Dionex ICS-3000 Operator's Manual

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ICS-3000 Ion Chromatography System

Operator's Manual

Document No. 065031

Revision 04

January 2008

This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transmitted, transcribed, stored in a retrieval system, or transmitted into any human or computer language, in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or disclosed to third parties without the express written permission of Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94088-3603 U.S.A.

DISCLAIMER OF WARRANTY AND LIMITED WARRANTY

THIS PUBLICATION IS PROVIDED “AS IS” WITHOUT WARRANTY OF ANY KIND. DIONEX CORPORATION DOES NOT WARRANT, GUARANTEE, OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE, OR THE RESULTS OF THE USE, OF THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY, RELIABILITY, CURRENTNESS, OR OTHERWISE. FURTHER, DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES.

TRADEMARKS

AES, Atlas, Chromeleon, EluGen, IonPac, OnGuard, and SRS are registered trademarks of Dionex Corporation. CarboPac, MicroMembrane, MMS, ReagentFree, and RFIC are trademarks of Dionex Corporation. Adobe, Adobe Reader, and Acrobat are registered trademarks of Adobe Systems, Incorporated. Kel-F is a registered trademark of 3M Corporation. FastLock and MSQ Plus are trademarks of Thermo Electron Corporation. PEEK is a trademark of Victrex PLC. PharMed and Tygon are registered trademarks of Saint-Gobain Performance Plastics. Teflon is a registered trademark of E.I. duPont de Nemours & Company. TitanHP is a trademark of Rheodyne LLC Ultem is a registered trademark of General Electric Company

PRINTING HISTORY

Revision 01, May 2005 Revision 02, July 2006 Revision 03, September 2006 Revision 04, January 2008

1 • Introduction

1.1 ICS-3000 System Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.1.1 ICS-3000 System Components . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.1.2 ICS-3000 System Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

1.2 ICS-3000 System Documentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

1.3 The ICS-3000 System Operator’s Manual . . . . . . . . . . . . . . . . . . . . . . 11

1.3.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

1.3.2 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

1.4.1 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2•Description

DP/SP Description

2.1 DP/SP Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

2.2 DP/SP Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

2.2.1 Pump Heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

2.2.2 Pressure Transducer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

2.2.3 Proportioning Valves (Gradient pump only) . . . . . . . . . . . . . . 20

2.2.4 Vacuum Degassing Module . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

2.2.5 Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

2.2.6 Static Mixer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

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ICS-3000 Ion Chromatography System

2.3 DP/SP Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23

2.3.1 Isocratic Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . . .23

2.3.2 Gradient Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . . .24

2.4 DP/SP Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25

2.5 Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29

2.6 EO (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30

EG Description

2.7 EG Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31

2.8 EG Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33

2.9 EG Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

2.10 EG Flow Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39

DC Description

2.11 DC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41

2.12 DC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .44

2.13 DC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47

2.14 Injection Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50

2.14.1 Injection Valve Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50

2.14.2 Injection Valve Plumbing . . . . . . . . . . . . . . . . . . . . . . . . . . . . .52

2.15 CD Conductivity Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .53

2.15.1 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . .53

2.15.2 Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55

2.15.3 System Flow Schematic for Conductivity Detection . . . . . . . .56

2.16 ED Electrochemical Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

2.16.1 Amperometry Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

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2.16.2 Combination pH–Ag/AgCl Reference Electrode . . . . . . . . . . . 58

2.16.3 DC Amperometric Detection . . . . . . . . . . . . . . . . . . . . . . . . . . 60

2.16.4 Integrated and Pulsed Amperometric Detection . . . . . . . . . . . 61

2.16.5 Cyclic Voltammetry Detection . . . . . . . . . . . . . . . . . . . . . . . . . 63

2.16.6 Waveforms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

2.16.7 Storing and Reprocessing Amperometry Data . . . . . . . . . . . . . 68

2.17 Automation Manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

2.17.1 High-Pressure Switching Valves . . . . . . . . . . . . . . . . . . . . . . . 74

2.17.2 Low-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

2.17.3 High- and Low-Pressure Valve Control . . . . . . . . . . . . . . . . . . 76

2.17.4 RCH-1 Reaction Coil Heater . . . . . . . . . . . . . . . . . . . . . . . . . . 78

2.18 I/O Option . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79

2.18.1 I/O Option Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

2.18.2 Analog Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81

2.18.3 Power, Relay, and TTL Outputs . . . . . . . . . . . . . . . . . . . . . . . . 84

2.18.4 TTL Inputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

TC Description

2.19 TC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

2.20 TC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

2.21 TC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

2.22 Injection Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

2.22.1 Injection Valve Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

2.22.2 Injection Valve Plumbing . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

2.23 Column Identification (ID) System . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

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ICS-3000 Ion Chromatography System

2.24 Gas and Humidity Sensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102

2.25 Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103

2.25.1 Predictive Performance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104

3 • Configurations

3.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105

4•Startup

4.1 Operating Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .113

4.1.1 EG Operating Precautions . . . . . . . . . . . . . . . . . . . . . . . . . . . .113

4.1.2 ED Amperometry Cell Operating Precautions . . . . . . . . . . . .115

4.2 System Startup Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .118

4.3 Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119

4.3.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . .119

4.3.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119

4.3.3 Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .120

4.3.4 Fill the Autosampler Vials and Load the Sample Tray . . . . . .120

DP/SP Startup

4.4 Set Up the Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123

4.5 Set Up the Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . . . . . .124

4.6 Start the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127

EG Startup

4.7 Setting the Eluent Concentration . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131

iv Doc. 065031-04 1/08

DC Startup

4.8 Start the DC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135

4.9 Equilibrate the System and Verify Operational Readiness . . . . . . . . . 136

TC Startup

4.10 Start the TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137

4.11 Equilibrate the System and Verify Operational Readiness . . . . . . . . . 138

5 • Operation

5.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

5.2 Loading Samples with an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . 140

5.3 Loading Samples with a Syringe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 140

5.3.1 Loading Samples with a Syringe (Push Method) . . . . . . . . . . 141

Contents

5.3.2 Loading Samples with a Vacuum Syringe (Pull Method) . . . 143

5.4 Example Commands for Loading and Injecting Samples . . . . . . . . . . 144

5.4.1 Commands for an AS Autosampler . . . . . . . . . . . . . . . . . . . . 144

5.4.2 Commands for an AS40 Autosampler . . . . . . . . . . . . . . . . . . 144

5.4.3 Commands for a Remote Inject Device . . . . . . . . . . . . . . . . . 145

5.5 Manual Sample Processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146

5.5.1 Saving Manual Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147

5.6 Automatic (Batch) Sample Processing . . . . . . . . . . . . . . . . . . . . . . . . 147

5.6.1 Creating a New Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148

5.6.2 Starting Batch Sample Processing . . . . . . . . . . . . . . . . . . . . . 149

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ICS-3000 Ion Chromatography System

6 • Shutdown

DP/SP Shutdown

EG Shutdown

6.1 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .153

6.2 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .153

DC Shutdown

6.3 Consumables Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .155

6.4 Amperometry Cell Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .155

6.4.1 Short-term Storage of the Amperometry Cell . . . . . . . . . . . . .155

6.4.2 Long-term Storage of the Amperometry Cell . . . . . . . . . . . . .155

TC Shutdown

6.5 Consumables Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157

6.6 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157

6.7 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157

7 • Maintenance

7.1 System Maintenance Checklists . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .159

7.1.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .159

7.1.2 Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .159

7.1.3 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .160

7.1.4 Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .160

DP/SP Routine Maintenance

7.2 DP/SP Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .161

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7.3 DP/SP Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161

7.4 DP/SP Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162

7.5 DP/SP Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 162

EG Routine Maintenance

7.6 EG Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163

7.7 EG Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163

7.8 EG Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163

DC Routine Maintenance

7.9 DC Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

7.10 DC Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

7.11 DC Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

7.12 DC Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 166

TC Routine Maintenance

7.13 TC Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167

7.14 TC Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167

7.15 TC Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 168

7.16 TC Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 168

8 • Troubleshooting

8.1 Audit Trail Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169

8.1.1 DP/SP Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170

8.1.2 EG Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171

8.1.3 DC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172

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8.1.4 TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .173

8.2 Noisy Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .178

8.3 Poor Retention Time Reproducibility . . . . . . . . . . . . . . . . . . . . . . . . . .181

8.4 Peak Retention Times Are Too Early . . . . . . . . . . . . . . . . . . . . . . . . . .183

8.5 Peak Retention Times Are Too Late . . . . . . . . . . . . . . . . . . . . . . . . . .183

8.6 No Peaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .183

8.7 Tailing Peaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .185

8.8 Low System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .185

8.9 High System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .186

8.10 Low Detector Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .186

8.11 High Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .187

DP/SP Troubleshooting

8.12 Troubleshooting DP/SP Error Messages . . . . . . . . . . . . . . . . . . . . . . .189

8.13 DP/SP Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .197

8.14 DP/SP Stops . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .198

8.15 DP/SP Liquid Leaks/Leak Alarm . . . . . . . . . . . . . . . . . . . . . . . . . . . . .199

8.16 Vacuum Degassing Module Low Vacuum . . . . . . . . . . . . . . . . . . . . . .201

8.17 Vacuum Degassing Module Does Not Run . . . . . . . . . . . . . . . . . . . . .201

8.18 DP/SP Digital I/O Port Inoperative . . . . . . . . . . . . . . . . . . . . . . . . . . .201

EG Troubleshooting

8.19 Troubleshooting EG Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . .203

8.20 EG ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .207

8.21 EG POWER LED Fails to Light . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .208

8.22 Liquid Leaks in the EG . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .208

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8.23 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 209

8.24 EG Stops Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 210

DC Troubleshooting

8.25 Troubleshooting DC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . 213

8.26 Liquid Leaks from DC Components . . . . . . . . . . . . . . . . . . . . . . . . . . 221

8.27 VALVE Button Not Working . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 222

8.28 Amperometry Cell Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . 223

8.28.1 Amperometry Cell pH Readout Always 7.0 . . . . . . . . . . . . . 223

8.28.2 Cannot Set Amperometry Cell pH Readout to 7.0 . . . . . . . . . 224

8.28.3 Shift in Amperometry Cell pH Readout . . . . . . . . . . . . . . . . . 224

8.28.4 No Amperometry Cell pH Readout or Intermittent Readout . 225

8.28.5 Leak in pH Reference Electrode Compartment . . . . . . . . . . . 225

8.28.6 Shift in Ag/AgCl Reference Potential . . . . . . . . . . . . . . . . . . 226

TC Troubleshooting

8.29 Troubleshooting TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . 227

8.30 TC ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 253

8.31 Liquid Leaks from TC Components . . . . . . . . . . . . . . . . . . . . . . . . . . 253

8.32 TC Temperature Does Not Increase . . . . . . . . . . . . . . . . . . . . . . . . . . 254

8.33 TC Temperature Stabilizer Not Operating Properly . . . . . . . . . . . . . . 255

9•Service

DP/SP Service

9.1 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257

9.2 Cleaning Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 258

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ICS-3000 Ion Chromatography System

9.3 Priming the DP/SP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .259

9.3.1 Priming with the

PUMP PRIME Button . . . . . . . . . . . . . . . . .259

9.3.2 Priming from the Control Panel . . . . . . . . . . . . . . . . . . . . . . .261

9.4 Replacing the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .262

9.5 Replacing a Piston Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .265

9.5.1 Removing the Pump Head and Piston . . . . . . . . . . . . . . . . . . .265

9.5.2 Cleaning the Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .268

9.5.3 Removing the Main Piston Seal . . . . . . . . . . . . . . . . . . . . . . .268

9.5.4 Removing the Piston Seal Wash Seal . . . . . . . . . . . . . . . . . . .269

9.5.5 Installing the Piston Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . .269

9.5.6 Reinstalling the Piston and Pump Head . . . . . . . . . . . . . . . . .270

9.6 Replacing the Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .271

9.6.1 Removing the Pump Head and Piston . . . . . . . . . . . . . . . . . . .271

9.6.2 Installing the New Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . .273

9.6.3 Reinstalling the Pump Head . . . . . . . . . . . . . . . . . . . . . . . . . .273

9.7 Replacing the Piston Seal Wash Tubing . . . . . . . . . . . . . . . . . . . . . . . .274

9.8 Replacing the DP/SP Priming Valve Knob Seal . . . . . . . . . . . . . . . . .276

9.9 Changing the DP/SP Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . .278

EG Service

9.10 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .281

9.11 Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . . .282

9.12 Replacing the EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .282

9.12.1 EG Flow Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .283

9.12.2 Removing the Old EluGen Cartridge . . . . . . . . . . . . . . . . . . .284

x Doc. 065031-04 1/08

Contents

9.12.3 Disposing of the Old EluGen Cartridge . . . . . . . . . . . . . . . . . 286

9.12.4 Installing the New EluGen Cartridge . . . . . . . . . . . . . . . . . . . 286

9.12.5 Conditioning the New EluGen Cartridge . . . . . . . . . . . . . . . . 288

9.12.6 Completing the EluGen Cartridge Installation . . . . . . . . . . . . 289

9.13 Replacing the CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 290

9.13.1 Removing the Old CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . 290

9.13.2 Installing and Hydrating the New CR-TC . . . . . . . . . . . . . . . 291

9.13.3 Completing the New CR-TC Plumbing . . . . . . . . . . . . . . . . . 292

9.14 Replacing the RFIC Eluent Degasser . . . . . . . . . . . . . . . . . . . . . . . . . 294

9.15 Installing a Backpressure Coil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 295

9.16 Changing the EG Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . 296

DC Service

9.17 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297

9.18 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 298

9.19 Rebuilding a High-Pressure (Injection) Valve . . . . . . . . . . . . . . . . . . 300

9.20 Replacing a High-Pressure (Injection) Valve Pod . . . . . . . . . . . . . . . . 302

9.21 Installing or Replacing an I/O Option Board . . . . . . . . . . . . . . . . . . . 305

9.22 Changing the DC Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . 307

9.23 CD Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 308

9.23.1 Calibrating the CD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 308

9.23.2 Replacing a Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309

9.23.3 Replacing a CD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 311

9.23.4 Removing Trapped Air from the Conductivity Cell . . . . . . . 312

9.24 ED Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 313

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ICS-3000 Ion Chromatography System

9.24.1 Disconnecting the Amperometry Cell . . . . . . . . . . . . . . . . . . .313

9.24.2 Replacing an Amperometry Cell Gasket . . . . . . . . . . . . . . . . .314

9.24.3 Polishing an Amperometry Cell Working Electrode . . . . . . . .317

9.24.4 Replacing an Amperometry Cell Reference Electrode . . . . . .320

9.24.5 Calibrating the Reference Electrode . . . . . . . . . . . . . . . . . . . .322

9.24.6 Replacing the Reference Electrode O-Ring . . . . . . . . . . . . . .324

9.24.7 Replacing an ED Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . .326

TC Service

9.25 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .327

9.26 Setting Up the Column ID System . . . . . . . . . . . . . . . . . . . . . . . . . . . .328

9.27 Rebuilding an Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .330

9.28 Replacing an Injection Valve Pod . . . . . . . . . . . . . . . . . . . . . . . . . . . .331

9.29 Changing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . .334

A • Specifications

DP/SP Specifications

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .335

A.2 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .335

A.3 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .335

A.4 Hydraulics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .336

A.5 Computer Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .337

A.6 I/O Interfaces and Inputs/Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . .337

EG Specifications

A.7 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .339

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Contents

A.8 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339

A.9 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339

A.10 EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 340

DC Specifications

A.11 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341

A.12 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341

A.13 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341

A.14 Lower Compartment Components . . . . . . . . . . . . . . . . . . . . . . . . . . . 342

A.15 Temperature Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 342

A.15.1 Upper Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 342

A.15.2 Lower Compartment (Optional) . . . . . . . . . . . . . . . . . . . . . . . 343

A.16 ICS-3000 Automation Manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 343

A.16.1 RCH-1 Reaction Coil Heater. . . . . . . . . . . . . . . . . . . . . . . . . . 343

A.16.2 Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 343

A.17 ICS-3000 Conductivity Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 344

A.18 ICS-3000 Electrochemical Detector . . . . . . . . . . . . . . . . . . . . . . . . . . 345

TC Specifications

A.19 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 347

A.20 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 347

A.21 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 347

A.22 Thermal Compartment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 348

B • Reordering Information

DP/SP Reordering Information

Doc. 065031-04 1/08 xiii

ICS-3000 Ion Chromatography System

EG Reordering Information

DC Reordering Information

TC Reordering Information

xiv Doc. 065031-04 1/08

1.1 ICS-3000 System Overview

1 • Introduction

Chromeleon®/Chromeleon

Xpress Monitor

ICS-3000 Eluent

Organizer

AS Autosampler

ICS-3000 Dual

ICS-3000

Detector/Chromatography

Module

Pump

ICS-3000 Eluent

Generator

Figure 1-1. ICS-3000 System for Dual-Analysis RFIC

The Dionex ICS-3000 Ion Chromatography System offers a full range of Reagent-

™ IC (RFIC™) components. RFIC combines automated eluent generation

Free and self-regenerating suppression to make IC easier and more powerful than ever

Doc. 065031-04 1/08 1

ICS-3000 Ion Chromatography System

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 results.

The dual-analysis capabilities (both simultaneous and sequential) of the ICS-3000 system let you maximize efficiency and throughput and minimize downtime. The modular system design lets you quickly configure and customize hardware.

1.1.1 ICS-3000 System Components

The table below identifies modules in the ICS-3000 product line, as well as additional products that can be added to an ICS-3000 system. Refer to the page number indicated here for a brief product overview.

Product Type Product Name

Pump

Detector/Chromatography Compartment

Detector (inside DC)

Accessory (inside DC)

Detector (outside DC)

Thermal Compartment

Eluent Generator

Eluent Organizer

ICS-3000 Dual Pump (see page 3)

ICS-3000 Single Pump (see page 3

ICS-3000 Detector/Chromatography Module (see page 3

ICS-3000 Conductivity Detector (see

page 4

)

ICS-3000 Electrochemical Detector (see

page 4

)

ICS-3000 Automation Manager (see

page 4

)

ICS-Series Photodiode Array Detector (see

page 7

)

ICS-Series Variable Wavelength Detector (see page 7

ICS-3000 Thermal Compartment (see

page 4

ICS-3000 Eluent Generator (see page 5)

ICS-3000 Eluent Organizer (see page 5)

)

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1 • Introduction

Autosampler

Mass Spectrometer

ICS-3000 Dual Pump (DP) and ICS-3000 Single Pump (SP)

AS Autosampler (see page 6)

AS40 Automated Sampler (see page 7

MSQ Plus™ (see page 8)

)

With flow rates ranging from 0.001 to 10.0 mL/min and operating pressures up to 35 MPa (5000 psi), the DP/SP is designed for both standard bore and microbore applications. The pump’s patented isokinetic pre-compression phase allows a precise, almost pulse-free flow.

The SP contains one isocratic pump or one gradient pump. The DP contains two gradient pumps, two isocratic pumps, or one isocratic pump and one gradient pump.

The isocratic pump delivers one eluent, while the gradient pump can deliver gradient mixtures of up to four eluent components. The selected eluent composition can be delivered as isocratic, isocratic proportioned, linear ramp, step, curved, or any combination of these.

With a DP, the second pump can be operated as a second-channel chromatography pump, an auxiliary dependent pump, or an auxiliary independent pump.

ICS-3000 Detector/Chromatography Module (DC)

The DC provides a temperature-controlled environment for ICS-3000 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 detector

• Electrochemical detector

• Injection valves

• Switching valves

• Guard and separator columns

• Suppressors

• ICS-3000 Automation Manager

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ICS-3000 Ion Chromatography System

ICS-3000 Conductivity Detector (CD)

The CD is a modular detector with integrated cell providing dual detection capabilities (series or parallel). The CD has a signal range up to 15,000 The CD is installed in the upper compartment of the DC.

ICS-3000 Electrochemical Detector (ED)

The ED is a modular detector and cell with dual-detection capabilities (series or parallel). The ED supports multiple waveforms, multiple integration times, and post-analysis data manipulation. The ED is also capable of providing 3D amperometry data. The ED cell can be configured with gold, silver, platinum, or glassy carbon working electrodes. The ED is installed in the upper compartment of the DC.

ICS-3000 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.

μS and supports high background, nonsuppressed applications.

ICS-3000 Thermal Compartment (TC)

The TC provides a temperature-controlled environment for ICS-3000 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.

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1 • Introduction

ICS-3000 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)

• A high pressure gas removal device that removes electrolysis gases

created during eluent generation

The following options must be ordered separately for installation inside the EG:

• A disposable EluGen® cartridge to generate eluent. Each cartridge

contains 900 mL of the appropriate electrolyte concentrate solution.

• A Continuously Regenerated Trap Column (CR-TC) to remove any

extraneous contaminants from the deionized water source. The CRTC is electrolytically-regenerated, which allows it to operate for extended periods without chemical regeneration.

ICS-3000 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 062629).

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 063493) 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 064387).

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ICS-3000 Ion Chromatography System

AS Autosampler (AS)

The AS is a powerful, full-featured autosampler that precisely delivers from 1.0 to 99.9 µL (in 0.1 µL increments) or 100 to 1000 µL (in 1 µL increments) of sample to an injection valve. The autosampler can operate in several modes:

• Concentrate—Sample is delivered to a single analytical system for

trace analysis and matrix elimination; a concentrator column is installed on the injection valve in place of a loop.

• Simultaneous—Sample is delivered to two analytical systems

simultaneously; a sample loop is installed on each injection valve. Sample is delivered equally to the two systems (50% of the volume to each), allowing two complete, separate analyses to be performed with just one sample.

• Sequential—Sample is delivered to two analytical systems in

sequence. This allows on-demand injection of two independent samples to two applications, using one autosampler. While the first system is being analyzed, the second system is being prepped and loaded for sample analysis.

• Sequential Concentrate—Sample is delivered to two analytical

systems in sequence; a concentrator column is installed on the injection valve in place of a loop.

• Reagent Prime (available in Concentrate mode only)—Primes the

lines with reagent. For example, implementing the Reagent Prime mode during the matrix elimination step ensures that the appropriate reagent is in line for matrix elimination and prevents crosscontamination between reagents.

• Reagent Flush (available in Concentrate mode only)—Flushes the

concentrator column with reagent (for example, a known source of clean deionized water) to remove unwanted sample matrix.

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1 • Introduction

AS40 Automated Sampler (AS40)

The AS40 is a low-cost, metal-free, sample loading device designed for ion chromatography applications. The AS40 is capable of delivering between 0.2 and 5.0 mL of sample in set increments. The AS40 holds between 66 and 88 vials, depending upon the vial size in use: 0.5 mL,

5.0 mL, or a combination of both sizes. Up to three injections can be taken from each vial.

The AS40 holds up to 11 cassettes of six 5-mL vials or eight 0.5-mL vials. Each sample is filtered during loading through a 20-µm filter in the vial cap, so there is no need to prefilter samples. Samples can be loaded against backpressures up to 690 kPa (100 psi) without an external sampling pump, thus facilitating preconcentration work.

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 individual wavelengths instead of the spectra offers two advantages: it eliminates the need to perform extractions for analyses that do not require spectral data and it conserves disk space.

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.

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ICS-3000 Ion Chromatography System

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). Both ionization techniques can be run in either the positive or negative ion polarity mode. The design of the interchangeable probes enables rapid switching of ionization modes.

During a scan, ions of selected mass-to-charge ratios are sequentially transmitted through a quadrupole mass filter analyzer. The MS detector has fully automatic mass scale calibration (15 to 2000 m/z) and tuning that makes optimization simple and direct. The MS detector can perform both full-range scans and selected ion monitoring (SIM) scans. When operating in conjunction with Chromeleon, the MSQ Plus can be set up to vary the scan type, the ionization technique, and the ion polarity mode.

8 Doc. 065031-04 1/08

1.1.2 ICS-3000 System Control

The ICS-3000 system is controlled by a PC configured with Chromeleon Chromatography Management System (version 6.7 or later) or Chromeleon Xpress. The Chromeleon System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress

monitoring of Dionex chromatography instruments, but does not include data management capabilities.

Chromeleon and Chromeleon Xpress provide a panel tabset that replaces and combines the module front panels into one centralized system control panel. A convenient Home panel (see Figure 1-2 system status. Individual tabs provide quick access to module functions, as well as detailed status and diagnostics.

1 • Introduction

Chromatography Management

provides real-time control and

) shows the overall

Figure 1-2. ICS-3000 Panel Tabset (Home Panel Shown)

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ICS-3000 Ion Chromatography System

1.2 ICS-3000 System Documentation

Every effort has been made to provide complete and accurate user documentation for the ICS-3000 system. The table below lists the primary sources of product information and the formats in which information is available.

Source Part

Number

ICS-3000 Ion Chromatography System Operator’s Manual

Installing the ICS-3000 Ion Chromatography System

AS Autosampler Operator’s Manual 065051 Yes No

ICS-Series Photodiode Array Detector Operator’s Manual

ICS-Series Variable Wavelength Detector Operator’s Manual

Chromeleon Xpress Quick Reference Guide 065070 Yes No

Chromeleon Xpress online Help N/A N/A N/A

Chromeleon Software User’s Guide

Installing the Chromeleon Chromatography Management System with a Dionex Ion Chromatograph (IC)

Chromeleon online Help N/A N/A N/A

065031 Yes No

065032 Yes Yes

065147 Yes No

065141 Yes No

4829.5060

031883 Yes Yes

PDF File

Ye s N o

Printed Manual

All Adobe

® PDF files listed above are shipped on the Dionex Reference Library

CD-ROM (P/N 053891), which is included in the ship kit of each ICS-3000 system module. In addition, the software manuals are provided as PDF files on the Chromeleon or Chromeleon Xpress CD-ROM.

A printed copy of the software installation instructions is provided in the software ship kit.

Consumables documentation: For complete information about Dionex columns, suppressors, EluGen cartridges, etc., refer to the appropriate product manual. These manuals are provided on the Reference Library CD-ROM.

10 Doc. 065031-04 1/08

1.3 The ICS-3000 System Operator’s Manual

1.3.1 Overview

The electronic version (i.e., PDF file) of the ICS-3000 system operator’s manual contains numerous hypertext links that can take you to other locations within the file. 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 Adob

e® Acrobat® or Adobe Reader® for assistance.

1 • Introduction

Chapter 1 Introduction

Chapter 2 Description

Chapter 3 System Configurations

Chapter 4 Getting Started

Chapter 5 Operation

Chapter 6 Shutdown

Chapter 7 Maintenance

An overview of the ICS-3000 system; includes a brief description of the ICS-3000 modules, the software required for ICS-3000 operation, and the ICS-3000 user manuals.

Detailed descriptions of ICS-3000 system components and important operating features; includes an introduction to Chromeleon and Chromeleon Xpress software.

Detailed illustrations of component plumbing for several different ICS-3000 system configurations.

Tasks to be performed before beginning operation of the ICS-3000 system.

Instructions for routine operation of the ICS-3000 system with Chromeleon or Chromeleon Xpress software.

Short-term and long-term shutdown procedures for the ICS-3000 system.

Routine preventive maintenance procedures for the ICS-3000 system.

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ICS-3000 Ion Chromatography System

Chapter 8 Troubleshooting

Minor problems that may occur during operation of the ICS-3000 system, with step-by-step procedures for how to isolate and eliminate the cause of each problem. Includes a list of Chromeleon and Chromeleon Xpress Audit Trail error messages, with an explanation of the possible cause of each message and the corrective action to take.

Chapter 9 Service

Step-by-step instructions for routine service and parts replacement procedures the user can perform for the ICS-3000 system.

Appendix A Specifications

Appendix B Reordering Information

Specifications and installation site requirements for the ICS-3000 modules.

Spare parts for the ICS-3000 modules.

1.3.2 Safety Messages and Notes

This manual contains warnings and precautionary statements that can prevent personal injury and/or damage to the ICS-3000 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.

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.

12 Doc. 065031-04 1/08

1 • Introduction

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.

Doc. 065031-04 1/08 13

ICS-3000 Ion Chromatography System

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.

1.4 Safety and Regulatory Information

The ICS-3000 system is designed for IC (ion chromatography) and HPLC (highperformance liquid chromatography) applications and should not be used for any other purpose. Operation of an ICS-3000 module in a manner not specified by Dionex may result in personal injury.

1.4.1 Safety Labels

The TUV GS, C, US Mark safety label and the CE Mark label on the ICS3000 modules indicate that they are in compliance with the following standards:

EMC Susceptibility and Immunity

• (DC, EG, DP, SP) EN 61326 1997 including A1:1998 and A2:2001

• (TC) EN 61326 1997 including A1:1998, A2:2001, and A3:2003

Safety

• (DC, EG, DP, SP) EN 61010-1:2001, UL 61010-1:2004, CAN/CSA-

C22.2 61010-1:2004

• (TC) EN 61010-1:2001, UL 61010A:2002, CAN/CSA-C22.2 61010-

1:2004

NOTE The TC does not carry the TUV GS Mark safety

label.

14 Doc. 065031-04 1/08

1 • Introduction

These symbols appear on the ICS-3000 modules or on labels affixed to the modules:

Alternating current

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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ICS-3000 Ion Chromatography System

16 Doc. 065031-04 1/08

DP/SP Description

2.1 DP/SP Front Features

A status bar on the front of the ICS-3000 Dual Pump (DP) and ICS-3000 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).

2 • Description

CONNECTED

ALARM

FLOW PRIME

PUMP 1 PUMP 2

FLOW PRIME

Figure 2-1. DP Status Bar

PRIME

FLOW

PUMP 1

Figure 2-2. SP Status Bar

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ICS-3000 Ion Chromatography System

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

CONNECTED

The DP/SP is connected to a Chromeleon or Chromeleon Xpress timebase.

Does not flash.

ALARM

A DP/SP-related problem has

Does not flash. occurred (for example, a pressure limit was activated). Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause.

PUMP 1 FLOW* PUMP 2 FLOW**

PUMP 1 PRIME* PUMP 2 PRIME**

The DP/SP is on and is delivering flow.

Use the

PRIME button to

prime the pump.

Does not flash.

The pump is being primed.

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. ** SP only: This button is not present.

18 Doc. 065031-04 1/08

2.2 DP/SP Interior Components

The pump’s mechanical components are located directly behind the front door of the module. Figure 2-3 both a gradient pump (pump 1) and an isocratic pump (pump 2).

For servicing components, the component mounting panel slides out about 5 cm (2 in) for easy access to components. To pull the panel out, use the handles on the top and bottom of the panel.

shows the mechanical components of a DP that contains

2 • DP/SP Description

Status Bar

Secondary Pump Head

Priming Valve

Pressure Transducer

Primary Pump Head

Peristaltic Pump (for

seal wash system) Vacuum Degas Chamber

(one channel)

Eluent Supply On/Off Valve

Tubing Chase (Pump 2)

Handle

Piston Seal Wash Reservoir

Vacuum Degas Chambers

(four channels)

Static Mixer

Proportioning Valve Fittings

Tubing Chase (Pump 1)

Leak Sensor

Figure 2-3. DP/SP Interior Components (DP Shown)

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ICS-3000 Ion Chromatography System

2.2.1 Pump Heads

The DP/SP is a zero-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, the pulsation increases as the operating pressure increases, since part of the delivery stroke is required to compress eluent in the pump head.

During the pre-compression phase, pulsation is minimized by velocity modulation of the drive. 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 Moduleware (the 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.

Flow output from the secondary pump head passes through a static mixer (described in Section 2.2.6 chromatography system (the injection valve, columns, and detector).

) before being directed to the remainder of the

2.2.3 Proportioning Valves (Gradient pump only)

In the gradient pump, eluent flows from the eluent reservoirs, through the vacuum degas chambers, and into a four-way proportioning valve assembly (see Figure 2-3 proportioned by the four valves.

20 Doc. 065031-04 1/08

). Programmed percentages of each eluent are

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

μL per channel

• A dual-stage diaphragm vacuum pump

• An on-board vacuum sensor

• The electronics required to operate the vacuum pump

2 • DP/SP Description

• 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 vacuum degassing module delivers the optimal degassing performance.

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. In Chromeleon or Chromeleon Xpress, select Command on the Control menu or press the F8 key.

2. In the Commands dialog box, select the pump name.

3. Select the Degasser command.

4. Select Off and click the Execute button.

5. To turn on the degasser again, select On and click Execute.

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ICS-3000 Ion Chromatography System

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.

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 seal 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 Dionex, the seal wash system is connected to pump 1 (the bottom pump). If necessary, connect the seal wash system to pump 2 (the top pump), instead. For instructions on how to replumb the system, refer to Section 4.5

NOTE Dionex offers an External Seal Wash Kit

(P/N 063518) for users who need to operate a piston seal wash system for both pumps in the DP. Installation instructions are provided in the kit.

2.2.6 Static Mixer

A GM-3 or GM-4 static mixer is installed after the secondary pump head (see Figure 2-3 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

μL when a GM-4 is installed. The gradient delay volume (or dwell

380 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.

22 Doc. 065031-04 1/08

). In the gradient pump, the mixer helps to ensure that

μL when a GM-3 is installed and

2.3 DP/SP Flow Schematics

ON/O

2.3.1 Isocratic Pump Flow Schematic

Figure 2-4 illustrates the liquid flow path through an isocratic pump.

2 • DP/SP Description

TO INJECTION VALV

ELUENT

OUTLET CHECK VALVE

VACUUM DEGAS

ELUENT SUPPLY

FF VALVE

PUMP HEAD

INLET CHECK VALVE

Figure 2-4. Isocratic Pump Flow Schematic

• Eluent flows from the reservoir, through the vacuum degas chamber

(if the vacuum degas module is installed), 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 remainder

of the chromatography system (the injection valve, columns, and detector).

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ICS-3000 Ion Chromatography System

2.3.2 Gradient Pump Flow Schematic

Figure 2-5 illustrates the liquid flow path through a gradient pump.

ELUENT

STATIC

MIXER

TO INJECTION VALV

OUTLET CHECK VALVE

VACUUM

DEGAS

PROPORTIONING

VALV E

PUMP HEAD

INLET CHECK VALVE

Figure 2-5. 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

• Flow exits the secondary pump head, continues through the static

mixer, and is then directed to the remainder of the chromatography system (the injection valve, columns, and detector).

24 Doc. 065031-04 1/08

2.4 DP/SP Rear Panel

Figure 2-6 illustrates the rear panel of the DP/SP.

2 • DP/SP Description

Tubing Chase (2)

Main Power Switch, Fuse Holder,

and Power Receptacle

Analog Pressure Output

Digital I/O Port

USB Receptacle

(“B” Connectors)

USB Ports (3)

(“A” Connectors)

Exhaust Port from Vacuum

Degas Module

Waste Line from

Drip Tray

Figure 2-6. 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).

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

Doc. 065031-04 1/08 25

ICS-3000 Ion Chromatography System

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 9.9

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 an AS40 Automated Sampler or other auxiliary device. The connector includes three TTL inputs and four relay outputs. Table 2-1

indicates the functions assigned to the connector pins.

For instructions on connecting the pump to an AS40, refer to the ICS-3000 Ion Chromatography System Installation Instructions (Document No. 065032). The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

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

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

26 Doc. 065031-04 1/08

2 • DP/SP Description

Pin Number Signal Name Signal Level Description

7 Relay 1 Out Potential-free Common

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

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ICS-3000 Ion Chromatography System

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. In Chromeleon or Chromeleon Xpress, select Command on the Control menu or press the F8 key.

2. In the Commands dialog box, select the pump name.

3. Select the AnalogOut command.

4. Select PumpTop in the AnalogOut drop-down box and click Execute.

USB Connections

• One USB receptacle (“B” type connector) allows a connection from the PC on

which Chromeleon or Chromeleon Xpress software is installed.

• Three USB (Universal Serial Bus) ports (“A” type connectors) are provided

for connections to other ICS-3000 modules.

One 1.8-m (6-ft) USB cable (P/N 960777) is provided in the ship kit (DP Ship Kit, P/N 062463; SP Ship Kit, P/N 063342).

Waste Lines

• One waste line is connected to the secondary pump head.

• One waste line exits the drip tray and is routed to the rear panel.

Place the free ends of the waste lines into one waste container. To maintain a positive siphon, position the waste container below the level of the pump.

NOTE To ensure proper drainage, the waste lines must remain

above the liquid level in the waste container.

28 Doc. 065031-04 1/08

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 2-liter plastic reservoir (P/N 062510) for offline vacuum degassing of eluents. The reservoir was not designed for this purpose.

N'utilisez pas le réservoir en plastique de 2 litres (N/P 062510) pour le dégazage à vide hors ligne d'éluants. Le réservoir n'a pas été conçu à cette fin.

Verwenden Sie den 2-Liter Plastikbehälter (Bestell-Nr. 062510) nicht zum Offline Vakkum-Entgasen von Eluenten. Der Behälter ist dafür nicht ausgelegt.

2 • DP/SP Description

All eluent reservoirs listed above are pressurizable. Although the DP/SP does not require pressurized reservoirs, Dionex recommends pressurizing reservoirs with helium or nitrogen under the following circumstances:

• When using eluents that are sensitive to contamination.

• 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).

Doc. 065031-04 1/08 29

ICS-3000 Ion Chromatography System

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

2.6 EO (Optional)

The ICS-3000 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 062629).

All eluent reservoirs available for use with the DP/SP can be pressurized. 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 063493) 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, ICS-Series Variable Wavelength Detector, or ICS-Series

Photodiode Array Detector is installed as the topmost module in the system, the TC/VWD/PDA Regulator Bracket Kit (P/N 064792) 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 062345).

30 Doc. 065031-04 1/08

EG Description

2.7 EG Front Features

The status bar on the front of the ICS-3000 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 2-7

CONNECTED

Button/LED Label

CONNECTED

ALARM

EGC 1 EGC 2

CR-TC 1 CR-TC 2

CR-TC

ALARM

EGC

Figure 2-7. EG Status Bar

If the LED Is On Comment

The EG is connected to a Chromeleon

-----

or Chromeleon Xpress timebase.

An EG-related problem has occurred (for example, the EluGen cartridge was disconnected).

The EluGen cartridge is on and is generating eluent.

Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause.

EGC 1 is always installed in the left section of the component compartment. EGC 2, if present, is installed in the right section of the compartment.

The CR-TC is on. CR-TC 1 is always installed in

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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ICS-3000 Ion Chromatography System

Button/LED Label

POWER

If the LED Is On Comment

Use this POWER button for routine on/off control of the 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.

The main power switch is on the EG rear panel.

32 Doc. 065031-04 1/08

2.8 EG Interior Components

Figure 2-8 shows the EG component compartment, which is located directly

behind the front door. The component mounting panel divides the compartment into two sections. In a single-channel EG, components are installed in the left section only.

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.

2 • EG Description

EluGen Cartridge

RFIC Eluent Degasser

Electrical Connectors

CR-TC

Waste Line

Drip Tray

Slide Release Latch

Figure 2-8. EG Interior Components

(Second (Right Side) Channel of a Dual-System EG Shown)

Doc. 065031-04 1/08 33

ICS-3000 Ion Chromatography System

EluGen Cartridge

Several types of EluGen cartridges are available for use with the EG (see the table below). Each cartridge contains 900 mL of the appropriate electrolyte concentrate solution for eluent generation.

EluGen Cartridge Part Number Function

EGC II K2CO3 EluGen Cartridge

058904 Generates potassium carbonate eluent

for anion exchange separations. Note: Produces a carbonate/bicarbonate mixture when installed with the EPM Electrolytic pH Modifier (P/N 063175)

EGC II KOH EluGen Cartridge

EGC II LiOH EluGen Cartridge

EGC II MSA EluGen Cartridge

EGC II NaOH EluGen Cartridge

and EGC-CO

058900 Generates potassium hydroxide eluent

for anion exchange separations.

058906 Generates lithium hydroxide eluent for

anion exchange separations.

058902 Generates methanesulfonic acid eluent

for cation exchange separations.

058908 Generates sodium hydroxide eluent for

anion exchange separations.

Mixer (P/N 061686).

For more information, refer to the EluGen cartridge manual. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

RFIC Eluent Degasser

The RFIC Eluent Degasser (P/N 062137) contains a tubing assembly that purges the electrolysis gas from the freshly-generated eluent before it is directed to the separator column.

Backpressure Coil (Optional)

The EluGen cartridge 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 EluGen cartridge refer to Section 9.15

34 Doc. 065031-04 1/08

OUTLET port. For details,

2 • EG Description

Continuously Regenerated Trap Column (CR-TC)

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

• CR-ATC (Continuously Regenerated Anion Trap Column, P/N 060477)

• CR-CTC (Continuously Regenerated Cation Trap Column, P/N 060478)

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

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

Modifier.

EluGen Cartridge or an EPM Electrolytic pH

2CO3

NOTE The IonPac

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

EPM Electrolytic pH Modifier and EGC-CO

® ATC-HC Trap Column (P/N 059604) or

Mixer

The EGC II K2CO3 EluGen Cartridge can be used with an EPM Electrolytic pH Modifier (P/N 063175) and an EGC-CO

Mixer (P/N 061686) to produce a

carbonate/bicarbonate mixture for use with anion exchange separations on carbonate-based IonPac columns.

After the cartridge generates potassium carbonate eluent, the EPM adjusts the eluent concentration to produce the carbonate/bicarbonate mixture. The EGC-

Mixer provides mixing necessary to produce a homogenous solution of

electrolytically-generated K

and KHCO3 eluent.

2CO3

For more information about these products, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Reference Library CD-ROM (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 or Chromeleon Xpress, 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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ICS-3000 Ion Chromatography System

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 EluGen cartridges or one cartridge and one EPM Electrolytic pH

Modifier

and

• Two Continuously Regenerated Trap Columns (CR-TC)

When operating with an EGC II K

EluGen Cartridge and the EPM, the

2CO3

cartridge 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.

Waste Line

The module waste line (white tubing) discharges liquid and gas waste from the RFIC Eluent Degasser. This line is marked

WASTE-GAS SEPARATOR inside the

EG.

NOTE A gas separator waste tube (P/N 045460) should be

connected to the EG waste line during installation. For details, refer to the ICS-3000 Ion Chromatography System Installation Instructions (Document No. 065032).

Place the free end of the waste line into a waste container. To maintain an active drain, position the waste container below the level of the EG.

NOTE To ensure proper drainage, each waste line must remain

above the liquid level in the waste container.

36 Doc. 065031-04 1/08

2.9 EG Rear Panel

Figure 2-9 illustrates the rear panel of the ICS-3000 Eluent Generator (EG).

2 • EG Description

Exhaust Fan

Gas Vent Lines

USB Receptacle

(“B” Connector)

USB Ports (2)

(“A” Connectors)

Fuse Holder, Main Power

Switch, and Power Receptacle

Tubing for Connecting to

Suppressors

Tub ing C hase

Drain Port from Drip Tray

Figure 2-9. 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 or Chromeleon Xpress software is installed.

• Two USB (Universal Serial Bus) ports (“A” type connectors) are provided for

connections to other ICS-3000 modules.

One 1.8-m (6-ft) USB cable (P/N 960777) is provided in the EG Ship Kit (P/N 062453).

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ICS-3000 Ion Chromatography System

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 9.16

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 2-7 press and hold the

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.

POWER button for 2 seconds.

). To turn off the EG,

Tubing Chase

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

Vent, Suppressor, and Drain Lines

• The gas vent line (clear tubing) discharges the electrolysis gas (H

or O2) that

is vented from the electrolyte reservoir of the EluGen cartridge.

• The lines exiting the tubing chase (white tubing) are for connecting the

REGEN IN port on the CR-TC or EPM Electrolytic pH Modifier to the REGEN OUT port on the suppressor.

• The drip tray drain port removes any liquid that collects in the drip tray in the

bottom of the EG. A clear corrugated tubing line is connected to this port during installation.

38 Doc. 065031-04 1/08

Place the free ends of the vent and drain lines into a waste container. To maintain a positive siphon, position the waste container below the level of the EG.

NOTE To ensure proper drainage, each waste line must remain

above the liquid level in the waste container.

2.10 EG Flow Schematic

Figure 2-10 illustrates the liquid flow path through the EG.

Deionized water is delivered by the DP/SP to the EluGen cartridge. DC current is applied to the cartridge to produce eluent.

The electrolytically-generated eluent flows through the Continuously Regenerated Trap Column (CR-TC) into the RFIC Eluent Degasser, 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 Atlas or SRS suppressor regenerant chamber to the CR-TC regenerant chamber, through the RFIC Eluent Degasser inside the EG, and finally to waste.

2 • EG Description

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

schematic showing the components required to generate a carbonate/bicarbonate mixture. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

Doc. 065031-04 1/08 39

ICS-3000 Ion Chromatography System

EGC VENT

To Waste

From pump

To injection valve port P

To gas separator waste tube

From suppressor REGEN OUT

Inlet

EGC

EGC OUT

Outlet

Eluent In Port

(red label)

Eluent

Out

Regen Out Port

Regen In Port (orange label )

RFIC

Eluent

Degasser

Regen

Out

(blue label )

Regen Out

Regen In

Eluent In

CR-TC

Eluent Out Port

(yellow label)

Figure 2-10. EG Flow Schematic Example

40 Doc. 065031-04 1/08

DC Description

2.11 DC Front Features

A status bar on the front of the ICS-3000 Detector/Chromatography Module (DC) (see Figure 2-12 LEDs that indicate the status of several DC components and functions.

) includes buttons for controlling certain DC functions, as well as

CONNECTED

12UPPER

ALARM

SUPPRESSOR OVEN VALVE 1 VALVE 2

LOWER LOAD INJECT LOAD INJECT

Figure 2-11. DC Status Bar

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

CONNECTED

The DC is connected to a

Does not flash. Chromeleon or Chromeleon Xpress timebase.

ALARM

The leak sensor is wet or there was a

Does not flash. valve or suppressor error. Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause.

SUPPRESSOR 1 SUPPRESSOR 2

OVEN UPPER

The suppressor is on and current is being applied.

The upper compartment is at its set temperature.

Does not flash.

The upper compartment is

transitioning to the set

temperature. The

compartment is not ready for

operation.

OVEN LOWER

The lower compartment is at its set temperature.

The lower compartment is

transitioning to the set

temperature. The

compartment is not ready for

operation.

Doc. 065031-04 1/08 41

ICS-3000 Ion Chromatography System

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

VALVE 1 LOAD VALVE 2 LOAD

VALVE 1 INJECT VALVE 2 INJECT

POWER

Use the VALVE 1 and VALV E 2 buttons to manually switch the

Valve error. See Section 8.25

for troubleshooting. position of the DC injection valves. The LEDs indicate whether the valve is in the Load or Inject position.

Use this POWER button for routine

Does not flash. 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 disabled in Chromeleon or Chromeleon Xpress. When disabled, the valve can be controlled only from the software. To enable or disable a button, open the Commands dialog box (press F8) and select the Valve1Button (or Valve2Button) command in the list of commands for the DC.

42 Doc. 065031-04 1/08

2 • DC Description

Sample Loading Ports

The front of the DC has two sample loading ports (see Figure 2-12) that can be connected to injection valves installed inside the DC. A syringe is used to manually load sample through the ports. For automated sample injection, the DC can be connected to an autosampler. For more information about sample injection, see Section 5.1

Sample Loading Ports

Figure 2-12. DC Sample Loading Ports

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ICS-3000 Ion Chromatography System

2.12 DC Interior Components

Figure 2-13 illustrates the interior compartments of the DC.

Upper Compartment

Automation

Manager Components

Electrochemical

Detector and Cell

Conductivity

Detector and Suppressor

Lower Compartment

Columns and

Injection Valves

Figure 2-13. DC Interior View Example

Upper Compartment

The upper compartment consists of two sections:

• The top section houses an optional ICS-3000 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 2.17

for details about the AM.

• The section below the AM section houses one or two detectors. The detectors

can be either two ICS-3000 Conductivity Detectors (CDs), two ICS-3000 Electrochemical Detectors (EDs), or one detector of each type. See

Section 2.15

ED.

44 Doc. 065031-04 1/08

for details about the CD and Section 2.16 for details about the

2 • DC Description

Suppressors for conductivity detection are installed in this compartment also. The following types of suppressors can be used:

• SRS Self-Regenerating Suppressor (SRS 300 or ULTRA II) (2- and 4-mm)

• AES Atlas Electrolytic Suppressor

• MMS™ MicroMembrane™ Suppressor (MMS 300 or MMS II)

Lower Compartment

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 electricallyactivated, two position valves. See Section 2.14 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 2-14

for details about the injection

Handle for pulling tray forward

Figure 2-14. DC Side View with Lower Compartment Tray Pulled Out

Doc. 065031-04 1/08 45

ICS-3000 Ion Chromatography System

Temperature Control

The following temperature control zones are possible with the DC, depending on the options installed:

• In the single-zone (shared) configuration, the upper and lower compartments

are in the same temperature zone. The temperature can be set to between 15 and 40 °C. Air flow passages between the compartments allow the temperature to stabilize equally in both compartments.

• In the dual-zone configuration, the lower compartment is isolated from the

upper compartment in a separate temperature zone. There is no common air flow between the upper and lower compartments. The temperature of the lower compartment can be set to between 10 and 70 °C. The temperature of the upper compartment can be set to between 15 and 40 °C.

• When a CD is installed, the heated conductivity cell can be set to 5 °C above

the upper compartment temperature, up to 60 °C.

• If an RCH-1 Reaction Coil Heater is installed in the AM, the temperature of

the RCH-1 heater can be set to 5 temperature, up to 80 °C.

°C above the upper compartment

The temperatures achieved for a particular zone can vary from the control range, depending on the ambient temperature (see the table below).

Temperature Zone Control

Range

Upper compartment (or shared zone)

Lower compartment 10 to 70 °C Minimum temperature ≥ (ambient − 5°C)

CD cell 15 to 60 °C Minimum temperature ≥ (upper compartment

RCH-1 15 to 80 °C Minimum temperature ≥ (upper compartment

15 to 40 °C If the RCH-1 is off:

Achieved Temperatures (Based on Ambient)

Minimum temperature ≥ (ambient − 10 °C) If the RCH-1 is at 80 °C or the CD cell is at 60 °C Minimum temperature ≥ (ambient − 5°C)

Maximum temperature ≥ (ambient + 50 °C)

temperature + 5 °C)

For example, if the ambient air temperature in your lab is 30 °C and you set the upper compartment temperature to 15 °C, the actual temperature achieved in the upper compartment will be about 20 °C.

46 Doc. 065031-04 1/08

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 compartments and to recalibrate, if required.

2.13 DC Rear Panel

Figure 2-15 illustrates the rear panel of the DC.

2 • DC Description

Tubing Chase (2)

Switched AC Sockets

Fuse Holder, Main

Power Switch, and Power Receptacle

External Low

Pressure Valve

Mounting Slots

USB Receptacle

(“B” Connector)

USB Ports (2)

(“A” Connectors)

External Low Pressure Valve

Connectors Analog Output and

TTL/Relay Connectors

(optional)

Drain Line Connector

Figure 2-15. 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.

Doc. 065031-04 1/08 47

ICS-3000 Ion Chromatography System

Switched AC Sockets

The two AC receptacles can be used to control the power to external devices. Use Chromeleon or Chromeleon Xpress to switch the power on and off. TTL inputs can also be used to control the AC sockets (see Section 2.18.4

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 9.19

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 2-12 press and hold the

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

POWER button for 2 seconds.

). To turn off the DC,

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 or Chromeleon Xpress software is installed.

The two USB ports (“A” type connectors) allow 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 062614, dual; P/N 063408, single).

48 Doc. 065031-04 1/08

2 • DC Description

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 or Chromeleon Xpress.

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 2.18

for details about the I/O option.

Doc. 065031-04 1/08 49

ICS-3000 Ion Chromatography System

2.14 Injection Valves

One or two injection valves can be installed in the lower compartment of the DC. The following models are available: 6-port (P/N 061961) and 10-port (P/N 061962).

2.14.1 Injection Valve Operation

Each ICS-3000 Ion Chromatography System injection valve has two operating positions: Load and Inject. Liquid flows through either the Load or Inject path, depending on the valve position.

Sample In

Sample Loop

(6) W

To Waste

Figure 2-16

AD POSITION

shows flow schematics for the 6-port valve.

INJECT POSITION

Sample In

To Column

L (4)(5) S

From Pump

= Sample

Sample Loop

(6) W

To Waste From Pump

= Eluent

L (4)(5) S

To Colum

Figure 2-16. 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 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 describes how to inject samples manually and Section 5.2 how to inject samples with an autosampler.

describes

50 Doc. 065031-04 1/08

2 • DC Description

Figure 2-17 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 possible, depending on the components to be connected to the valve and the application to be run. Refer to the appropriate Dionex Application Note for more information.

Large

Loop

Sample In

LOAD POSITION

(Loop Loading)

Concentrator

To Waste

Carrier Pump In

To C o lumn

Eluent

Pump In

To Waste

Large

Loop

Sample In

= Sample = Carrier = Eluent

INJECT POSITION

(Concentrator Loading)

Concentrator

To Waste

Carrier Pump In

To Colum Eluent

Pump In

To Waste

Figure 2-17. 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 2-17

, 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.

Doc. 065031-04 1/08 51

ICS-3000 Ion Chromatography System

• 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.

2.14.2 Injection Valve Plumbing

Figure 2-18 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 10 μL PEEK and L (4).

Dionex offers sample loops in various sizes. If needed, the pre-installed 10 μL loop can be replaced with a loop that has a different sample injection volume.

™ sample loop (P/N 042949) is installed between ports L (1)

Figure 2-18. Injection Valve Plumbing (6-Port Valve)

52 Doc. 065031-04 1/08

2.15 CD Conductivity Detector

One or two ICS-3000 Conductivity Detectors (CDs) can be installed in the DC. Each 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). A suppressor (optional) can be installed on the clips on the lower part of the CD. The cell and suppressor are installed in the upper compartment of the DC (see Figure 2-13 accessible to the user.

Conductivity

Cell

Suppressor

(Optional)

(SRS model

shown)

2 • DC Description

). The detector electronics are not

Figure 2-19. Conductivity Detector with Suppressor

2.15.1 Heated Conductivity Cell

The DC 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 and low dispersion. Temperature control and compensation help ensure good peak reproducibility and baseline stability.

Doc. 065031-04 1/08 53

μL),

ICS-3000 Ion Chromatography System

Temperature Control

Temperature directly affects the conductivity of a solution. For example, laboratory heating and air conditioning systems can cause a regular slow 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 middle and upper 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.

Follow these steps to change the temperature compensation factor:

1. In Chromeleon or Chromeleon Xpress, select Command on the Control menu or press the F8 key.

2. In the Commands dialog box, select the conductivity detector.

3. Select the Temperature_Compensation command and enter the desired value.

4. Click Execute.

54 Doc. 065031-04 1/08

2.15.2 Suppressor

The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. The CD can operate with an AES, SRS 300, SRS ULTRA II, MMS 300, or MMS III suppressor.

2 • DC Description

The suppressor is installed below the cell on the CD (see Figure 2-19 The suppressor cable plugs into the connector next to the detector (on either the left or the right side, depending on which side the CD is installed) (see Figure 2-20

Figure 2-20. Suppressor Connection (Right-Side Installation)

NOTE It is also possible to control a suppressor with an

ICS-3000 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.

Plug in the suppressor cable here

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 Dionex Reference Library CD-ROM (P/N 053891).

NOTE A gas separator waste tube (P/N 045460) should be

connected to the suppressor waste line during installation to prevent accumulation of oxygen or hydrogen gasses. For details, refer to the ICS-3000

Ion Chromatography System Installation Instructions

(Document No. 065032).

Doc. 065031-04 1/08 55

ICS-3000 Ion Chromatography System

2.15.3 System Flow Schematic for Conductivity Detection

Figure 2-21 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 Dionex Reference Library CD-ROM (P/N 053891).

OUT

CELLCOND

SUPPRESSOR

GUARD

WASTE

SEPARATOR COLUMN

SAMPLE

VALV E

TEMPERATURE

STABILIZER

ELUENT

PUMP or ELUENT GENERATOR

Figure 2-21. DC Flow Schematic for Conductivity Detection

(Suppression in Recycle Mode)

• Eluent from the pump or EG flows into the injection valve .

• After sample is loaded into the sample loop 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, then on to the guard and separator columns , and then through the suppressor .

• From the suppressor, the mixture flows through the cell , where the

analytes are detected. A digital signal is sent to Chromeleon or Chromeleon Xpress software.

• Finally, the mixture flows out of the cell and is recycled back into the

suppressor , where it is used as the water source for the regenerant chamber. Flow is then routed to waste . If an EG is installed, flow is routed to the CR-TC (see Section 2.10

56 Doc. 065031-04 1/08

for details).

2.16 ED Electrochemical Detector

One or two ICS-3000 Electrochemical Detectors (EDs) can be installed in the DC. Each complete ED assembly consists of an amperometry 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 2-13 electronics are not accessible to the user.

The ED can perform the following electrochemical detection modes:

• DC amperometry (see Section 2.16.3)

• Integrated amperometry (includes pulsed amperometry) (see Section 2.16.4)

• Cyclic voltammetry (see Section 2.16.5)

2.16.1 Amperometry Cell

The ED amperometry cell is a three-electrode voltammetric cell. It is a miniature flow-through cell with a titanium cell body (the counter electrode), a working electrode, and a combination pH-Ag/AgCl reference electrode (see Figure 2-22 depends on the application. Four conventional (non-disposable) working electrode types are available: gold, platinum, silver, and glassy carbon. Three disposable working electrodes types are available: gold, silver, and platinum.

). The cell mounts on the front of the detector. The detector

2 • DC Description

). The type of working electrode used

Working Electrode

Figure 2-22. Amperometry Cell (Titanium Cell Shown)

Doc. 065031-04 1/08 57

Cell Body

(counter electrode)

Reference

Electrode

ICS-3000 Ion Chromatography System

Cell Design

The ED amperometry 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 (0.25 also allows operation with high efficiency, narrow bore 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.

Amperometry Cell Solvent Compatibility

The amperometry cell can be used with common reversed-phase solvents such as methanol and acetonitrile. If a disposable working electrode is used, the percentage of methanol should not exceed 30% and the percentage of acetonitrile should not exceed 10%. 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.

μL) of the channel

2.16.2 Combination pH–Ag/AgCl Reference Electrode

The 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

58 Doc. 065031-04 1/08

2 • DC Description

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 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 reference electrode to dry 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 install fitting plugs. For longer shutdowns, remove the electrode from the cell and store it in its storage cap filled with saturated KCl solution. See Section 6.4 detailed storage instructions.

for

Monitoring the Amperometry 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 reference electrode needs regenerating or replacing, thus improving the reproducibility of your analyses. See

Section 4.1.2

NOTE Monitor the pH when the reference electrode is used in

Doc. 065031-04 1/08 59

for how to monitor the pH readout.

the Ag mode as well as in the pH mode.

ICS-3000 Ion Chromatography System

2.16.3 DC Amperometric Detection

In DC amperometry, a constant potential is applied to the working electrode. The potential can be entered into a program file (PGM) (see

Figure 2-23

) or on the Control panel for direct control.

Figure 2-23. DC Amperometry Program Wizard Page

The applied voltage can be programmed up to 10 times during the run. The actual number of potential changes allowed depends on the available data storage capacity, which is determined by the length of the run and the data sampling rate.

60 Doc. 065031-04 1/08

2 • DC Description

2.16.4 Integrated and Pulsed Amperometric Detection

Integrated and pulsed amperometric detection are similar to DC amperometry (see Section 2.16.3 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 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 2.16.6

Pulsed Amperometric Detection

for more information about waveforms.

In pulsed amperometric detection (also known as PAD), current is integrated at a single constant potential (see Figure 2-24

) in that molecules are oxidized or

+0.7

Potential (Volts)

+0.1

-0.1

Delay

Integration

0.2 0.40.0 Time (Seconds)

E2 E3

0.6

. Analytical Potential

. Cleaning Potential

. Reconditioning Potentia

Figure 2-24. 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 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.

Doc. 065031-04 1/08 61

ICS-3000 Ion Chromatography System

Integrated Amperometric Detection

With integrated amperometric detection (also known as IA or IPAD), current is integrated at two or more potentials (see Figure 2-25

+0.60

+0.35 Potential (Volts)

-0.10

-0.60

0.0

Integration

0.2

Time (Seconds)

E1, E2 E3 E4

0.6

0.8

E1, E2. E3.

Cleaning Potential

E4.

Reconditioning Potential

Analytical Potentials

Figure 2-25. Example Integrated Amperometry Waveform

With the example waveform shown in Figure 2-25

, 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.

62 Doc. 065031-04 1/08

2.16.5 Cyclic Voltammetry Detection

Seconds

(

)

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.

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 2.16.6

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.

2.16.6 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.

2 • DC Description

Cyclic Voltammetry Waveforms

Cyclic voltammetry waveforms consist of three steps, each with a time and a potential. The waveform forms a triangle, with the first step always at time zero and the first and third steps always having the same potential.

Figure 2-26

shows an example of a triangular waveform used in cyclic

voltammetry.

0.60

0.40

0.20

0.00

0.00 5.00 10.00 15.00 20.00 25.00 30.00

olts

-0.20

-0.40

-0.60

(0.00, -0.80

-0.80

Figure 2-26. Example Cyclic Voltammetry Waveforms

14.0, 0.60

(28.0, -0.80)

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ICS-3000 Ion Chromatography System

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 ΔV×

------------------------------------Sweep Rate= CV Cycle Time

2 1.4× V

-------------------- 0.1

28s

Cyclic voltammetry waveforms are defined manually on the Chromeleon or Chromeleon Xpress electrochemical detector Control panel. Click the CV Mode button to display the following window.

Figure 2-27. Cyclic Voltammetry Control Panel

Integrated Amperometry Waveforms

---

Integrated amperometry waveforms are included in a Program file in Chromeleon or Chromeleon Xpress. 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.

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2 • DC Description

• 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.

• The integration interval generates one integrated data point per

waveform.

Chromeleon and Chromeleon Xpress provide several pre-programmed waveforms (see Figure 2-28

Figure 2-28. Pre-Programmed Waveforms

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ICS-3000 Ion Chromatography System

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 2-29

Options page to view the Waveform Editor.

). Click the Edit button on the Program Wizard: ED

Figure 2-29. Waveform Editor

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2 • DC Description

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 2-24 potentials are being applied (see the example waveform in Figure 2-25

With scanning waveforms, integration occurs while the potential is being increased linearly over time (see the example scanning waveform in

Figure 2-30

). 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 2.16.7 known substance with an unknown can help to identify unknown peaks or to determine whether a substance is coeluting with another.

1.0

) or while a series of stepped

). Comparison of I-t plots of a

Potential

(Volts)

0.0

-1.0

-2.5

0.0

0.5

E1E2. Pre-adsorption potential

. Scanning potentials

Reductive cleaning potential

E3.

. Oxidative cleaning potential

Integration

1.0

Time (Seconds)

1.5

Figure 2-30. Example Scanning Waveform

2.0

E3/E4

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ICS-3000 Ion Chromatography System

2.16.7 Storing and Reprocessing Amperometry Data

NOTE Chromeleon Xpress cannot store or reprocess

amperometry data.

Chromeleon provides storage of both 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 2-31 The retention time (in minutes) is on the x-axis and the detector response (in nanoCoulombs) is on the y-axis.

Analytical Column: CarboPac PA10 and Guard Eluent: 18 mM NaOH Flow Rate: 1.5 mL/min Detection: Pulsed Amperometry

Response (nC)

Electrode: Gold Waveform: Quadruple Potential

Peaks: 1. L-Fucose

(4 x 250 mm)

2. D-Galactosamine

3. D-Glucosamine

4. D-Galactose

5. D-Glucose

6. D-Mannose

0510

Retention Time (Minutes)

Minutes

Figure 2-31. Example Chromatogram for a Pulsed Amperometry Application

For 3D integrated 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—is collected. For details about

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2 • DC Description

how to acquire 3D amperometry data, refer to the 3D Amperometry User’s Manual (Document No. 065218).

Chromeleon displays and lets you reprocess the 3D data in the 3D Amperometry View window (see Figure 2-32 double-click the sample in the Browser to open the chromatogram. On the View menu, click 3D-Amperometry,

). To open the window,

Sample

Injection Data

I-t Plot

(current vs.

waveform

time)

Waveform

Plot

Chromatogram

Plot

3D Amperometry

Data Plot

Figure 2-32. 3D Amperometry View Window in Chromeleon

The window is divided into several display areas:

Sample injection data Displays information about the sample.

Chromatogram plot Displays a chromatogram of data selected

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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ICS-3000 Ion Chromatography System

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 2-33 y-axis is the waveform period (ms). The z-axis, which is not visible on the plot, is the response (nA).

retention time (min)

). The x-axis is the retention time (min) and the

waveform time (ms)

)

(

Figure 2-33. 3D Amperometry Data in Chromeleon: Iso View

NOTE The 3D data shown in Figures 2-33 through 2-36

was collected using an analytical waveform (see

“

Analytical vs. Scanning Waveforms” on page 67).

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

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2 • DC Description

of responses as well as the color mappings (see Figure 2-34). For this view, imagine you are standing in front and slightly to the left of the plot.

response (nA)

)

(

retention time (min)

Figure 2-34. 3D Amperometry Data in Chromeleon: 3D View

Baseline Correction

Based on the peak recognition algorithm, 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.

To enable baseline correction, select Baseline correction on the General tab page of the 3D Amperometry Decoration dialog box.

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ICS-3000 Ion Chromatography System

Figure 2-35 is an example of 3D amperometry data before baseline

correction is enabled.

Figure 2-35. 3D Amperometry Data Before Baseline Correction

Figure 2-36

Figure 2-36. 3D Amperometry Data After Baseline Correction

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shows the same data after baseline correction is enabled.

2.17 Automation Manager

The ICS-3000 Automation Manager (AM) provides a mounting location for various components used for performing matrix elimination, large volume preconcentration, post-column reagent addition, and other functions.

Each AM consists of a tray on which valves and other components are installed (see Figure 2-37

Figure 2-13

valve, reagent reservoirs, etc.) depend on the application. Refer to Chapter 3 the configuration schematic for your application.

). The tray is installed in the upper compartment of the DC (see

). Connections to other components in the system (pump, injection

2 • DC Description

for

High-Pressure Valve #1

ow-Pressure

Valve #1

High-Pressure Valve #2

ow-Pressure

Valve #2

Figure 2-37. ICS-3000 Automation Manager

The AM is available in the following configurations:

Components Included

Two 10-port high-pressure valves Two low-pressure 3-way valves

One 10-port high-pressure valve One low-pressure 3-way valve

AM Part Number

061738

061736

emperature

Stabilizer

RCH-1 Reaction Coil Heater

One 6-port high-pressure valve

061740

One low-pressure 3-way valve

AM tray with no valves 061734

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ICS-3000 Ion Chromatography System

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 (0.010-in) ID 062561

Temperature stabilizer, microbore, 0.125-mm (0.005-in) ID 062562

2.17.1 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 2-38 and Figure 2-39 valve position.

show the liquid flow path through the valve ports at each

POSITION A

POSITION B

Figure 2-38. High-Pressure Switching Valve Flow Schematics: 6-Port Valve

POSITION A

POSITION B

Figure 2-39. High-Pressure Switching Valve Flow Schematics: 10-Port Valve

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Valve port connections to chromatography components vary, depending

on the application. Refer to Chapter 3 your application.

Valves are controlled by Chromeleon or Chromeleon Xpress (see

Section 2.17.3

2.17.2 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 2-40

Valve port connections to chromatography components vary, depending on the application. Refer to Chapter 3 your application.

Valves are controlled by Chromeleon or Chromeleon Xpress (see

Section 2.17.3

2 • DC Description

for the configuration schematic for

for the system flow schematic for

FF POSITION

COM

(N.C.)

(N.O.)

N.C. = normally closed N.O. = normally open COM = common flow

N POSITION

COM

(N.C.)

(N.O.)

Note:

When the valve is off (i.e., it is not energized), port 0 is open (N.O.) and port 1 is closed (N.C.). Conversely, the valve is on, 1 is open and port 0 is closed.

when

port

Figure 2-40. Three-Way Low-Pressure Valve Flow Schematics

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ICS-3000 Ion Chromatography System

2.17.3 High- and Low-Pressure Valve Control

Chromeleon or Chromeleon Xpress is used to control the high- and lowpressure valves. Commands for valve control can be included in a program (see Figure 2-41 controlled manually from a Control panel (see Figure 2-42

) for automated control, or the valves can be

Figure 2-41. Program Wizard Relay and State Devices Options Page

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2 • DC Description

Figure 2-42. DC Control Panel

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ICS-3000 Ion Chromatography System

2.17.4 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.

Commands for heater control can be included in a program (see

Figure 2-43

manually from the DC Control panel (see Figure 2-42

) for automated control, or the heater can be controlled

Figure 2-43. Program Wizard DC Options Page

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2.18 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 2-44 pin.

2 • DC Description

describes the functions assigned to each connector

onnector

Position

1 2 3 4 5 6 7 8 9

10 11

1 2 3 4 5 6 7 8 9

10 11

Pin Function

Analog

Det 1

–

Analog

Det 2

–

+5V

–

Gnd

N.O. COM

Rly 1 N.C. N.O.

Rly 2

COM N.C.

TTL Out1

Gnd

TTL Out2

Gnd

TTL In 1

TTL In 2

TTL In 3

TTL In 4

TTL In 5

TTL In 6

TTL In 7

TTL In 8

Description

16-bit analog output from detector #2

+5 V, 200 mA

Ground

Relay contacts output Connect for either normally open (N.O.) or normally closed (N.C.)

Solid state relay contacts output Connect for either normally open (N.O.) or normally closed (N.C.)

Note:

Relays are capable of switching 2 A at 24 VDC.

TTL Output 1 (332 pull up to +5 V, 100 mA sink)

Ground

TTL Output 1 (332 pull up to +5 V, 100 mA sink)

Ground

TTL Input 1

TTL Input 2

TTL Input 3

TTL Input 4

TTL Input 5

TTL Input 6

TTL Input 7

TTL Input 8

Note:

in software.

TTL input functions are assigned

Figure 2-44. Optional Rear Panel I/O Connector Strips

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ICS-3000 Ion Chromatography System

2.18.1 I/O Option Connections

1. Locate the twisted pair of wires (P/N 043598) and 12position connector plugs (P/N 923686) (see Figure 2-45 provided with the I/O option board.

)

Position 1

Locking Screws

Position 12

2. For each I/O function

Figure 2-45. 12-Position Connector Plug

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 2-44 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 Server Configuration program (see Section 2.18.4

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2 • DC Description

2.18.2 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 2-15 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 2.18.1

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. Tab le 2- 2 the settings. You select the desired settings on the detector Control panel (see Figure 2-46

Analog Output Setting Values Description

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 fullscale voltage output of 1 V.

). The analog

describes

Range Conductivity:

0.01 to 15,000 μS

DC Amperometry: 50 pA to 300 μA

Integrated Amperometry: 50 pC to 200 μC

Table 2-2. Analog Output Configuration Settings

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Sets the full-scale detector response value. The range to use depends on the detector readings expected for the application. For example, selecting a range of 20 microSiemens (μS) will limit you to viewing conductivity readings of 20 μS or less.

ICS-3000 Ion Chromatography System

Analog Output Setting Values Description

Recorder calibration Zero, Full Scale,

Normal

Offset level 0 to 100% Use this setting to adjust the zero

Polarity Positive, Negative Use this setting to set the polarity of

Use this setting to calibrate a 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.

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.

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

analog output

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

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Use this setting to send a positive pulse to the analog output as an event marker. A mark is typically used to indicate a sample injection.

2 • DC Description

Figure 2-46. Conductivity Detector Control Panel

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ICS-3000 Ion Chromatography System

2.18.3 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 2-47 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.

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 2.18.1

connection instructions.

and the documentation for the external device for

RELAY OUTPUT CONFIGURATION

Rear Panel

Pins

N.O.

COM

N.C.

N.O.

COM

N.C.

Relay Output

(on DC Electronics)

Non-Energized Relay

Energized Relay

Figure 2-47. Relay Output Configuration

NOTE

The relays are capable of switching 2 A at 24 VDC.

For a normally open connection, connect a COM pin and an N.O. pin.

For a normally closed connection, connect a COM pin and an N.C. pin.

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Dionex ICS-3000 Operator's Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1.1 ICS-3000 System Overview

1.1.1 ICS-3000 System Components

1.1.2 ICS-3000 System Control

1.2 ICS-3000 System Documentation

1.3 The ICS-3000 System Operator’s Manual

1.3.1 Overview

1.3.2 Safety Messages and Notes

1.4 Safety and Regulatory Information

1.4.1 Safety Labels

DP/SP Description

2.1 DP/SP Front Features

2.2 DP/SP Interior Components

2.2.1 Pump Heads

2.2.2 Pressure Transducer

2.2.3 Proportioning Valves (Gradient pump only)

2.2.4 Vacuum Degassing Module

2.2.5 Piston Seal Wash System

2.2.6 Static Mixer

2.3 DP/SP Flow Schematics

2.3.1 Isocratic Pump Flow Schematic

2.3.2 Gradient Pump Flow Schematic

2.4 DP/SP Rear Panel

2.5 Eluent Reservoirs

2.6 EO (Optional)

EG Description

2.7 EG Front Features

2.8 EG Interior Components

2.9 EG Rear Panel

2.10 EG Flow Schematic

DC Description

2.11 DC Front Features

2.12 DC Interior Components

2.13 DC Rear Panel

2.14 Injection Valves

2.14.1 Injection Valve Operation

2.14.2 Injection Valve Plumbing

2.15 CD Conductivity Detector

2.15.1 Heated Conductivity Cell

2.15.2 Suppressor

2.15.3 System Flow Schematic for Conductivity Detection

2.16 ED Electrochemical Detector

2.16.1 Amperometry Cell

2.16.3 DC Amperometric Detection

2.16.4 Integrated and Pulsed Amperometric Detection

2.16.5 Cyclic Voltammetry Detection

2.16.6 Waveforms

2.16.7 Storing and Reprocessing Amperometry Data

2.17 Automation Manager

2.17.1 High-Pressure Switching Valves

2.17.2 Low-Pressure Valves

2.17.3 High- and Low-Pressure Valve Control

2.17.4 RCH-1 Reaction Coil Heater

2.18 I/O Option

2.18.1 I/O Option Connections

2.18.2 Analog Outputs

2.18.3 Power, Relay, and TTL Outputs