad. Then, applying firm pressure in a figure eight motion, polish the
surface of the electrode block for about one minute. If the pad dries
out while polishing, add water sparingly. However, never allow the
polishing compound to dry on the electrode.
c. Use ASTM Type I (18 megohm-cm) filtered and deionized water that
meets the specifications listed in Section 1.5 to rinse off all traces of
polishing compound from the electrode block. An ultrasonic cleaner
is effective for thoroughly cleaning the electrode block. Carefully
rinse the surface of the block with ASTM Type I (18 megohm-cm)
filtered and deionized water.
4. If you used the coarse polishing compound in Step 3, repeat the step with
the fine compound.
5. Using a moist piece of polishing cloth (with no polishing compound
added), rub the polished surface free of residual polishing compound
particles.
6. Inspect the surface of the working electrode to make sure that it is clean.
Repeat Step 5, if necessary.

NOTE The polishing pads are reusable. Do not rinse the pol-
ishing compound from the pads. After initial use, add
only enough polishing compound to maintain the coat-
ing on the pad.

7. Replace the working electrode block and yoke knob. Fingertighten the
knob by turning it a full 360 degrees.

NOTE It is not possible to overtighten the yoke knob. Once


the knob clicks into place, it does not tighten any fur-
ther. The yoke knob ensures constant pressure is
applied to the cell.

8. Orient the cell assembly with the yoke knob on the left and push the cell
onto its mounting location in the DC compartment.
9. Reconnect the cell’s inlet and outlet lines.
10. Reconnect the electrical cables.
11. Start the pump flow.

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12. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.
13. Reapply the electrode potential. The baseline will drift for more than
1 hour as the cell re-equilibrates. Peak area values may require up to
12 hours to stabilize.

9.28.5 Replacing a pH-Ag/AgCl Reference Electrode


When to Replace a pH-Ag/AgCl Reference Electrode

Replace the pH-Ag/AgCl reference electrode if performance problems occur


that are not corrected by regenerating the electrode. Performance problems
can include no pH readouts, a shift in Ag/AgCl reference potential or
incorrect readouts, baseline spikes, or a decreased response even with a
freshly polished working electrode. The pH-Ag/AgCl reference electrode
typically lasts from 3 months to 1 year, depending on use.

NOTE To regenerate a pH-Ag/AgCl reference electrode, soak


it in a solution of 1 M KCl and 1 M HCl.

Items Needed

• pH-Ag/AgCl reference electrode (P/N 061879)

pH-Ag/AgCl Reference Electrode Replacement Procedure

1. Follow the instructions in Section 9.28.1 to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.

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9 • DC Service

2. Unscrew the pH-Ag/AgCl reference electrode and remove it from the cell
body (see Figure 9-56).

Unscrew
the pH-Ag/AgCl
reference electrode

Figure 9-56. Removing the pH-Ag/AgCl Reference Electrode


(Cell Configured for Analytical IC Shown)

3. Unscrew the storage cap from the new pH-Ag/AgCl reference electrode
(see Figure 9-57). Save the cap.
Always store the electrode in the storage cap filled with saturated KCl
solution when the cell is not in use. This prevents the pH-Ag/AgCl
reference electrode membrane from drying out and damaging the
electrode. See Section 6.4 for storage instructions.

Save the
storage cap

Figure 9-57. pH-Ag/AgCl Reference Electrode in Storage Cap

4. Rinse the new electrode thoroughly in ASTM Type I (18 megohm-cm)


filtered and deionized water that meets the specifications listed in
Section 1.5 to remove any precipitated salt.
5. Calibrate the pH-Ag/AgCl reference electrode (see Section 9.28.6).

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9.28.6 Calibrating the pH-Ag/AgCl Reference Electrode


When to Calibrate

• Calibrate after installing a new pH-Ag/AgCl reference electrode.

Items Needed

• A buffer solution with a pH of 7.00


• A second buffer solution with a different pH (typically one that matches
the pH of the eluent used in your application; in most cases, this is either
pH 10 or pH 4)

pH-Ag/AgCl Reference Electrode Calibration Procedure

1. Complete the following if you are calibrating an electrode that is currently


in use:
a. Follow the instructions in Section 9.28.1 to turn off the cell voltage,
stop the pump flow, and disconnect the cell from the detector.
b. Unscrew the pH-Ag/AgCl reference electrode and remove it from the
cell body (see Figure 9-56).
c. To remove any precipitated salt, rinse the pH-Ag/AgCl reference
electrode thoroughly in ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
2. With the pH-Ag/AgCl reference electrode removed from the cell, connect
the cell and electrode electrical cables to the detector.
3. On the Chromeleon 7 ePanel Set, click the ED tab; on the Chromeleon 6.8
panel tabset, click the EC Detector tab.

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9 • DC Service

4. Click the Calibration button. The Wellness panel opens, see Figure 9-58.

Figure 9-58. Wellness Panel: Dionex ICS-5000 Electrochemical


Detector
(Chromeleon 7 Version Shown)

5. Follow the instructions on the panel to calibrate the electrode.


6. Disconnect the pH-Ag/AgCl reference electrode cable and the cell cable.
7. Grasp the cell body and pull straight out to remove the cell from the
detector.
Capillary If you are installing the pH-Ag/AgCl reference electrode in a capillary IC
IC system, go on to page 396.
If you are installing the pH-Ag/AgCl reference electrode in an analytical IC
system, go on to page 398.

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Capillary Installing the pH-Ag/AgCl Reference Electrode in the Cell for a Capillary
IC IC System

1. To avoid any hydraulic pressure buildup when inserting the pH-Ag/AgCl


reference electrode into the cell, make sure that fitting plugs are not
installed on the cell inlet and outlet fittings.
2. Use a sharp tool (for example, the tip of a safety pin or a straight pin) to
remove the pH-Ag/AgCl reference electrode O-ring (see Figure 9-59).

pH-Ag/AgCl
Reference
Electrode
O-Ring
(remove for
capillary IC)

Figure 9-59. pH-Ag/AgCl Reference Electrode O-Ring

3. Using tweezers, install the reference electrode gasket for capillary IC


(P/N 072162) into the bottom of the reference electrode well (see
Figure 9-60).

Reference
Electrode Gasket
for Capillary IC

Figure 9-60. Reference Electrode Gasket for Capillary IC

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9 • DC Service

4. Make sure the gasket is centered in the bottom of the well and that it does
not block the inlet and outlet of the well. The inlet and outlet are small
round openings in the bottom of the well (see Figure 9-61).

Reference
Electrode Well
Inlet
Reference
Electrode Well
Outlet

Figure 9-61. Reference Electrode Well with Reference Electrode


Gasket for Capillary IC Installed

5. Verify that the reference electrode O-ring has


been removed and the reference electrode
gasket is correctly installed in the bottom of the
well.
6. Screw the pH-Ag/AgCl reference electrode into
the reference electrode well and tighten it
fingertight (see Figure 9-62).

Figure 9-62. Installing the pH-Ag/AgCl Reference


Electrode In the Reference Electrode Well

7. Orient the cell assembly with the yoke knob on the left and then push the
cell onto its mounting location on the ED.
8. Connect the reference electrode cable and the cell cable.
9. Reconnect the cell inlet and outlet lines.

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10. Start the pump flow.


11. Turn on the DC power.
12. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.

Installing the pH-Ag/AgCl Reference Electrode in the Cell for an


Analytical IC System

1. To avoid any hydraulic pressure buildup when inserting the reference


electrode into the cell, make sure that fitting plugs are not installed on the
cell inlet and outlet fittings.
2. Verify that the pH-Ag/AgCl reference electrode O-ring is present (see
Figure 9-63) and then screw the pH-Ag/AgCl reference electrode into the
reference electrode well and tighten it fingertight (see Figure 9-62).

pH-Ag/AgCl
Reference
Electrode
O-Ring

Figure 9-63. pH-Ag/AgCl reference electrode O-Ring

3. Orient the cell assembly with the yoke knob on the left (see Figure 9-52)
and push the cell onto its mounting location in the DC compartment.
4. Reconnect the cell inlet and outlet lines.
5. Start the pump flow.
6. Turn on the DC power.
7. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.

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9.28.7 Replacing the pH-Ag/AgCl Reference Electrode O-Ring


1. Follow the instructions in Section 9.28.1, to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.
2. Unscrew the pH-Ag/AgCl reference electrode and remove it from the cell
body (see Figure 9-64).

Unscrew the
pH-Ag/AgCl
reference
electrode

Figure 9-64. Removing the pH-Ag/AgCl Reference Electrode


(Cell Configured for Analytical IC Shown)

3. To remove any precipitated salt, rinse the pH-Ag/AgCl reference


electrode thoroughly in ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
4. Use a sharp tool (for example, the tip of a safety pin or a straight pin) to
remove the pH-Ag/AgCl reference electrode O-ring (see Figure 9-65).

pH-Ag/AgCl
Reference
Electrode
O-Ring

Figure 9-65. Removing the pH-Ag/AgCl Reference Electrode O-Ring

5. Slide the new O-ring (P/N 014067) onto the electrode.

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6. To avoid any hydraulic pressure buildup when inserting the pH-Ag/AgCl


reference electrode, make sure that fitting plugs are not installed on the
cell inlet and outlet fittings.
7. Screw the pH-Ag/AgCl reference electrode into the cell body and tighten
fingertight.
8. Orient the cell assembly with the yoke knob on the left and push the cell
onto its mounting location in the DC compartment (see Figure 9-52).
9. Reconnect the two cables and the liquid lines.
10. Start the pump flow.
11. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.

9.28.8 Replacing a PdH Reference Electrode


When to Replace a PdH Reference Electrode

Replace the PdH reference electrode if its sensing surface is damaged or if the
electrode no longer seals properly. Replace the PdH electrode if performance
has degraded (for example, lower response, higher background, or spikes).
The PdH reference electrode typically lasts several years, depending on use.

Items Needed

• PdH reference electrode (P/N 072075)


• Tweezers
• Wrench

PdH Reference Electrode Replacement Procedure

1. Follow the instructions in Section 9.28.1 to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.

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9 • DC Service

2. Use a wrench to unscrew the PdH reference electrode nut and then
remove the nut from the reference electrode well (see Figure 9-66).

Nut

Figure 9-66. Unscrewing the PdH Reference Electrode Nut

3. Pull the reference electrode out of the well (see Figure 9-67).

PdH Reference
Electrode

Figure 9-67. Removing the PdH Reference Electrode from the


Reference Electrode Well

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4. Using tweezers, remove the PdH reference electrode gasket from the well
(see Figure 9-68).

Notch in
well

PdH Reference
Electrode Gasket

Figure 9-68. Removing the PdH Reference Electrode Gasket

5. Using tweezers, grasp the new PdH reference electrode gasket


(P/N 072214) on its edge (see Figure 9-69). To avoid deforming the
gasket cutout, do not place the tweezer tips on the cutout.

Cutout PdH Reference


Electrode Gasket

Figure 9-69. Installing the PdH Reference Electrode Gasket

6. Align the gasket so that the notched edge of the gasket aligns with the
corresponding notch in the reference electrode well and press the gasket
into the well.

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9 • DC Service

7. To avoid any hydraulic pressure buildup when inserting the reference


electrode into the cell, make sure that fitting plugs are not installed on the
cell inlet and outlet fittings.
8. Align the fitting on the end of the PdH reference electrode so that the
knobs on the fitting align with the grooves in the reference electrode well
(see Figure 9-70).
9. Insert the fitting into the well.

PdH Reference
Electrode

Knobs

Grooves

Figure 9-70. Inserting the PdH Reference Electrode Fitting into the
Reference Electrode Well

10. Screw the nut on the PdH reference electrode into the reference electrode
well and tighten it fingertight (see Figure 9-71). After fingertightening,
use a wrench to tighten the nut an additional 20 to 30 degrees.

Nut

Figure 9-71. Installing the PdH Reference Electrode Nut

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11. Orient the cell assembly with the yoke knob on the left and then push the
cell onto its mounting location on the ED.
12. Connect the reference electrode cable and the cell cable.
13. Reconnect the cell inlet and outlet fittings.
14. Condition the PdH reference electrode (refer to the instructions below).

Conditioning the PdH Reference Electrode

Condition the PdH reference electrode after plumbing the cell:


1. On the Chromeleon 7ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. Pump panel: Set the pump flow rate to 0.01 mL/min. This turns on
the pump flow, also.
b. EG panel: Enter 100 mM in the Target Concentration field. This
turns on the power to the EGC, also.
c. Verify that eluent is exiting the cell.
d. ED panel: Set the reference electrode mode to PdH.
e. Select DC amperometry mode, set the cell voltage to 0.000 V, and
turn on the cell voltage. Switch to integrated amperometry mode and
select the PdH-referenced carbohydrate waveform.
2. Condition the electrode for 1 hour at these settings.
3. Turn off the pump flow. This turns off the EGC power and the cell
voltage.

9.28.9 Replacing an ED Detector


1. Turn off the pump flow.
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.
3. Open the DC upper door and disconnect the cell inlet and outlet lines.
4. Disconnect the reference electrode cable and the cell cable.
5. Grasp the cell body and pull straight out to remove the cell from the
detector.

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9 • DC Service

6. Press the release lever located below the detector. The detector pops out
slightly from the DC compartment. Grasp the detector and pull outward to
remove the detector from the compartment.
7. Note the electrical plug on the back of the detector and the receptacle on
the inside of the DC.
8. Push the new detector into the opening in the DC and press firmly to
ensure the electrical connection is secure.
9. Reinstall the cell and reconnect the cell inlet and outlet lines and the
cables.

NOTE If you are installing an ED detector in a system that previ-


ously was set up for conductivity detection, remove the sup-
pressor cartridge from the IC Cube and replace it with a
suppressor bypass cartridge (P/N 072055). For IC Cube car-
tridge installation instructions, see Section 9.26.1.

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ICS-5000
TC TC Service

To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le compartiment thermique


avant d'ouvrir la porte ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der TC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

9.29 Replacing Tubing and Fittings


The TC is plumbed with the tubing and fittings listed below.

Tubing Size and Type Color P/N Used For


0.125 mm (0.005 in) ID PEEK Black 052310 Standard bore
system connections
0.25 mm (0.010 in) ID PEEK Red 052306 Microbore system
connections
10 mm (0.39 in) ID polyethylene Colorless 055075 Waste line

Use double-cone 10-32 ferrule fittings (P/N 043276) and 10-32 bolts
(P/N 043275) for all tubing connections. For tightening requirements, refer to
Installation of Dionex Liquid Line Fittings (Document No. 031432). The
manual is on the Thermo Scientific Reference Library DVD (P/N 053891).
Use a tubing cutter to cut tubing to the required length. Make sure the cut is at
a right angle to the length of the tubing and there are no nicks or burrs on the
end.

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9.30 Setting Up the Column ID System


The TC Ship Kit (P/N 064789) includes two column ID chip cards (P/N 5710.
1500). The optional Column ID Kit (P/N 066353) includes five chip cards.
These are the main steps required to implement the column ID system:
• Specify the column you want to monitor.
• Install a column ID chip card for the column.
• Close the TC door and select the column properties to be monitored.

To select the column to be monitored:

1. Start the Chromeleon 7 Instrument Configuration program or the


Chromeleon 6.8 Server Configuration program.
2. Under the instrument or timebase, right-click the TC and select
Properties on the context menu.
3. In the TC Properties dialog box, select the Components tab to display the
Components tab page (see Figure 9-72).

Figure 9-72. TC Properties Dialog Box: Components Tab Page

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9 • TC Service

4. Select the check box for the column to be monitored (A, B, C, or D) and
click OK.

To install a column ID chip card:

1. To attach a column ID chip card to the column,


wrap the strap around the column, insert the
rivet into one of the holes on the strap, and
press to secure the strap to the column (see
Figure 9-73).

Figure 9-73. Attaching the Column ID System to the Column

2. Insert the chip card (with the Dionex logo


facing up) into the appropriate card reader (A,
B, C, or D) along the top of the compartment
(see Figure 9-74).
When the chip card is installed correctly, the
LED next to the slot is green.

Figure 9-74. Inserting a Column ID Chip Card

3. Install a chip card for any other columns to be monitored.

To select the column properties to be monitored:

1. Close the TC door, if it is open. (You cannot select column properties


unless the door is closed.)
2. On the TC Control panel, click the Column Details... button.
This opens the Column Details screen.
3. For each column, specify the properties the column ID system will
monitor. When you finish, click Close.

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9.31 Rebuilding an Injection Valve


Thermo Fisher Scientific recommends rebuilding the TC injection valve
annually. The Injection Valve Rebuild Kit (P/N 057896, 6-port valve;
P/N 061759, 10-port valve) contains all required replacement parts.

NOTE Substitution of non-Dionex/Thermo Fisher Scientific parts


may impair valve performance and void the product war-
ranty.

NOTE If you prefer, you can replace the injection valve “pod,”
instead of rebuilding the valve. Replacing the pod is easier
and faster than rebuilding the valve.

1. Turn off the pump flow.


2. Press the POWER button on the front of the TC to turn off the power.

To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le compartiment thermique


avant d'ouvrir la porte ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der TC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs oder Servicearbeiten
durchführen.

3. Open the TC door.


4. Disconnect each liquid line connected to the injection valve.
5. Follow the instructions provided in the Rebuild Kit to replace the rotor
seal, isolation seal, and stator face.

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9 • TC Service

6. Reconnect all liquid lines to the injection valve (see Figure 9-75).

(Green)

TO INJECT SAMPLE IN
VALVE -W (from door
inject port or
autosampler)
W (6)

S (5)

25 μL SAMPLE LOOP
(Orange) L (4)

TO INJECT
VALVE -P TO INJ (Red - microbore)
VALVE -C (Black - standard bore)

Figure 9-75. Injection Valve Plumbing (6-Port Valve)

7. Turn on the power to the TC.


8. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required (see Section 9.29).
9. Close the TC door.

9.32 Replacing an Injection Valve Pod


This procedure describes how to replace the mechanical part (the “pod”) of
the TC injection valve.

NOTE If the valve electronics require service, contact Thermo


Fisher Scientific. Electronics-related repair procedures must
be performed by Thermo Fisher Scientific personnel.

NOTE Substitution of non-Dionex/Thermo Fisher Scientific parts


may impair valve performance and void the product war-
ranty.

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1. Turn off the pump flow from the Control panel in Chromeleon 6.8 or
Chromeleon 7 or press PUMP FLOW on the front of the pump.

To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.

Afin d'éviter toute brûlure, laisser refroidir le compartiment thermique


avant d'ouvrir la porte ou d'effectuer des opérations de maintenance.

Um Verletzungen zu vermeiden, warten Sie bitte, bis der TC abgekühlt


ist, ehe Sie die Tür öffnen bzw. Wartungs-oder Servicearbeiten
durchführen.

2. Open the TC door.


3. Disconnect each liquid line connected to the valve.
4. Unscrew the black locking ring on
the front of the valve (see
Figure 9-76) and remove the ring.
5. Grasp the front of the valve pod
and pull out firmly to remove it Black
from the TC. Locking
Ring

Figure 9-76. Unscrewing the Locking Ring

6. Check that the new pod has the correct number of ports for the injection
valve being serviced.
7. Align the slots in the new pod with the runner in the valve holder in the
TC (see Figure 9-77). Valve pods are keyed to fit only one way (one slot
is narrower than the other). Verify that the slots are aligned with their
matching runners.

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9 • TC Service

8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-77). If necessary, twist the end of the
pod to adjust the position of the splines.

Valve Pod Valve Holder

Slot (larger)
Runner (larger)

Splines

Figure 9-77. Injection Valve Pod and Pod Holder

9. Push the pod into the holder until it clicks into place. Replace the black
locking ring.
10. Reconnect all liquid lines to the valve.
11. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required (see Section 9.29).
12. Close the TC door.

9.33 Changing the Main Power Fuses


1. Press the POWER button on the front of the TC for 2 seconds to turn off
the power.
2. Disconnect the main power cord from both its source and from the TC
rear panel.

HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the TC.

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HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa


source et du panneau arrière du TC.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und


der Netzbuchse auf der Rückseite des TC.

3. The fuse cartridge is located next to the main power switch (see
Figure 9-78). Use a small screwdriver to remove the fuse cartridge.

Fuse Cartridge

Figure 9-78. TC Fuse Cartridge

4. Replace the two fuses with new 2 A IEC 60127-2 time lag fuses
(P/N 954776). Thermo Fisher Scientific recommends always replacing
both fuses.
5. Reinstall the fuse cartridge.
6. Reconnect the main power cord and turn on the power.

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A • Specifications

ICS-5000
DP/SP DP/SP Specifications

ICS-5000 SP Single Pump and DP Dual Pump Specifications


Type Dual-piston (in series), microprocessor controlled,
constant stroke, variable speed, patented
Isokinetic Eluent Precompression
Construction Chemically inert, metal-free PEEK pump heads
and flow path; compatible with aqueous eluents
from pH 0–14 and reversed-phase solvents
Pressure Range 0–35 MPa (0–5000 psi) (Analytical)
0–41 MPa (0–6000 psi) (Capillary)
Flow Rate Range • 0.000–10.000 mL/min with settable flow
increments at 0.001 mL/min (Analytical)
• 0.001–3.000 mL/min with settable flow
increments at 0.0001 mL/min (Capillary)
Flow Rate Precision <0.1% (Analytical)
Flow Rate Accuracy <0.1% (Analytical) at 14 MPa (2000 psi)
Pressure Ripple < 1.0% (Analytical) at 1.0 mL/min typical
< 0.2% (with damper) at 10 μL/min at 14 MPa
(2000 psi)
Pressure None required
Vacuum Degasser Integrated, optional 1 channel for isocratic pump or
4 channel for quaternary pump
Piston Seal Wash Standard, automatic operation
Gradient Formation Quaternary low pressure (Analytical only) or
electrolytic eluent generation at high pressure
(Analytical and Capillary)
RFIC-EG Gradients 0.1–100 mM (Analytical)
0.1–200 mM (Capillary)

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ICS-5000 SP Single Pump and DP Dual Pump Specifications (Continued)


Gradient Profiles Any combination of an unlimited number of linear,
convex, and concave positive and negative
gradient profiles
Gradient Proportioning ±0.5% at 2 mL/min
Accuracy and Precision
(Analytical only)
Gradient Mixing Passive mixers for 2 mm and 4 mm ID columns,
(Analytical only) optional
Eluent Generation Optional eluent generation (RFIC-EG)
Eluent On/Off Valve Electrically actuated, standard
Leak Sensor Optical, standard
System Software
Software Chromeleon Chromatography Management
Software, supports Microsoft Windows® XP or
Vista
Automated Procedure Yes, standard feature
Wizards
System Smart Startup Yes, standard feature
and Shutdown
System Wellness and Yes, standard feature
Predictive Performance
Application Templates Yes, standard feature
Automation Support of Yes, fully controls over 300 different instruments
3rd Party Instruments from more than 30 manufacturers, including GC,
HPLC, and MS
Customizable System Yes, standard feature
Control Panels
Signal Channels Pump pressure
Data Trending Plots Yes, all device numerical parameters
System Status Virtual Yes, standard feature
Channels
Power Failure Protection Yes, standard feature

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A • Specifications

ICS-5000 SP Single Pump and DP Dual Pump Specifications (Continued)


System Trigger Yes, standard feature
Commands and
Conditionals
Daily Audit Trail Yes, standard feature
Sample Audit Trail Yes, standard feature
System Calibration Yes, factory, present, and previous. Completely
Storage user selectable
Customized Reporting Yes, standard feature with unlimited report
workbooks
GLP Compliance Yes, optional
Electrical
Main Power 90–264 VAC, 47–63 Hz
Requirements (Auto-sensing power supply; no manual voltage or
frequency adjustment required)
Typical input power: 28 W
Maximum line draw: 1.2 A at 110 VAC
Fuse Requirements Two IEC 60127-2 slow-blow fuses (P/N 954773)
rated at 2 A, 250 V
Physical
Dimensions (h × w × d) 36 × 21 × 48 cm (14 × 8.25 × 19 in.)
Weight SP: 20.4 kg (45 lb)
DP: 24.1 kg (55 lb)
Flow Path All polymeric (PEEK), anion or cation
configurations
Environmental
Operating Temperature 4–40 °C (40–104 °F)
Operating Humidity 5–95% relative humidity (noncondensing)

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ICS-5000
EG EG Specifications

ICS-5000 EG Eluent Generator Specifications


Minimum and Maximum 0.1–100 mM (Analytical)
Eluent Concentrations 0.1–200 mM (Capillary)
Flow Rates 0.100–3.000 mL/min (Analytical)
0.001–0.030 mL/min (Capillary)
Eluent Types KOH, LiOH, NaOH
(Analytical) Carbonate
Carbonate/Bicarbonate
Carbonate with pH modifier
MSA
Eluent Types KOH
(Capillary) MSA
Maximum Operating 21 MPa (3000 psi) (Analytical)
Pressure 35 MPa (5000 psi) (Capillary)
Maximum Solvent Cations: None
Concentration (Analytical Anions: 25% methanol
and Capillary)
Gradient Profiles Standard, any combination of an unlimited number
of linear, convex, and concave positive and
negative gradient profiles
Number of Cartridges Two–dual cartridge support
Supported
RFIC Eluent Degasser Eluent degasser housed in the EG module
(Analytical Only)
System Software
Software Chromeleon Chromatography Data System,
supports Microsoft Windows XP and Vista
Automated Procedure Yes, standard feature
Wizards
System Smart Startup Yes, standard feature
and Shutdown
System Wellness and Yes, standard feature
Predictive Performance

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Dionex ICS-5000 Operator’s Manual

ICS-5000 EG Eluent Generator Specifications (Continued)


Application Templates Yes, standard feature
Automation Support of Yes, fully controls over 300 different instruments
Third-Party Instruments including GC, HPLC, and MS from more than 30
manufacturers.
Customizable System Yes, standard feature
Control Panels
Signal Channels Eluent concentration
Data Trending Plots Device numerical parameters plotted
System Status Virtual Yes, standard feature
Channels
Power Failure Protection Yes, standard feature
System Trigger Yes, standard feature
Commands and
Conditionals
Daily Audit Trail Yes, standard feature
Sample Audit Trail Yes, standard feature
Eluent Cartridge Yes, serial number and expiration date
Information Storage
Customized Reporting Yes, standard feature with unlimited report
workbooks
GLP Compliance Yes, optional package provides security system,
modification history, and electronic signatures
Electrical
Main Power 90–264 VAC, 47–63 Hz
Requirements (Auto-sensing power supply; no manual voltage or
frequency adjustment required)
Typical input power: 18 W
Maximum line draw: 1 A at 110 VAC
Fuse Requirements Two IEC 60127-2 slow-blow fuses (P/N 954773)
rated at 2 A, 250 V

420 Doc. 065342-06 12/11


A • EG Specifications

ICS-5000 EG Eluent Generator Specifications (Continued)


Physical
Dimensions (h × w × d) 41 × 23 × 56 cm (16 × 8.75 × 21.5 in.)
Weight 25 kg (40 lb) (without optional items)
Flow Path All polymeric (PEEK), anion or cation
configurations
Environmental
Operating Temperature 4–40 °C (40–104 °F)
Operating Humidity 5–95% relative humidity (noncondensing)

ICS-5000 ER Eluent Regeneration Specifications (Analytical IC Only)


Eluents Carbonate and carbonate/bicarbonate
combinations up to 20 mM
MSA up to 34 mM
Flow Rates 1.00–2.00 mL/min
Continuous Operation Up to 28 days or 2000 samples, typically
with 4 L of Eluent
Always On, Always Yes, standard feature
Ready Capable
Remains Fully Calibrated Yes, standard feature. Results are traceable to a
for Extended Periods of single calibration
Time (28 Days)
System Wellness Consumables usage monitoring for predictive
maintenance
Maximum Operating 21 MPa (3000 psi)
Pressure
Operating Temperature 4–40 °C
Range

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Dionex ICS-5000 Operator’s Manual

422 Doc. 065342-06 12/11


ICS-5000
DC DC Specifications

Dionex ICS-5000 DC Detector/Chromatography Compartment Specifications


Dual Temperature Zone Upper Zone Temperature Range: 10–40 °C
Model: Independent (minimum temperature: ambient -20 °C)
Temperature Control of (maximum temperature: ambient +20 °C)
Each Zone Lower Zone Temperature Range: 10–70 °C
(minimum temperature: ambient -15 °C)
(maximum temperature: ambient +50 °C)
Temperature Accuracy: ±0.5 °C
Temperature Stability: ±0.2 °C
Temperature Precision: ±0.2 °C
Lower Zone (Analytical) Injection Valves: Up to two 6- or 10-port valves
(upgradeable, field installable)
Up to two column sets 1–9 mm diameter
Maximum Column Length: 250 mm plus 50 mm
guard column
Precolumn Heat Exchangers: two (2 mm or 4 mm
column ID version)
Automation Manager: Injection Valves: Up to two high-pressure valves,
(Optional, Analytical either 6- or 10-port, 2-position
Only) Low Pressure Valves: Up to two inert, 2- or 3-way
Reaction Coil Heater (RCH): Holds two reaction
coils
RCH Temperature Range: 5 °C above upper zone,
80 °C maximum
AutoPrep Kit: Dual loop with sample pre-
concentration
All valves and heater upgradeable and field
installable
Capillary IC Cube: One or two IC Cube modules hold the following:
(Optional – but required Injection Valves: Up to two (one per cube) high-
for capillary chemistries) pressure valves, 4-port, 2-position
EG Degasser
Column and Guard
Carbonate Removal Device
Capillary Suppressor (See Suppressor section)
IC Cubes and cartridges are customer installable,
with pre-formed tubing and color-coded labeling
Capillary column heater, 15 to 80 °C

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Dionex ICS-5000 Operator’s Manual

Dionex ICS-5000 DC Detector/Chromatography Compartment Specifications


Flow Path Plumbing configurations for 4 mm, 2 mm, and
0.4 mm columns, fully inert, PEEK
Detectors Any combination of two conductivity or
electrochemical detectors, upgradeable and field
installable. Dual detectors can be operated
simultaneously or independently. Optional remote
operation up to 3 m from instrument
Analog Signal Output Two analog output channels, two 24 V relays, two
TTL Out and eight TTL In lines, upgradeable and
field installable, optional
Leak Detection Optical leak sensor standard
Application Control Yes, standard. All DC modules come equipped with
Automation two switched AC controllers built-in to automate
external devices and the ability to control up to six
low-pressure 2-way or 3-way valves for fluidic
automation
Suppression
Non -suppressed Yes, supported
conductivity
Suppressor wear parts None. No valves, pumps, peristaltic pump tubin,g
or inline filters required
Chemical Suppression 2 mm and 4 mm anion and cation membrane
suppression available
Displacement Chemical 2 mm and 4 mm anion and cation membrane
Suppression suppression available
Electrolytic Suppression, 0.4 mm (with optional IC Cube), 2 mm and 4 mm
Self-Regenerating. anion and cation. Membrane and MonoDisc
suppression bed types available. Membrane for
capillary (0.4 mm) suppressor.
Electrolytic Suppression, 0.4 mm (with optional IC Cube), 2 mm and 4 mm
Self-Regenerating, anion and cation. Membrane and MonoDisc
External Water Mode suppression bed types available for 2 mm and
4 mm. Membrane for capillary (0.4 mm)
suppressor.
Salt Converter Available in 2 mm and 4 mm versions
AMMS-ICE Available in 2 mm and 4 mm versions

424 Doc. 065342-06 12/11


A • DC Specifications

Dionex ICS-5000 DC Detector/Chromatography Compartment Specifications


Carbonic Acid Removal ASRS and AMMS plus CRD 300 for 2 mm and
for Anions 4 mm versions, CRD (0.4 mm) for capillary
suppressors
Suppression Capacities Anion SRS 300 (4 mm): 200 μeq/min
Cation SRS 300 (4 mm): 110 μeq/min
Anion SRS 300 (2 mm): 50 μeq/min
Cation SRS 300 (2 mm): 37.5 μeq/min
Anion MMS 300 (4 mm): 150 μeq/min
Cation MMS 300 (4 mm): 150 μeq/min
Anion MMS 300 (2 mm): 37.5 μeq/min
Cation MMS 300 (2 mm): 37.5 μeq/min
Anion AES: 25 μeq/min
Cation AES: 25 μeq/min
AMMS-ICE: N/A
Anion CES (0.4 mm ): 2 μeq/min
Cation CES (0.4 mm ): 1.5 μeq/min
Suppressor Void SRS 300 (4 mm): <50 μL
Volumes SRS 300 (2 mm): <15 μL
MMS 300 (4 mm): <50 μL
MMS 300 (2 mm): <15 μL
AMMS-ICE 300 (4 mm): <50 μL
AMMS-ICE 300 (2 mm): <15 μL
AES (Anion or Cation): <35 μL
Anion CES (0.4 mm): <1.0 μL
Cation CES (0.4 mm):<1.0 μL
System Software
Software Chromeleon Chromatography Data System,
requires Microsoft Windows XP or Vista
Automated Procedure Yes, standard feature
Wizards
System Smart Startup Yes, standard feature
and Shutdown
System Wellness and Yes, standard feature
Predictive Performance
Application Templates Yes, standard feature

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Dionex ICS-5000 Operator’s Manual

Dionex ICS-5000 DC Detector/Chromatography Compartment Specifications


Automation Support of Yes, fully controls over 300 different instruments
Third-Party Instruments from more than 30 manufacturers, including GC,
HPLC, and MS.
Customizable System Yes, standard feature
Control Panels
Signal Channels Detector signals, detector background signals,
temperatures
Data Trending Plots Yes, all device numerical parameters plotted
System Status Virtual Yes, standard feature
Channels
Power Failure Protection Yes, standard feature
System Trigger Yes, standard feature
Commands and
Conditionals
Daily Audit Trail Yes, standard feature
Sample Audit Trail Yes, standard feature
System Calibration Yes, factory, current, and previous. Completely
Storage user selectable
Customized Reporting Yes, standard feature with unlimited report
workbooks
GLP Compliance Yes, optional
Electrical
Main Power 90–265 VAC, 47–63 Hz (Auto-sensing power
Requirements supply; no manual voltage or frequency adjustment
required)
Typical input power: 200 W
Maximum line draw: 9.2 A at 110 VAC
Fuse Requirements Two IEC 60127-2 slow-blow fuses (P/N 954772)
rated at 10 A, 250 V

426 Doc. 065342-06 12/11


A • DC Specifications

Dionex ICS-5000 DC Detector/Chromatography Compartment Specifications


Physical Specifications
Dimensions 44.5 × 42 × 57 cm (17.5 × 16.5 × 22.5 in)
(h × w × d):
Weight 38 kg (84 lb)
Flow Path All polymeric (PEEK), anion or cation
configurations
Environmental
Operating Temperature 4–40 °C (40–104 °F)
Operating Humidity 5– 95% relative humidity (noncondensing)

Dionex ICS-5000 Conductivity Detector Specifications


Electronics Type Microprocessor controlled digital signal processing,
autoranging
Cell Drive 8 kHz square wave
Linearity 1%
Resolution 0.00238 nS/cm
Output Range Digital Signal Range: 0–15,000 µS/cm,
Analog Signal Range: 0–15,000 µS/cm
Noise, Wet <0.2 nS at 23 µS/cm background
<0.1 nS at 1 µS/cm background
Filter Rise times 0 to 10 s, programmable
Sampling Rate 1 to 100 Hz, user settable or automatic
Cell Temperature 5 °C above DC upper zone temperature to 60 °C
maximum. User settable, working range is identical
to settable range.
Cell Temperature <0.001 °C
Stability
Cell Temperature Default 1.7% per °C; programmable from 0–3% per
Compensation °C
Flow Cell Maximum 10 MPa (1500 psi)
Pressure
Flow Cell Volume 0.7 µL (Analytical), 0.02 µL (Capillary)

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Dionex ICS-5000 Operator’s Manual

Dionex ICS-5000 Conductivity Detector Specifications (Continued)


Cell Electrodes Passivated 316 stainless steel. Compatible with
MSA
Cell Body Chemically inert polymeric material
Heat Exchanger Inert, tortuous-path for low axial dispersion
System Software
Software Chromeleon Chromatography Data System,
requires Microsoft Windows XP or Vista
Automated Procedure Yes, standard feature
Wizards
System Smart Startup Yes, standard feature
and Shutdown
System Wellness and Yes, standard feature
Predictive Performance
Application Templates Yes, standard feature
Automation Support of Yes, fully controls over 300 different instruments
Third-Party Instruments from more than 30 manufacturers, including GC,
HPLC, and MS
Customizable System Yes, standard feature
Control Panels
Signal Channels Conductivity, Total Conductivity
Data Trending Yes, all device numerical parameters plotted
System Status Virtual Yes, standard feature
Channels
Power Failure Protection Yes, standard feature
System Trigger Yes, standard feature
Commands and
Conditionals
Daily Audit Trail Yes, standard feature
Sample Audit Trail Yes, standard feature
System Calibration Yes, factory, present, and previous. Completely
Storage user selectable
Customized Reporting Yes, standard feature with unlimited report
workbooks

428 Doc. 065342-06 12/11


A • DC Specifications

Dionex ICS-5000 Conductivity Detector Specifications (Continued)


GLP Compliance Yes, optional
Physical
Dimensions 6.9 × 16.7 × 9.9 cm (2.7 × 6.5 × 3.9 in)
(h x w x d)
Weight 400 g (1.6 lb.)

ICS-5000 ED Electrochemical Detector Specifications


Electronics Type Microprocessor controlled digital signal processing
Electronic Noise (Wet IPAD (Au electrode) < 50 pC @ 10 mM KOH, DC
Noise) (Capillary and Amperometry (GC) < 10 pA @ catecholamine
Analytical) eluent
Potential Range -2.0 to 2.0 V in 0.001 V increments
Signal Range: Digital and Integrated amperometry: 50 pC to 200 µC
Analog DC amperometry: 5 pA to 74 µA
Filter 0–10 s response time, user settable
Control Mode Local or remote control using relay closures or
TTL, or control using Chromeleon via DC module
Cell Body Titanium body with narrow bore PEEK inlet tubing
for capillary format, titanium inlet tubing for
analytical format. Compatible with 0.2–0.6 mm ID
columns (PEEK inlet), 2– 7 mm ID columns
(titanium inlet)
Working Electrodes Conventional: gold, glassy carbon, platinum, and
silver
Disposable: gold, platinum, carbon and silver
Reference Electrode pH-Ag/AgCl combination, one piece design
(Analytical and Capillary)
PdH combination, one piece design
(Capillary only)
Autoranging Yes
Analog Output User selectable full scale of 10, 100, or 1000 mV
Cell Volume @ Working <0.2 µL
Electrode

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Dionex ICS-5000 Operator’s Manual

ICS-5000 ED Electrochemical Detector Specifications (Continued)


Maximum Cell Operating 0.7 MPa (100 psi)
Pressure
System Software
Software Chromeleon Chromatography Data System,
requires Microsoft Windows XP or Vista
Detection Modes DC amperometry, pulsed amperometry, and
integrated amperometry
Detection modes include use of multiple
waveforms and multiple integration times to
optimize detection conditions for individual
analytes
Integrated amperometry mode—unlimited changes
to the waveform profile's number of segments,
duration of each segment, and voltage applied at
each segment
3-D Amperometry Three-dimensional display of the raw integrated
amperometry data set, with crosshairs on an
isoamperometric plot used to select slices of the
plot along the applied voltage axis (to render a
chromatogram) and along the time axis (to render
a voltammogram)
Automated Procedure Yes, standard feature
Wizards
System Smart Startup Yes, standard feature
and Shutdown
System Wellness and Yes, standard feature
Predictive Performance
Application Templates Yes, standard feature
Automation Support of Yes, fully controls over 300 different instruments
Third-Party Instruments from more than 30 manufacturers, including GC,
HPLC, and MS
Customizable System Yes, standard feature
Control Panels
Signal Channels Electrochemical and total electrochemical signals
Data Trending Plots Yes, all device numerical parameters plotted

430 Doc. 065342-06 12/11


A • DC Specifications

ICS-5000 ED Electrochemical Detector Specifications (Continued)


System Status Virtual Yes, standard feature
Channels
Power Failure Protection Yes, standard feature
System Trigger Yes, standard feature
Commands and
Conditionals
Daily Audit Trail Yes, standard feature
Sample Audit Trail Yes, standard feature
System Calibration Yes, factory, present, and previous. Completely
Storage user selectable
Customized Reporting Yes, standard feature with unlimited report
workbooks
GLP Compliance Yes, optional
Physical
Dimensions 6.9 × 16.7 × 9.9 cm (2.7 × 6.5 × 3.9 in)
(h x w x d)
Weight 400 g (1.6 lb.)

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Dionex ICS-5000 Operator’s Manual

432 Doc. 065342-06 12/11


ICS-5000
DC TC Specifications

ICS-5000 TC Thermal Compartment Specifications


Temperature Range 5–85 °C (max. 18 °C below ambient) in 0.1 °C
increments
Temperature Accuracy: ±0.5 °C
Performance Stability: ±0.1 °C
Precision: ±0.1 °C
Heat-up/Cool-down Time Typically 15 min
20 °C to 50 °C and 50 °C to 20 °C
High-Pressure Valve 6-port, 2-position Rheodyne PEEK (injection) valve
Types 10-port, 2-position Rheodyne PEEK (switching)
valve
Column Capacity Three column sets; 1–9 mm
Maximum Column 300 mm + 50 mm guard column
Length
Precolumn Heat Two low delay volume exchangers
Exchangers (optional)
Leak Detection Humidity and vapor sensors
TTL and Relay Inputs Two digital inputs/outputs
and Outputs Two relay outputs
Control Chromeleon Chromatography Data System
Computer Connection USB
Electrical
Main Power 90–264 VAC, 47–63 Hz (Auto-sensing power
Requirements supply; no manual voltage or frequency adjustment
required)
Power limit: 150 W
Fuse Requirements Two IEC 60127-2 time lag fuses (P/N 954776)
rated at 2 A, 250 V
Physical
Dimensions 17.4 × 44.4 × 50.3 cm (6.8 × 17.5 × 19.8 in.)
Weight 15.4 kg (34 lb)

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Dionex ICS-5000 Operator’s Manual

ICS-5000 TC Thermal Compartment Specifications (Continued)


Environmental
Operating Temperature 10–35 °C (50–95 °F)
Operating Humidity 5–80% relative (noncondensing)

434 Doc. 065342-06 12/11


B • Reordering Information

ICS-5000
DP/SP DP/SP Reordering Information

Part Number Item


Pump Head Components
074447 (capillary) Primary pump head
062083 (analytical)
074240 (capillary) Secondary pump head
062079 (analytical)
044541 (capillary) Inlet check valve assembly (for primary pump head)
045722 (analytical) (includes inlet nut and 1/8 in cartridge)
044520 (capillary) Outlet check valve assembly (for primary pump head)
045721 (analytical) (includes outlet nut and 1/8 in cartridge)
075493 (capillary) Main piston seal
064946 (analytical)
074371 Backup ring (for capillary pumps)
040695 O-ring (for capillary or analytical pump)
074446 (capillary) Seal wash body
062064 (analytical)
068628 (capillary) Piston seal wash seal
063382 (analytical)
068627 (capillary) Retainer for piston seal wash seal
062092 (analytical)
068646 (capillary) Piston
062082 (analytical)
063968 Priming valve for secondary pump head
(for capillary or analytical pump)
063382 Priming valve knob seal for secondary pump head
(for capillary or analytical pump)

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Dionex ICS-5000 Operator’s Manual

Part Number Item


Piston Seal Wash System
064155 Piston seal wash reservoir
063268 PharMed tubing, 0.159 cm (0.0625 in) ID
Note: Order 12 in of tubing for replacement of piston
seal wash tubing.
064079 Tygon 2075 tubing, 0.15 cm (0.060 in) ID
Note: Order 12 in of tubing for replacement of piston
seal wash tubing.
063518 External Seal Wash Kit
Eluent Storage and Delivery
072059 EO without reservoirs
072057 Dionex ICS-5000 Eluent Organizer with 2 2-liter
reservoirs
072058 Dionex ICS-5000 Eluent Organizer with 4 2-liter
reservoirs
063291 Eluent reservoir (plastic), 1-liter
062510 Eluent reservoir (plastic), 2-liter
063292 Eluent reservoir (plastic), 4-liter
074423 EO Regulator Accessory and Stand
064792 TC/VWD/PDA Regulator Bracket Kit
074422 Regulator
045987 Filter, end-line
044105 Filter, high-pressure inline
Miscellaneous
042126 GM-3 Gradient Mixer
049135 GM-4 Gradient Mixer
043276 Ferrule fitting, 10-32 double-cone
0643275 Fitting bolt, 10-32 (for double-cone ferrule fitting)
062511 Ferrule fitting, 1/16 in
052230 Fitting bolt, 1/16 in
042772 Plug

436 Doc. 065342-06 12/11


B • Reordering Information

Part Number Item


054578 Syringe, 10 cc
954773 Fuse, IEC 60127-2 slow-blow; rated at 2 A, 250 V
063246 USB cable, 1 m (3 ft) long
005.9001A Cinch connector, 2-pin
Maintenance Kits
075038 ICS-5000 Analytical Pump Preventive Maintenance Kit
075039 ICS-5000 Capillary Pump Preventive Maintenance Kit

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Dionex ICS-5000 Operator’s Manual

438 Doc. 065342-06 12/11


ICS-5000
EG EG Reordering Information

Part Number Item


Consumables for Capillary EG
072076 EGC KOH (Capillary)
072077 EGC MSA (Capillary)
072078 CR-ATC (Capillary)
072079 CR-CTC (Capillary)
Consumables for Analytical EG
074536 EGC III K2CO3
074532 EGC III KOH
074534 EGC III LiOH
074535 EGC III MSA
074533 EGC III NaOH
060477 CR-ATC
060478 CR-CTC
080135 EPM III Electrolytic pH Modifier
061686 EGC-CO3 Mixer (4 mm)
063443 EGC-CO3 Mixer (2 mm)
Precision Cut Tubing for Capillary EG
072203 0.062 mm (0.0025 in) ID PEEK, 61 cm (24 in); CR-TC
ELUENT OUT to EG Degas ELUENT IN
072204 0.062 mm (0.0025 in) ID PEEK, 18 cm (7 in); CR-TC
ELUENT IN to EGC OUT
Backpressure Coils
053762 Backpressure coil, 2.0 mL/min, 500 psi, 4 mm
053763 Backpressure coil, 2.0 mL/min, 1000 psi, 4 mm
053764 Backpressure coil, 0.5 mL/min, 500 psi, 2 mm
053765 Backpressure coil, 0.5 mL/min, 1000 psi, 2 mm

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Dionex ICS-5000 Operator’s Manual

Part Number Item


Miscellaneous
074459 EG degas cartridge (for capillary IC systems). Can be
used with system pressures up to 35 MPa (5000 psi).
074218 RFIC Eluent Degasser (f5or analytical IC systems)
954773 Fuse, IEC 60127-2 slow-blow; rated at 2 A, 250 V
063246 USB cable, 1 m (3 ft) long
043276 Ferrule fitting, 10-32 double-cone
043275 Fitting bolt, 10-32 (for double-cone ferrule fitting)
046985 Mini-screwdriver

440 Doc. 065342-06 12/11


ICS-5000
DC DC Reordering Information

Part Number Item


Valves and Accessories
074525 High-pressure (injection), 4-port
061961 High-pressure (injection or switching valve), 6-port
061962 High-pressure (injection or switching valve), 10-port
061971 Low-pressure valve, 3-way
061745 Low-pressure valve, 2-way
042949 Sample loop, 10 L
042857 Sample loop, 25 L
044105 Filter, high-pressure inline (for sample filtering)
024305 Luer adapter fitting, 1/4-28 (for manual injections)
016388 Syringe, 1 cc (for manual injections)
074698 Valve rebuild kit, 4-port
057896 Valve rebuild kit, 6-port
061759 Valve rebuild kit, 10-port
IC Cube and Accessories for Capillary IC
072000 Dionex IC Cube
072186 IC Cube tubing kit (includes precision cut tubing for
column connections)
074459 EG degas cartridge (capillary). Can be used with system
pressures up to 35 MPa (5000 psi).
072052 ACES 300 Anion Capillary Electrolytic Suppressor
072053 CCES 300 Cation Capillary Electrolytic Suppressor
072055 Suppressor bypass cartridge
072054 CRD 200 Carbonate Removal Device (Capillary)
072056 CRD bypass cartridge

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Dionex ICS-5000 Operator’s Manual

Part Number Item


Conductivity Detector for Capillary IC
072041 Dionex ICS-5000 Conductivity Detector (Capillary)
Conductivity Detector and Accessories for Analytical IC
061716 Dionex ICS-5000 Conductivity Detector (Analytical)
056116 AAES Anion Atlas Electrolytic Suppressor
056118 CAES Cation Atlas Electrolytic Suppressor
064555 ASRS 300 2 mm Anion Self-Regenerating Suppressor
064556 CSRS 300 4 mm Cation Self-Regenerating Suppressor
064557 CSRS 300 2 mm Cation Self-Regenerating Suppressor
045460 Suppressor gas separator waste tube
045877 Backpressure coil for 4 mm suppressor
045878 Backpressure coil for 2 mm suppressor
Electrochemical Detector and Accessories for Capillary and Analytical IC
072042 Dionex ICS-5000 Electrochemical Detector (ED) (without
cell)
072044 ED cell
061879 pH-Ag/AgCl reference electrode
014067 O-ring for pH-Ag/AgCl reference electrode (for analytical)
072162 Gasket for pH-Ag/AgCl reference electrode (for capillary)
072075 PdH reference electrode
072214 Gasket for PdH reference electrode
061749 ED gold conventional working electrode, with gasket and
polishing kit
061751 ED platinum conventional working electrode, with gasket
and polishing kit
061753 ED glassy carbon conventional working electrode, with
gasket and polishing kit
061755 ED silver conventional working electrode, with gasket and
polishing kit
045972 Gasket, PTFE, 0.001 in (for conventional working
electrode)

442 Doc. 065342-06 12/11


B • DC Reordering Information

Part Number Item


063722 ED AAA gold working electrode, with gasket and polishing
kit
060082 Gold AAA-Direct disposable working electrodes
(6 electrodes, with 2 gaskets)
060139 Gold carbohydrate disposable working electrodes
(polyester substrate) (6 electrodes, with 2 gaskets)
066480 Gold carbohydrate disposable working electrodes (PTFE
substrate) (6 electrodes, with 2 gaskets)
064440 Platinum disposable working electrodes
(6 electrodes, with 2 gaskets)
063003 Silver disposable working electrodes
(6 electrodes, with 2 gaskets)
069336 Carbon disposable working electrodes
(6 electrodes, with 2 gaskets)
060141 Gaskets for disposable working electrodes, PTFE,
0.002-in (4 gaskets) (for analytical systems)
069339 Gasket for carbon disposable working electrodes, ULTEM,
0.001-in (for analytical systems)
072117 Gasket for disposable working electrodes, PTFE, 0.001 in
(2 gaskets) (for capillary systems)
062158 ED cell polypropylene support block (for use with
disposable electrodes)
036313 Polishing kit
036319 Coarse polishing compound
036318 Fine polishing compound
036321 Polishing pads
Automation Manager
061738 Dionex ICS-5000 Automation Manager, two 10-port high-
pressure valves, two low-pressure 3-way valves
061736 Dionex ICS-5000 Automation Manager, one 10-port high-
pressure valve, one low-pressure 3-way valve
061740 Dionex ICS-5000 Automation Manager, one 6-port high-
pressure valve, one low-pressure 3-way valve

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Dionex ICS-5000 Operator’s Manual

Part Number Item


061734 Dionex ICS-5000 Automation Manager, tray with no
valves
061746 RCH-1 Reaction Coil Heater
062561 Temperature stabilizer, standard bore, 0.25 mm (0.010 in)
ID
062562 Temperature stabilizer, microbore, 0.125 mm (0.005 in) ID
Analog Output/Relay/TTL
062201 I/O option
923686 Connector plug, 12-position
043598 Twisted pair of wires
Miscellaneous
954772 Fuse, IEC 60127-2 slow-blow; rated at 10 A, 250 V
960777 USB cable, 1.8 m (6 ft) long
062437 Leak sensor
043276 Ferrule fitting, 10-32 double-cone
043275 Fitting bolt, 10-32 (for double-cone ferrule fitting)
044105 Filter, high-pressure inline
Maintenance Kits
075040 0.4 L Internal Loop High-Pressure Valve Preventive
Maintenance Kit
075041 6-Port High-Pressure Valve Preventive Maintenance Kit
075042 10-Port High-Pressure Valve Preventive Maintenance Kit

444 Doc. 065342-06 12/11


ICS-5000
DC TC Reordering Information

Part Number Item


Valves and Accessories
057896 Injection Valve Rebuild Kit for 6-port valve (includes valve
seal, hexagon wrench, and instructions)
061759 Injection Valve Rebuild Kit for 10-port valve (includes
valve seal, hexagon wrench, and instructions)
061961 Injection valve head (including seal) for 2-position, 6-port
valve
061962 Injection valve head (including seal) for 2-position, 10-port
valve
042857 Sample loop, 25 µL
Consumables
6710.1505 Column ID Kit (includes five column ID chip cards)
064786 Column Clips Kit (includes six column clips)
064548 Temperature stabilizer, standard bore, 0.25 mm (0.010 in)
ID
064650 Temperature stabilizer, microbore, 0.125 mm (0.005 in) ID
Miscellaneous
954776 Fuse, IEC 60127-2 time lag, rated at 2 A (two fuses
required)
063246 USB cable, 1 m (3 ft)
6000.1004 6-pin mini-DIN signal cable, 5 m (16.4 ft)
064792 TC/VWD/PDA Regulator Bracket Kit
Maintenance Kit
075041 6-Port High-Pressure Valve Preventive Maintenance Kit
075042 10-Port High-Pressure Valve Preventive Maintenance Kit

Doc. 065342-06 12/11 445


Dionex ICS-5000 Operator’s Manual

446 Doc. 065342-06 12/11


Index

Symbols Ag/AgCl half-cell, 77


Air bubbles (conductivity cell), 383
% Offset (analog out), 86 Air particulate samples, 147
+5V output (DC), 83, 87 Air pressure requirements, 146, 154
Alarm conditions
See Error messages
Numerics Alarm LED (DC), 51
10-port valve Alarm LED (DP/SP), 22
AM, 96 Alarm LED (EG), 256
DC, 65 – 67 LED is lighted, 253
TC, 123 Troubleshooting, 253
See also High-pressure valves Alarm LED (TC), 115
2D data Amperometry cell
Integrated amperometry, 107, 109 Cell design, 76
Pulsed amperometry, 109 Cell gasket replacement, 386
3D amperometry data, 111 – 113 Description, 75
3D plot description, 112 – 113 Electrodes, 75
Chromatogram, 111 Maintenance, 143
Definition, 110 Monitoring the pH readout, 78
Displayed in Chromeleon, 110 Operating precautions, 143
Isoamperometric plot description, 112 pH cannot be set to 7.0, 272
I-t plot, 111 pH limits, 145
3-way low-pressure valves Polishing the working electrode, 389
See Low-pressure valves Reordering, 442
4-port valve, 66 Solvent compatibility, 76
6-port valve Storage, 187
DC, 65, 96 Troubleshooting, 271
TC, 122, 124 Amperometry detection
See also High-pressure valves, Injection See Cyclic voltammetry
valves See DC amperometry
See Integrated amperometry
See Pulsed amperometry
Analog output, 85
A Connection instructions, 84
AAES, 71 Connectors, 82 – 83
AC sockets (DC), 81 Description, 85
ACES 300, 57 Full-scale, 86
ACES 300 (Capillary), 71 Mark, 86
Acetonitrile, 76

Doc. 065342-06 12/11 Index-1


Dionex ICS-5000 Operator’s Manual

Offset level, 86 Autorecycle mode, 73 – 74


Polarity, 86 Autosampler
Range, 85 Controlling with relays/TTLs, 87
Recorder calibration, 86 Filling vials, 146, 149
Selecting settings, 85 Injecting samples, 178
Analog pressure output, 32 Loading the tray, 146, 149
Analog-to-digital converter, 85 Sample loading, 178
Analytical IC applications Autozero, 167
Conductivity detector for, 69
CR-TC trap column for, 42
Eluent generator cartridges for, 41
Suppressors for, 71
B
System configurations, 129 Background conductivity
Annual maintenance High, 225
DC, 193, 200, 202, 444 – 445 Offsetting, 167
DP, 192, 196, 437 Backpressure coil (CD)
EG, 197 Reordering, 442
SP, 193, 196, 437 Requirements, 384
TC, 202 Backpressure coil (EG), 43, 47
Application Wizard, 174, 176 Installation, 355
Applications, 129 – 139 Reordering, 439
AS Autosampler, 3, 9 Backpressure, excessive
Example program/instrument method, Causes of, 223
182 Problems caused by, 141
Needle seal assembly, 359, 362 Backpressure, low
AS-AP Autosampler, 8 Causes of, 223
Example program/instrument method, How to increase, 43, 141, 215
181 Problems caused by, 215
AS-DV Autosampler Baseline
Example program/instrument method, Noisy or drifting, 215
181 Oscillations, 383
ASRS 300, 71 Shift, 104
Atlas Electrolytic Suppressor (AES), 62 Spikes, 217
Gas separator waste tube, 72 Stability, 69
Audit Trail, 22, 37 Bottles
Error messages, 203 See Reservoirs, eluent
Icons, 203 Bromate
Automation Manager (AM), 3, 94 Post-column reagent addition, 139
Description, 8, 94 Bubbles
High-pressure valves, 96 Removing from the cell, 383
Low-pressure valves, 97 Bulkhead connectors (EG), 44
Ordering, 443
RCH-1 Reaction Coil Heater, 101

Index-2 Doc. 065342-06 12/11


Index

Button descriptions Pulsed amperometry example, 109


DC, 51 Water dip in, 148
DP/SP, 21 – 22 Chromeleon, 11
EG, 37 Alarm conditions, 259, 275
TC, 115 Application Wizard, 174, 176
Audit Trail, 22, 37, 203
Audit Trail error messages, 203
C Commands dialog box, 26, 126, 156
Connected LED, 51
Cables Controlling external valves, 82
Power cord, 357, 370 – 371, 413 Controlling high-pressure valves, 98
Signal cable, 6-pin mini-DIN, 121, 445 Controlling low-pressure valves, 98
USB, 33, 46, 437, 440, 444 – 445 Controlling power, relays, and TTL
CAES, 71 outputs, 89
Calibration Controlling switched AC sockets, 81
CD cell, 379, 381 Creating a sequence, 174
pH-Ag/AgCl reference electrode, 394 ePanel Set, 11, 149, 171
Recorder (analog) output, 86 Home panel, 11
Capillary IC applications, 2 Installation manual, 14
Conductivity detector for, 69 Instrument method, 172
CR-TC trap column for, 42 Panel tabset, 11, 151, 171
DC components for, 54 Processing method, 174
Eluent generator cartridges for, 41 Programs, 172
Injection valves for, 65 Programs/Instrument methods, 178, 180
Replacing capillary columns, 374 – 379 Quantification method, 176
Suppressors for, 71 Sequence Wizard, 174 – 175
System configurations, 129 Starting, 149 – 151
Tube fitting installation, 303 – 304 Troubleshooting communication
Tubing and fittings (DC), 359 problems, 256
Carbohydrate analysis, 140 USB connections (DC), 81
Carbonate mixer, 43 USB connections (DP/SP), 33
Carbonate/bicarbonate eluent, 41, 43, 164 USB connections (EG), 45
CCES 300, 57 USB connections (TC), 121
CCES 300 (Capillary), 71 User’s guide, 14
CD cell disconnected error, 259 Virtual Column Separation Simulator,
CD cell over safe temperature, 260 172, 176
CE mark, 19 Chromeleon Instrument Configuration, 84,
cETLus mark, 19 408
Check valve cartridges Assigning TTL input functions, 90
Replacement procedure, 312 Chromeleon Server Configuration, 84, 408
Chromatogram Assigning TTL input functions, 90
Amperometry data, 111 Cinch connector
Dips instead of peaks, 86 Pin assignments, 32

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Dionex ICS-5000 Operator’s Manual

CMMS, 71 Connected LED (DC)


Column clips LED is lighted, 51
Reordering, 445 Connected LED (DP/SP)
Column ID chip card, 118, 125 LED is lighted, 22
Reordering, 445 Connected LED (EG)
Slots for installation, 118 LED is lighted, 37, 115
Column ID system, 125 Connected LED (TC)
Chip card readers, 118 LED is lighted, 115
Installing a chip card, 409 Counter electrode, 75 – 76
Selecting a column, 408 CRD bypass cartridge (for IC Cube), 56
Selecting column properties, 409 CRD cartridge (for IC Cube), 56
Column open circuit, 260 CR-TC trap column, 5, 42
Column over safe temperature, 260, 266 Contamination, 225
Column properties Hydration procedure, 351
Primary, 125, 290, 295 Replacement procedure, 349 – 354
Secondary, 125 CSRS 300, 71
Selecting for column ID system, 409 Cyclic voltammetry, 105
Columns Data collection rate, 105
Sizes available, 62 Example, 106
Commands Sweep rate, 106
AS Autosampler control, 182 Triangle waveform, 106
AS-AP Autosampler control, 181 Waveforms, 105, 107
AS-DV Autosampler control, 181
Creating a program, 172
Commands dialog box, 26, 126, 156
Compartment open circuit, 261
D
Compartment over safe temperature, 261 Daily maintenance
Concentrator column, 68, 123 DC, 199
Condensation, 199 DP/SP, 195
Conductivity Detector (CD), 3, 7 EG, 197
Air bubble removal, 383 TC, 201
Analytical IC system version, 69 Data
Capillary IC system version, 69 Displaying 3D amperometry data, 110
Cell calibration, 379 Reprocessing amperometry data, 109
Cell description, 69 Data collection rate
Cell temperature control, 69 Cyclic voltammetry, 105
Description, 69 Electrochemical detector, 110
Effect of temperature on conductivity, 69 Integrated amperometry, 107
Leaking, 270 Data compression
Replacement procedure, 382 Cyclic voltammetry, 105
Specifications, 427 DC amperometry, 102
Temperature compensation, 70 Entering the potential, 102
Configuration drawings, 129 – 139 DC Temperature Calibration Kit, 64

Index-4 Doc. 065342-06 12/11


Index

Declaration of Conformity, 19 Pressure limit tripped, 223, 255 – 256


Degassing eluents, 25 Pressure limits for EG, 158
Deionized water requirements, 20 Priming procedures, 308 – 311
Detector Priming valve knob seal replacement, 329
See Conductivity Detector (CD) Product warranty, 303
See Electrochemical Detector (ED) Pulse damper (for capillary pump), 27
Detector output Selecting pressure limits, 158
Low, 224 Shutdown procedure, 183
Detector/Chromatography Module (DC), 2, 7 Spare parts, 435
Alarm LED is lighted, 51 Specifications, 415
Automation Manager (AM), 94 Start-up procedures, 153
Electrochemical Detector (ED), 75 Static mixer, 27
Flow schematics, 73 – 74 Status bar buttons and LEDs, 21
Front description, 51 System configurations, 129, 137
I/O option, 83 USB connections, 33
Maintenance, 199 Waste lines, 33
Rebuilding the injection valve, 366 Dual system configuration, 132, 135 – 136
Service procedures, 359
Spare parts, 441
Specifications, 423
System configuration, 129
E
Temperature control, 63 EC cell
Disposable working electrodes, 75 See Amperometry cell
Reordering, 443 ED cell
Drain port See Amperometry cell
TC, 121 ED cell disconnected error, 261 – 264
Drifting baseline, 215 EGC
Dual Pump (DP), 2 – 3 See Eluent generator cartridges
Analog pressure output, 32 Electrochemical detection
Digital I/O port, 31 DC amperometry, 102
Fuse replacement, 330 Integrated amperometry, 103
Fuses, 31 Pulsed amperometry, 103
Maintenance, annual, 196 Electrochemical Detector (ED), 3, 7, 75, 429
Maintenance, daily, 195 3D data, 111 – 113
Maintenance, periodic, 196 Amperometric cell description, 75
Maintenance, weekly, 195 Data storage, 109
Operating humidity, 417 Description, 61, 75
Operating temperature, 417 Detection modes, 75, 102
Piston replacement procedure, 323 Palladium hydrogen (PdH) reference
Piston seal replacement procedure, 316 – electrode, 79
321, 323 – 324 pH-Ag/AgCl reference electrode, 77
Piston seal wash tubing replacement Reordering information, 442
procedure, 326 Replacement procedure, 404

Doc. 065342-06 12/11 Index-5


Dionex ICS-5000 Operator’s Manual

Shutdown procedure, 187 Waste lines, 46 – 47


Working electrodes, 75 Eluent generator cartridges, 41
See also Amperometry cell Backpressure requirement, 43, 141 – 142,
Electrodes, 76 255 – 256
Reference, 75 Conditioning procedure, 186
Working, 75 Electrical connections, 44
Electrolysis gases Frit, outlet, 223, 336
Purging from eluent, 43, 58, 141 Leaks, 223, 253 – 254
Venting from system, 46 Replacement procedure, 336 – 349
Eluemt generator cartridges, 5 Selecting the eluent concentration, 161
Eluent concentration, 161 – 163 Start-up procedures, 186
Eluent generation Storage, long-term, 186
Electrolysis gases, 43, 58 Storage, short-term, 185
Eluent Generator (EG), 2, 5 Eluent Organizer (EO), 2, 6, 34
Alarm LED is lighted, 253, 256 Eluent proportioning valves, 25
Analytical IC systems, 40 Eluent reservoirs
Backpressure, 43 See Reservoirs, eluent
Backpressure coil, 215 Eluent, filtering, 36
Capillary IC system, 39 Eluents
Component description, 38, 41 – 43 Aqueous, 196
Degas cartridge (for IC Cube), 58 Degassing, 25
Electrical connections (consumables), 44 Filtering, 153
Eluent concentration ranges, 161 – 163 Flushing lines after eluent change, 218
Eluent generator cartridges, 5 Monitoring pH, 77
Fuse cartridge, 46 Outgassing, 383
Fuses, 46 End-line filter
Gas vent line, 46 See Filter, end-line
Leak sensor, 43, 252 EO Regulator Kit, 35
Liquid flow path, 47 – 49 ePanel Set, 11, 149, 171
Liquid leaks, 253 – 254 EPM III Electrolytic pH Modifier, 41, 43 –
Main power switch, 46 44, 252
Maintenance, 197 Equilibration, 166, 170
Operating precautions, 141 Error messages
Power LED does not light, 254 Audit Trail description, 203
Pump pressure limits, 256 DC summary, 207
Rear panel description, 45 – 46 DP/SP summary, 204
Selecting the eluent concentration, 161 EG summary, 205
Shutdown procedures, 185 TC summary, 209
Spare parts, 439 Error messages (DC), 259 – 269
Specifications, 419 CD cell disconnected, 259
Status bar buttons and LEDs, 37 CD cell over safe temperature, 260
System configuration, 129 Column open circuit, 260
USB connections, 45 Column over safe temperature, 260, 266

Index-6 Doc. 065342-06 12/11


Index

Compartment open circuit, 261 EG invalid flow, 246


Compartment over safe temperature, 261 EG invalid flow rate-concentration, 246
ED cell disconnected, 261 – 264 EG over current, 247
High-pressure valve error, 265 EG over power, 248
Lower leak sensor wet, 267 EG over voltage, 248 – 249
Reaction coil open circuit, 267 Leak sensor wet, 252
Reaction coil over safe temperature, 268 Error messages (TC)
Suppressor over current, 268 AcqOff with previous AcqOn, 275
Suppressor over power, 268 Acquisition still on at program end, 275
Suppressor over voltage, 269 All samples must specify same value, 275
Upper leak sensor wet, 269 Can’t execute Disconnect command, 276
Error messages (DP/SP), 227 – 234 Can’t execute Standby command, 276
Abnormal drive current, 227 Can’t find TC3000.HEX image, 276
Camshaft index too early, 228 Can’t start acquisition, 277
Camshaft index too late, 228 Can’t start TC firmware, 277
Camshaft sensor always alight, 228 Can’t use device x, 278
Degasser malfunction, 228 Card data checksum error, 279
Excessive drive current, 229 Command unavailable in demo mode,
Function cannot be adjusted by user, 234 279
Invalid flow value, 229 Communication error, 279
Leak detected, 229 Communication interface is closed, 292
Maximum purge pressure exceeded, 232 Communication time-out, 280
Motor malfunction, 230 Compartment door is open, 293
Motor position error, 230 Configuration doesn’t match, 280
Pressure fallen below lower limit, 231 Configuration mismatch, 280
Pressure in working cylinder exceeded Counter x exceeded its limit, 293
safety limit, 233 Current flow out of limits, 280
Program with this name already exists, Current pressure out of limits, 281
227 Current temperature out of limits, 281
Pump block carryover pressure too high, Data buffer overrun, 281
230 Data format on chip card unsupported,
Relay 4 configured for inject 293
synchronization, 232 Device control feature not available, 282
System pressure exceeded safety limit, Device is not remote, 282
233 Device not found on USB, 283
Upper pressure limit exceeded, 234 Either the current date is . . ., 283
Error messages (EG), 241 – 253 Error deleting flash memory, 283
CR-TC mode is off for a virtual pump., Error during storing of card data, 284
243 Error finishing download, 277
CR-TC over current, 242 Error programming flash memory, 284
CR-TC stopped due to zero flow, 243 Executing this command will reset . . .,
EG cartridge disconnected, 244 284
EG invalid concentration, 245 Firmware download in progress, 285

Doc. 065342-06 12/11 Index-7


Dionex ICS-5000 Operator’s Manual

Gas leak detected, 285 Warning threshold must be lower . . ., 296


Humidity leak detected, 285 X position error, 298
Illegal parameter, 286 You do not have the privilege . . ., 298
Injections limit has been exceeded, 294 eWorkflows, 173
Injections limit will be exceeded, 294 External low-pressure valves (DC), 82
Invalid date/time format, 286 External Seal Wash Kit, 27, 154, 436
Invalid enumerated value, 286
Next qualification is due, 286
Next qualification is overdue, 287
Next qualification was due on . . ., 287
F
Next service is due in . . ., 287 Filter, end-line
Next service is overdue, 287 Bacterial contamination, 196
No chip card in reader, 288 Installation
No response from x, 288 Maintenance, 195
Nominal temperature must be set . . ., 294 Filter, inline, 36
Nominal temperature value out of range, Fittings (DC)
294 Replacing, 359
Operating columns above . . ., 289 Requirements, 359
Oven not fully operable, 294 Fittings (DP/SP)
Parameter x value exceeded . . ., 289 Replacing, 306
Primary column ID property . . ., 295 Requirements, 306
Primary property x already assigned, 290 Fittings (EG)
Properties cannot be changed, 290 – 291 Replacing, 333
Raw data file x cannot be created, 291 Requirements, 333
Raw data file x cannot be written, 291 Fittings (TC)
Starting data acquisition manually . . ., Replacing, 407
292 Requirements, 407
TC firmware download failed, 277 Flow restrictions, 196
TC is not remote, 282 Front description (DC)
The command can format . . ., 292 Buttons and LEDs, 51
There was already an AcqOff . . ., 296 Front description (DP/SP)
There was already an AcqOn . . ., 296 Buttons and LEDs, 21 – 22
This function cannot be adjusted, 297 Front description (EG)
This operation may affect . . ., 297 Buttons and LEDs, 37
Two AcqOn commands for channel, 296 Front description (TC)
Unknown error code, 297 LEDs, 115
Unknown format of card data, 297 Full-scale analog output, 86
Upper limit must be higher . . ., 295 Response range, 85
USB/LAN communication error, 283 Voltage output ranges, 85
Value for parameter is not within . . ., 289 Fuses (DC), 81
Value x replaced by . . ., 289 Replacement procedure, 371
Warning threshold must be higher . . ., Fuses (DP/SP), 30
296 Replacement procedure, 330

Index-8 Doc. 065342-06 12/11


Index

Fuses (EG), 46 For analytical IC system, 65


Replacement procedure, 357 For capillary IC system, 65
Fuses (TC), 119 High-pressure valves (TC), 117, 122
Replacement procedure, 413 Reordering, 445
Humidity leak in TC, 115, 126, 285
Humidity sensor, 126, 285
G Hybrid system configuration, 129, 132
Gas leak in TC, 115, 126, 285
Gas sensor, 126, 285
Gas separator waste tube, 72 I
Installation, 142 I/O option (DC), 82 – 83, 444
Reordering, 442 +5V output, 83
Gas vent line (EG), 46 Analog outputs, 83
Glassy carbon electrodes, 75 Connections, 84
GM-3 Gradient Mixer, 27, 219, 436 Power output, 87
GM-4 Gradient Mixer, 27, 219, 436 Relay outputs, 83
Gold electrodes, 75 TTL inputs and outputs, 83
Gradient proportioning valves, 25 IC Cube, 55
Cartridge replacement procedure, 372 –
373
H Column cartridge, 58
Column heater, 58
Half-cells, 77
CRD bypass cartridge, 56
Heater
CRD cartridge, 56
Conductivity cell, 69
EG degas cartridge, 58
Reaction coil, 101
Flow schematic for conductivity
High pressure limit
detection, 59
Limit is tripped, 233 – 234
Flow schematic for electrochemical
Selecting, 158 detection, 60
High-pressure fittings, 305 Suppressor bypass cartridge, 57
High-pressure inline filter, 36 Suppressor cartridge, 57
High-pressure valve error, 265 Tubing and fittings, 360
High-pressure valves (AM) ICS-5000 Automation Manager (AM)
Controlling, 98 See Automation Manager (AM)
Flow schematics, 96 ICS-5000 Conductivity Detector (CD)
Installed in AM, 94 See Conductivity Detector (CD)
Rebuilding, 366 ICS-5000 Detector/Chromatography Module
Reordering, 441 See Detector/Chromatography Module
Replacing, 367 (DC)
High-pressure valves (DC), 65 ICS-5000 Dual Pump (DP)
10-port valve, 68 See Dual Pump (DP)
4-port valve, 66 ICS-5000 Electrochemical Detector (ED)
6-port valve, 67

Doc. 065342-06 12/11 Index-9


Dionex ICS-5000 Operator’s Manual

See Electrochemical Detector (ED) Interior components (DC), 53


ICS-5000 Eluent Generator (EG) Analytical IC components, 61
See Eluent Generator (EG) Conductivity Detector (CD), 54, 61
ICS-5000 Eluent Organizer (EO) Electrochemical Detector (ED), 54, 61
See Eluent Organizer (EO) IC Cube, 55
ICS-5000 IC System Lower compartment description, 62
Overview, 1 – 2, 11 Suppressor types, 62
Software control, 11 Upper compartment description (for
User manuals, 14 – 15 analytical IC), 61
ICS-5000 Single Pump (SP) Upper compartment description (for
See Single Pump (SP) capillary IC), 54
ICS-5000 Thermal Compartment (TC) Inverted edge TTL input control (DC), 93
See Thermal Compartment (TC) Inverted pulse TTL input control (DC), 93
Injecting samples, 180 IonPac ATC-HC Trap Column, 42
Injection ports IonPac CTC-1 Trap Column, 42
Loading with a syringe, 179 IPAD
Injection valves (DC), 65 See Integrated amperometry
Flow schematics (10-port valve), 68 I-t plot, 111
Flow schematics (4-port valve), 66
Flow schematics (6-port valve), 67
Leaking, 270
Operation, 65 – 68
L
Rebuilding, 366 Leak sensor (EG), 43, 252
Reordering, 441 Leak sensors (DC)
Replacing mechanical parts (Pod), 367 Lower leak sensor wet alarm, 267
Types available, 62 Replacement, 364
Injection valves (TC), 122 Upper leak sensor wet alarm, 269
Flow schematics (10-port valve), 123 Leak sensors (TC)
Flow schematics (6-port valve), 122 Gas, 126, 285
Leaking, 300 Humidity, 126, 285
Operation, 122 – 123 Leaks
Plumbing (6-port valve), 124 Conductivity cell, 270
Rebuilding, 366, 410 DC, 270
Replacing mechanical parts (pod), 411 EG, 43, 252
Types available, 117 Gas, 115, 126, 285, 299
Inline filter, 36 Humidity, 115, 126, 285, 299
Instrument method (Chromeleon), 172 Injection valve (DC), 270
Integrated amperometry, 103 Injection valve (TC), 300
3D data, 109 Reference electrode, 274
Data storage, 109 Suppressor, 270
Integration interval, 104, 107 Temperature stabilizer (TC), 300
Waveform characteristics, 107 LED descriptions (DC), 51, 115
Waveform example, 104 LED descriptions (DP/SP), 21 – 22

Index-10 Doc. 065342-06 12/11


Index

LED descriptions (EG), 37 DC, 199, 201


LED descriptions (TC), 115 DP/SP, 195
Lithium hydroxide eluent, 41 EG, 197
Loading samples, 178 TC, 201
With a syringe, 178 Maintenance, periodic
With a vacuum syringe, 179 DP/SP, 196
With an autosampler, 178 TC, 201
Loading the autosampler tray, 146, 149 Maintenance, weekly
Low detector output, 224 DC, 199
Low pressure limit DP/SP, 195
Selecting, 158 EG, 197
Lower compartment (DC) TC, 201
Description, 62 Manuals for ICS-5000 system, 14 – 15
Lower oven LED, 51 Mark (analog output), 86
Low-pressure valves, 82 Matrix elimination, 61, 94
Controlling, 98 System configuration, 137 – 138
External valve outputs (DC), 82 Methanesulfonic acid eluent, 41
Flow schematic, 97 Methanol, 76
Installed in AM, 94 Microbore IC applications, 2
Reordering, 441 MicroMembrane Suppressor (MMS), 62, 71
Luer adapter fitting See also Suppressor
Reordering, 441 Mixer, static, 27
Mobile phases
See Eluents
M Moduleware, 203
MSQ Plus Mass Spectrometer, 3, 10
Main power receptacle
DC, 81
DP/SP, 30
EG, 46 N
TC, 119 Needle seal assembly (AS), 359, 362
Main power switch Nitrite in samples, 147
DC, 81 Noisy baseline, 215
DP/SP, 30 Normal edge TTL input control (DC), 93
EG, 46 Normal pulse TTL input control (DC), 93
TC, 119
Maintenance, annual
DC, 200
DP, 196
O
EG, 197 Offset percentage (analog out), 86
SP, 196 Offsetting background conductivity, 167
TC, 202 Open circuit, 267
Maintenance, daily Operating temperature
DP/SP, 417

Doc. 065342-06 12/11 Index-11


Dionex ICS-5000 Operator’s Manual

Operation pH half-cell, 77
Analyzing samples, 172 pH limits, 145
Creating a sequence, 173 – 174 pH modifier, 43
Direct control of modules, 171 pH reading
Filling vials, 146, 149 Adjusting potentials for, 77
Loading samples, 178 Always 7.0, 271
Overview, 172 Cannot be set to 7.0, 272
Sample preparation, 147 Effect on potentials, 77
Starting a sequence, 176 – 177 Monitoring, 78
Organic solvent, 77 Nonexistent, 273
Oven (TC), 116 pH-Ag/AgCl reference electrode, 75, 77
See also Temperature control (TC) Long-term storage, 187
Oven LED (TC) O-ring replacement procedure, 399
LED is flashing, 116, 300 Replacement procedure, 392
LED is lighted, 116 See also Reference electrode
Oven LEDs (DC) Photodiode Array Detector, 3, 9
LED is flashing, 51 Regulator Bracket Kit, 35
LED is lighted, 51 Piston seal wash solution, 26, 183
Piston seal wash system, 26, 154
Activation, 26
P Dual pump seal wash option, 27, 154, 436
Replumbing the DP connections, 154
PAD Setup, 156
See Pulsed amperometry Piston seals
Palladium hydrogen (PdH) reference Replacement procedure, 316
electrode, 79 Pistons
Replacement procedure, 400 Replacement procedure, 323
Panel tabset, 11 Platinum working electrodes, 75
Home panel, 11, 149, 151 Plot, I-t, 111
How to display, 157, 165, 169, 255 – 256 Plumbing
Parameters Replacing DC tubing and fittings, 359
Chromeleon commands, 172 Replacing DP/SP tubing and fittings, 306
Peak height Replacing EG tubing and fittings, 333
Reproducibility, 69 Replacing TC tubing and fittings, 407
Peaks Plumbing configuration drawings, 129 – 139
Fronting, 118 Polarity
Reversed, 86 Analog output, 86
Tailing, 118, 222 Polishing kit (ED)
Periodic maintenance Reordering, 443
DC, 199 Polishing working electrodes, 389
DP/SP, 196 Post-column reagent addition, 61, 94, 139
TC, 201 Potassium carbonate eluent, 41, 43
pH gradient, 77 Potassium hydroxide eluent, 41

Index-12 Doc. 065342-06 12/11


Index

Potential shifting, 77, 274 Leaks, 237


Power cord, 357, 370 – 371, 413 Malfunction, 218, 220
Power LED (DC), 52 Pulse damper (for capillary pump), 27
Power LED (DP/SP), 22 Pulsed amperometry, 103
Power LED (EG), 38 3D data, 109
Power LED (TC), 116 Chromatogram example, 110
Power output (DC) Data storage, 109
I/O option, 82 – 83, 87 Integration interval, 103
Power receptacle Waveform example, 103
DC, 81 See also Integrated amperometry
DP/SP, 30 Pump
EG, 46 See Dual Pump (DP), Single Pump (SP)
TC, 119
Power switch (rear panel)
DC, 81
DP/SP, 30
Q
EG, 46 Quantification method, 176
TC, 119
Pre-concentration, 61, 94
Predictive Performance, 128 R
Pressure limit settings, 158 Raw data, 110
Pressure limits tripped, 223 RCH-1 Reaction Coil Heater, 101
Pressure transducer, 25 Controlling, 101
Pressurizable eluent reservoirs Installed in AM, 94
Installation, 35 Open circuit error, 267
Priming procedures (DP/SP), 308 – 309 Over safe temperature, 268
From the Control panel, 310 Reordering, 444
Priming with a syringe, 310 – 311 Reagent-Free IC (RFIC), 1
Priming with the Prime button, 310 – 311 System configurations, 129 – 140
With the Prime button, 310 Rear panel (DC), 82
Priming valve AC sockets, 81
Leakage from knob, 238 Analog outputs, 82
Seal knob replacement procedure, 329 Description, 80
Problems Fuses, 81
See Troubleshooting I/O option, 82, 444
Processing samples, 172 Power switch, 81
Product warranty, voiding, 303 TTL and relay connectors, 82
Program Wizard USB connections, 81
Waveforms, 108 Rear panel (DP/SP)
Programs (Chromeleon) Analog pressure output, 32
Autosampler control, 178, 180 Digital I/O port, 31
Creating programs, 172 Fuses, 31
Proportioning valves, 25 Power receptacle, 31

Doc. 065342-06 12/11 Index-13


Dionex ICS-5000 Operator’s Manual

Power switch, 30 Reprocessing amperometry data, 109


USB connections, 33 Reproducibility
Waste lines, 33 Affected by amperometry cell pH, 78
Rear panel (EG), 45 Affected by temperature changes, 70
Exhaust fan, 45 Reproducibility is poor, 218
Fuse cartridge, 46 Reservoirs, eluent, 34
Gas vent line, 46 – 47 Cleaning, 214, 219, 308
Power switch, 46 Installation in EO, 6, 34 – 35
USB connections, 45 Pressurizing, 34
Waste lines, 46 – 47 Retention time
Rear panel (TC) Troubleshooting, 220
Description, 119 Variations, 118
Digital I/O connectors, 120 Reversed-phase solvents, 76
Fuses, 119 RFIC Eluent Degasser, 43, 47
Power switch, 119 Leaks, 253 – 254
USB connections, 121 Pressure requirements, 141
Waste line, 121 Replacement procedure, 355
Rear-seal wash Tubing rupture, 141, 223, 255
See Piston seal wash system RFIC-ER, 6
Recorder RFIC-ESP, 6
Analog output setting, 86 Running samples, 172
Calibrating, 86 See also Sample processing
Recycle mode, 73
Redox reactions, 77
Reference electrode, 75
Contaminated, 272
S
Faulty, 274 Safety icons, 35
Leaking, 274 Safety messages, 16, 35
Preventing from drying out, 78 Salt crystals, preventing, 197
Reordering information, 442 Sample analysis overview, 172
Shutdown procedure, 187 Sample loading
Reference potential shift, 78, 274 With a syringe, 179
Regulator Bracket Kit, TC/VWD/PDA, 35 With an autosampler, 178
Regulator Kit, EO, 35 Sample loop (DC)
Relay connectors (DC), 82 – 84 Injecting, 66 – 67, 69
Configuring, 87 Loading, 68, 178 – 179
Relay outputs (DC), 82 Reordering, 441
Controlling, 89 Sample loop (TC)
Reordering information Injecting, 123
DC, 441 Injection valve connections, 124
DP/SP, 435 Loading, 122 – 123
EG, 439 Reordering, 445
TC, 445 Sample processing, 172

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Index

Sample tray Check valve cartridge replacement, 312


Loading, 146, 149 Eluent reservoir cleaning, 308
See Tray Fuse replacement, 330
Samples Piston replacement, 323
Collecting and storing, 147 Piston seal replacement, 316 – 321, 323 –
Diluting, 148 324
Filtering, 147 Piston seal wash tubing replacement, 326
Loading, 178 – 179 Priming, 310 – 311
Pretreating, 147 Priming valve knob seal replacement, 329
See also High-pressure valves, Injection Service procedures (EG)
valves CR-TC replacement, 349 – 354
Self-Regenerating Suppressor (SRS), 47, 62 Eluent generator cartridge replacement,
Gas separator waste tube, 72 336 – 349
Hydrating, 185 – 186 Fuse replacement, 357
Start-up procedure, 185 – 186 Service procedures (TC)
See also Suppressor Column ID system setup, 408 – 409
Sensor, gas, 115, 126, 285 Fuse replacement, 413
Sensor, humidity, 115, 126, 285 Injection valve pod replacement, 411
Sequence Wizard, 173 – 176 Injection valve rebuilding, 410
Service procedures (DC) Tubing and fittings replacement, 407
Amperometry cell gasket replacement, Shift in reference potential, 274
386 Ship Kit (DC), 81
Capillary column replacement, 374 Ship Kit (DP/SP, 33
CD cell air removal, 383 Ship Kit (EG), 46
CD cell calibration, 379 Ship Kit (TC), 121
Conductivity detector replacement, 382 Shutdown
Electrochemical detector replacement, DC, 187
404 DP/SP, 183
Fuse replacement, 371 EG, 185
IC Cube cartridge replacement, 372 TC, 189
Injection valve Pod replacement, 367 Silver electrodes, 75
Injection valve rebuilding, 366, 410 Single Pump (SP), 2 – 3
Leak sensor replacement, 364 Analog pressure output, 32
PdH reference electrode replacement, 400 Digital I/O port, 31
pH-Ag/AgCl reference electrode O-ring Fuse replacement procedure, 330
replacement, 399 Fuses, 31
pH-Ag/AgCl reference electrode Maintenance, annual, 196
replacement, 392 Maintenance, daily, 195
Replacing capillary columns, 375 – 379 Maintenance, periodic, 196
Suppressor replacement, 381 Maintenance, weekly, 195
Tubing and fittings replacement, 359 Operating humidity, 417
Working electrode polishing, 389 Operating temperature, 417
Service procedures (DP/SP) Piston replacement procedure, 323

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Dionex ICS-5000 Operator’s Manual

Piston seal replacement procedure, 316 – Static mixer, 219


321, 323 – 324 See also GM-3 Gradient Mixer
Piston seal wash tubing replacement Status bar (DC), 51
procedure, 326 LEDs described, 51, 115
Pressure limit tripped, 223, 255 – 256 Status bar (DP/SP)
Pressure limits for EG, 158 LEDs described, 22
Priming procedures, 308 – 311 Status bar (EG)
Priming valve knob seal replacement LEDs described, 38
procedure, 329 Status bar (TC)
Product warranty, 303 LEDs described, 115
Pulse damper (for capillary pump), 27 Sulfite in samples, 147
Selecting pressure limits, 158 Suppressor
Shutdown procedure, 183 Description, 71
Spare parts, 435 For analytical IC system, 71
Specifications, 415 For capillary IC system, 71
Start-up procedures, 153 Leaking, 270
Static mixer, 27 Reordering, 442
Status bar buttons and LEDs, 21 Replacement procedure, 381
System configurations, 129, 138 Types supported, 62
USB connections, 33 Suppressor alarms
Waste lines, 33 Suppressor over current, 268
Sodium hydroxide eluent, 41 Suppressor over power, 268
Solvent compatibility (ED), 76 Suppressor over voltage, 269
Spare parts Suppressor bypass cartridge (for IC Cube), 57
DC, 441 Suppressor cartridge (for IC Cube), 57
DP/SP, 435 Suppressor LEDs (DC)
EG, 439 LED is lighted, 51
TC, 445 Switched AC sockets (DC), 81
Specifications Syringe
Conductivity Detector (CD), 427 Reordering, 441
DC, 423 Syringe injection, 178
DP/SP, 415 Vacuum, 179
EG, 419 System configuration drawings, 129 – 139
Electrochemical Detector (ED), 429 Analytical IC RFIC-EG dual CD and ED
TC, 433 system, 136
Standard bore IC applications, 2 Analytical IC RFIC-EG dual CD system,
Start-up procedures 135
DC, 165 Analytical IC RFIC-EG single system,
DP/SP, 153 134
EG, 161 Analytical IC system (non-RFIC), 133
Equilibrate the system, 166, 170 Analytical RFIC-EG with post-column
Offsetting the background, 167 reagent addition, 139 – 140
TC, 169

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Index

Capillary IC RFIC-EG dual CD and EG Triangle waveform, 106


system, 131 Troubleshooting (DC)
Capillary IC RFIC-EG dual CD system, Alarm conditions (DC), 259
130 Amperometry cell, 271
Hybrid RFIC-EG dual CD analytical and Error messages (DC), 259
CD capillary system, 132 Liquid leaks (DC), 270
Matrix elimination, 137 – 138 pH readout always at 7.0, 271
System Wellness, 128 pH readout cannot be set to 7.0, 272
pH readout nonexistent, 273
Reference electrode leaks, 274
T Reference potential shifts, 274
VALVE button not working, 271
TC/VWD/PDA Regulator Bracket Kit, 35 Troubleshooting (DP/SP)
Temperature calibration (DC), 64 Chromatographic reproducibility, 218
Temperature control (CD), 69 Digital I/O port not operating, 239
Minimizing the effect of variations, 70 Leak alarm, 237
Temperature compensation, 70 Liquid leaks, 237
Temperature control (DC), 63 Pump does not start, 235
Cell heater, 70 Pump stops unexpectedly, 236
Temperature control (TC), 118, 127 Vacuum degassing module low vacuum,
Temperature stabilizer (TC), 8, 118 238
Liquid leaks, 300 Troubleshooting (EG)
Operating problem, 301 Alarm LED is lighted, 253
Thermal Compartment (TC), 3, 8 EG stops operation, 256
Alarm LED is lighted, 115 Error messages, 241
Digital I/O connectors, 120 Leaking fittings, 253
Front description, 115 Liquid leaks, 254
Maintenance, 201 – 202 No flow, 255
Moduleware update, 278 Power LED does not light, 254
Oven LED is flashing, 116 Troubleshooting (system-wide), 203
Oven LED is lighted, 116 High background, 225
Rebuilding the injection valve, 410 Low detector output, 224
Regulator Bracket Kit, 35 Noisy baseline, 215
Replacing the injection valve pod, 411 Retention times too early, 220
Service procedures, 407 Retention times too late, 220
Shutdown procedure, 189 Tailing peaks, 222
Signal cable, 121, 445 Troubleshooting (TC)
Specifications, 433 Alarm conditions (TC), 275
Theory of operation, 127 Alarm LED is lighted, 299
Trace analyses, 9 Liquid leaks, 300
Trap column, 5 Temperature does not increase, 301
Tray, autosampler Temperature stabilizer not operating, 301
Loading, 146, 149

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Dionex ICS-5000 Operator’s Manual

TTL and relay connectors (DC), 82 – 83 Vacuum is low, 238


Installation instructions, 84 VALVE buttons (DC), 52
TTL inputs (DC), 82 Enabling/disabling, 52
Control types, 92 Troubleshooting, 271
Functions available, 89 Valve LEDs (DC)
TTL outputs (DC), 82 LED is flashing, 52
Controlling, 87 LED is lighted, 52
TTL/Relay control Valve LEDs (TC)
DC Control panel, 87 LED is flashing, 115, 299
DC relay output configuration, 87 LED is lighted, 115
Operating failure, 239 Valves
Tubing See High-pressure valves, Injection
Replacing (DC), 359 valves, Low-pressure valves
Replacing (DP/SP), 306 Variable Wavelength Detector, 3, 10
Replacing (EG), 333 Regulator Bracket Kit, 35
Replacing (TC), 407 Vials, 146, 149
Filling, 146, 149
Virtual Column Separation Simulator, 172,
U 176
Voltammetry, 105
Upper compartment (DC) See also Cyclic voltammetry
Description, 61 VP Vacuum Pump, 140
Upper oven LED, 51
USB cables
DC, 81
DP/SP, 33 W
EG, 46 Waste container (EG)
Reordering (DC), 444 Preventing gas buildup, 142
Reordering (DP/SP), 437 Waste disposal, 201
Reordering (EG), 440 Waste lines (CD)
Reordering (TC), 445 Gas separator waste tube, 72
TC, 121 Waste lines (DC), 82
USB connections Blocked, 270
DC, 81 Waste lines (DP/SP), 33
DP/SP, 33 Waste lines (EG), 46 – 47
EG, 257 Blocked or incorrectly installed, 253 –
TC, 121 254
Waste lines (TC)
Blocked, 300
V Water dip, 148
Water samples, 147
Vacuum degassing module, 25 Waveform Editor, 108
Daily maintenance, 195
On/off control, 26

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Index

Waveforms, 105
Cyclic voltammetry, 105
Defining, 108
Integrated amperometry, 107
Integrated amperometry example, 104
Maximum length, 107
Pre-programmed, 108
Pulsed amperometry example, 103
Weekly maintenance
DC, 199
DP/SP, 195
EG, 197
TC, 201
Wellness, 128
Wireframe plot, 112
Working electrodes, 75
Maintenance, 143
Materials, 75
Polishing, 389

Z
Zero position (analog out), 86

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Dionex ICS-5000 Operator’s Manual

Index-20 Doc. 065342-06 12/11

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