Oritron ICS-2100 User Manual

ICS-2100 Ion Chromatography System

Operator’s Manual

Document No. 065291

Revision 01 March 2009

This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transmitte d, tr anscribed, 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 Dione x 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 T HE USE, OF THIS PUBLICA TION 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, AMMS ICE, ASRS, Chromeleon, EluGen, IonPac, OnGuard, and SRS are registered trademarks of Dionex Corporation. AutoNeutraliz ation, MicroMembran e, MMS, and MonoDisk are trademarks of Dionex Corporation. Acrobat, Adobe, and Adobe Reader are registered trademarks of Adobe Systems, Incorporated. Microsoft and Windows Vista are registered trademarks of Microsoft Corporation. PEEK is a trademark of Victrex PLC. Teflon is a registered trademark of E.I. duPont de Nemours & Company.

PRINTING HISTORY

Revision 01, March 2009

1 • Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.1 Introduction to Ion Chromatography (IC) . . . . . . . . . . . . . . . . . . . . . . . . 1

1.2 Overview of the ICS-2100 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

1.3 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

1.3.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

1.4.1 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

2 • Features. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.1.1 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.1.2 Top Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

2.1.3 Component Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

2.1.4 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

2.2 Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

2.3 Chromeleon and Chromeleon Xpress . . . . . . . . . . . . . . . . . . . . . . . . . . 30

2.3.1 The Panel Tabset . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

2.3.2 Software Control Modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

2.3.3 System Wellness . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

2.4 System Component Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

2.4.1 Vacuum Degas Assembly (Optional) . . . . . . . . . . . . . . . . . . . . 32

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2.4.2 Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34

2.4.3 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34

2.4.4 Eluent Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

2.4.5 Auxiliary Power Supply (Optional) . . . . . . . . . . . . . . . . . . . . . .42

2.4.6 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42

2.4.7 Auxiliary Valve (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . .44

2.4.8 Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .45

2.4.9 Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46

2.4.10 DS6 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . 46

3 • Operation and Maintenance . . . . . . . . . . . . . . . . . . . . . . . .49

3.1 Operation Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

3.2 Turning On the System Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .51

3.3 Connecting to Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .52

3.4 Set Up the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .54

3.4.1 Filter the Deionized Water . . . . . . . . . . . . . . . . . . . . . . . . . . . .54

3.4.2 Fill the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .54

3.4.3 Set the Eluent Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .54

3.4.4 Connect the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .56

3.5 Check All Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

3.6 Prime the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .57

3.7 Set System Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .58

3.8 Equilibrate the System and Verify Operational Status . . . . . . . . . . . . .59

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3.9 Prepare Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

3.9.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . . . 60

3.9.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

3.9.3 Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

3.10 Loading and Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

3.10.1 Loading Samples with a Syringe . . . . . . . . . . . . . . . . . . . . . . . 63

3.10.2 Loading Samples with a Vacuum Syringe . . . . . . . . . . . . . . . . 64

3.10.3 Loading Samples with an Autosampler . . . . . . . . . . . . . . . . . . 64

3.10.4 Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

3.11 Processing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

3.11.1 Manual Sample Processing . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

3.11.2 Automatic (Batch) Sample Processing . . . . . . . . . . . . . . . . . . . 66

3.12 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

4 • Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

4.1 Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

4.2 Troubleshooting Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

4.3 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

4.4 Pump Difficult to Prime or Loses Prime . . . . . . . . . . . . . . . . . . . . . . . . 88

4.5 Pump Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90

4.6 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90

4.7 Erratic Flow/Pressure Reading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

4.8 Excessive System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92

4.9 Peak “Ghosting” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

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ICS-2100 Ion Chromatography System

4.10 Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . . .94

4.11 Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . . . .94

4.12 No Cell Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .94

4.13 High Cell Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95

4.14 Baseline Noise or Drift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .96

4.15 Vacuum Degas Assembly Does Not Run . . . . . . . . . . . . . . . . . . . . . . . .97

5•Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99

5.1 Diagnostic and Calibration Procedures . . . . . . . . . . . . . . . . . . . . . . . . .99

5.1.1 Chromeleon Wellness Panel Overview . . . . . . . . . . . . . . . . . .100

5.1.2 Diagnostic and Calibration Touch Screen Overview . . . . . . .102

5.1.3 Calibrating the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . .103

5.1.4 Calibrating the Flow Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . .106

5.1.5 Calibrating the Vacuum Degas Assembly . . . . . . . . . . . . . . . .108

5.2 Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . . .109

5.3 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .113

5.4 Rebuilding the Injection Valve or Auxiliary Valve . . . . . . . . . . . . . . .114

5.5 Replacing an Auxiliary Valve Pod . . . . . . . . . . . . . . . . . . . . . . . . . . . .116

5.6 Cleaning and Replacing the Pump Check Valves . . . . . . . . . . . . . . . .118

5.7 Replacing a Pump Piston Seal and Piston Rinse Seal . . . . . . . . . . . . .120

5.8 Replacing a Pump Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .124

5.9 Replacing the Waste Valve or Priming Valve O-Ring . . . . . . . . . . . . .125

5.10 Replacing the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127

5.11 Replacing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .130

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5.12 Replacing the Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

5.13 Replacing the Column Heater Heat Exchanger . . . . . . . . . . . . . . . . . . 134

5.14 Replacing the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135

5.15 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137

5.16 Priming the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138

5.16.1 Priming the Eluent Lines with a Syringe . . . . . . . . . . . . . . . . 138

5.16.2 Priming with the Prime Button . . . . . . . . . . . . . . . . . . . . . . . . 140

5.17 Priming the Pump with Isopropyl Alcohol . . . . . . . . . . . . . . . . . . . . . 141

5.18 Changing Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142

5.19 Replacing an EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143

5.19.1 Replacing a KOH, LiOH, MSA, or NaOH

EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143

5.19.2 Replacing a K2CO3 Cartridge . . . . . . . . . . . . . . . . . . . . . . . . 151

5.20 Replacing the CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165

5.21 Replacing the EPM Electrolytic pH Modifier . . . . . . . . . . . . . . . . . . . 169

5.21.1 Recording the EPM Serial Number in Chromeleon . . . . . . . . 170

5.21.2 Plumbing the EPM for Hydrating and Conditioning . . . . . . . 171

5.21.3 Hydrating and Conditioning the EPM . . . . . . . . . . . . . . . . . . 173

5.22 Replacing the EGC CO3 Mixer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174

5.22.1 Installing the New EGC CO3 Mixer . . . . . . . . . . . . . . . . . . . 174

5.22.2 Filling the EGC CO3 Mixer with Deionized Water . . . . . . . . 175

5.22.3 Filling the EGC CO3 Mixer with Eluent . . . . . . . . . . . . . . . . 178

5.23 Replacing the EGC Holder and Degas Assembly . . . . . . . . . . . . . . . . 185

5.23.1 Disconnecting and Removing the EluGen Cartridge . . . . . . . 185

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5.23.2 Removing the CR-TC and Reinstalling it

in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . .188

5.23.3 Removing the EPM and Reinstalling it

in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . .190

5.23.4 Installing the New EGC Holder Without a CR-TC

or EPM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .192

5.23.5 Reinstalling the EluGen Cartridge . . . . . . . . . . . . . . . . . . . . . .193

A • Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .195

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .195

A.2 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .195

A.3 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .196

A.4 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .196

A.5 Analytical Pump and Fluidics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .196

A.6 Eluent Generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .198

A.7 Detector Electronics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .200

A.8 Conductivity Cell with Heat Exchanger . . . . . . . . . . . . . . . . . . . . . . . .200

A.9 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .202

A.10 Auxiliary Valve (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .202

A.11 Vacuum Degas Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .202

A.12 Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .202

A.13 Auxiliary Power Supply (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . .202

A.14 Suppressors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .203

A.15 Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .204

A.16 System Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .204

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B • Touch Screen Operation. . . . . . . . . . . . . . . . . . . . . . . . . . . 207

B.1 Using the Touch Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 207

B.2 Using the Touch Screen with Chromeleon . . . . . . . . . . . . . . . . . . . . . 210

B.3 Overview of ICS-2100 Touch Screen Pages . . . . . . . . . . . . . . . . . . . . 211

B.4 Home Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 212

B.4.1 Home Page Pump Controls . . . . . . . . . . . . . . . . . . . . . . . . . . 212

B.4.2 Home Page EGC Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . 214

B.4.3 Home Page Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . 214

B.4.4 Home Page Injection Valve Controls . . . . . . . . . . . . . . . . . . . 215

B.4.5 Home Page Detector Controls . . . . . . . . . . . . . . . . . . . . . . . . 215

B.4.6 Other Home Page Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . 216

B.5 Plot Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 217

B.6 Status Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218

B.6.1 Viewing Other Status Parameters . . . . . . . . . . . . . . . . . . . . . . 220

B.6.2 Status Parameter Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 221

B.7 Pump Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 223

B.7.1 Setting Pump Pressure Limits and Selecting

the Pressure Unit 223

B.7.2 Setting Degas Operating Parameters (Optional) . . . . . . . . . . 224

B.7.3 Controlling the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . 225

B.8 Eluent Generator Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 226

B.8.1 EGC Serial Number . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 226

B.8.2 Setting the Eluent Concentration . . . . . . . . . . . . . . . . . . . . . . 227

B.8.3 Controlling the Eluent Generator Power . . . . . . . . . . . . . . . . 228

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B.8.4 Monitoring the EluGen Cartridge Life . . . . . . . . . . . . . . . . . .228

B.8.5 Controlling the CR-TC Power . . . . . . . . . . . . . . . . . . . . . . . . .229

B.9 Suppressor Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .230

B.10 Detector Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .231

B.10.1 Setting the Data Rise Time . . . . . . . . . . . . . . . . . . . . . . . . . . .232

B.10.2 Selecting the Conductivity Polarity . . . . . . . . . . . . . . . . . . . . .232

B.10.3 Setting Analog Out Options . . . . . . . . . . . . . . . . . . . . . . . . . .233

B.11 Information Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .234

B.12 Module Setup Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .235

B.13 Input/Output Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .236

B.14 Diagnostic and Calibration Pages . . . . . . . . . . . . . . . . . . . . . . . . . . . . .236

C • TTL and Relay Control. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .239

C.1 TTL and Relay Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .239

C.1.1 Selecting TTL Input Functions and Control Types . . . . . . . . .242

C.2 Controlling TTL and Relay Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . .245

C.3 Example Setup for Stand-Alone Operation . . . . . . . . . . . . . . . . . . . . .246

D • Reordering Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . .251

E•FAQ. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .255

E.1 How do I hook up an autosampler? . . . . . . . . . . . . . . . . . . . . . . . . . . .255

E.2 How do I print? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .255

E.3 Why are the retention times moving? . . . . . . . . . . . . . . . . . . . . . . . . . .255

viii Doc. 065291-01 3/09

Contents

E.4 How do I adjust retention times? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255

E.5 When should I remake standards? . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255

E.6 When should I replace the eluent generator cartridge? . . . . . . . . . . . 256

E.7 How do I start Chromeleon? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

E.8 How do I delete data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

E.9 How do I back up data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

E.10 How do I shut off the system? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

E.11 How do I store columns? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

E.12 How do I know when a column is dirty? . . . . . . . . . . . . . . . . . . . . . . . 257

E.13 How do I clean a column? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257

E.14 Why is the conductivity high? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257

E.15 How do I configure and operate the auxiliary valve? . . . . . . . . . . . . . 257

F • Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259

Index

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ICS-2100 Ion Chromatography System

x Doc. 065291-01 3/09

1 • Introduction

1.1 Introduction to Ion Chromatography (IC)

The Dionex ICS-2100 Ion Chromatography System (ICS-2100) performs ion

analyses using suppressed or non-suppressed conductivity detection. An ion

chromatography system typically consists of a liquid eluent, a high-pressure

pump, a sample injector, a guard and separator column, a chemical suppressor, a

conductivity cell, and a data collection system.

Before running a sample, the ion chromatography system is calibrated using a

standard solution. By comparing the data obtained from a sample to that obtained

from the known standard, sample ions can be identified and quantitated. The data

collection system, typically a computer running chromatography software,

produces a chromatogram (a plot of the detector output vs. time). The

chromatography software converts each peak in the chromatogram to a sample

concentration and produces a printout of the results.

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ICS-2100 Ion Chromatography System

A typical IC analysis consists of six stages (see Figure 1-1).

. Data Analysis

Conductivity

Cell

Suppressor

5. Detectio

1. Eluent

Eluent

Delivery

Pump

2. Sample Injection

1. Eluent Delivery

• Eluent, a liquid that helps to separate the sample ions, carries the

sample through the ion chromatography system. The ICS-2100 includes an eluent generator, which generates eluent online from deionized water.

• When the ICS-2100 is controlled from the front panel, only isocratic

eluent delivery is possible. This means that the eluent composition and concentration remain constant throughout the run. Gradient delivery (a change in concentration over time) is possible when the ICS-2100 is controlled by Chromeleon Management System (the data collection system for the ICS-2100).

4. Suppression

Separator

Column

3. Separation

Guard Column

Injection

Valve

Sample Loop

Sample

Figure 1-1. Ion Analysis Process

Chromatography

2. Sample Injection

• The liquid sample is loaded into a sample loop either manually or

automatically (if an automated sampler is installed). When triggered, the ICS-2100 injects the sample into the eluent stream.

2 Doc. 065291-01 3/09

• The pump pushes the eluent and sample through the guard and

separator columns (chemically-inert tubes packed with a polymeric resin). The guard column removes contaminants that might poison the separator column.

3. Separation

• As the eluent and sample are pumped through the separator column,

the sample ions are separated. In the ICS-2100, the mode of separation is called ion exchange. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites.

4. Suppression

• After the eluent and sample ions leave the column, they flow through

a suppressor that selectively enhances detection of the sample ions while suppressing the conductivity of the eluent.

5. Detection

• A conductivity cell measures the electrical conductance of the sample

ions as they emerge from the suppressor and produces a signal based on a chemical or physical property of the analyte.

1 • Introduction

6. Data Analysis

• The conductivity cell transmits the signal to a data collection system.

• The data collection system (for the ICS-2100, this is the

Chromeleon ions based on retention time, and quantifies each analyte by integrating the peak area or peak height. The data is quantitated by comparing the sample peaks in a chromatogram to those produced from a standard solution. The results are displayed as a chromatogram and the concentrations of ionic analytes can be automatically determined and tabulated.

Doc. 065291-01 3/09 3

Chromatography Management System) identifies the

ICS-2100 Ion Chromatography System

1.2 Overview of the ICS-2100

The ICS-2100 is an integrated ion chromatography system containing an eluent generator, pump, injection valve, column heater, and conductivity detector. Other system components, including a guard column, separator column, and suppressor vary, depending on the analyses to be performed.

The ICS-2100 can be configured with a vacuum degas assembly for online eluent degassing. If desired, the second eluent generator power supply can be configured to power an auxiliary electrolytic device, such as a water purifier.

An optional second high-pressure valve (6-port or 10-port) can be installed for sample preparation applications.

ICS-2100 operation can be controlled in one of two ways:

• Remotely, with a personal computer running Microsoft

Windows XP and Chromeleon software (version 6.80 SR6a or later). Chromeleon also provides data acquisition and data processing functions.

• Locally, with the front panel LCD touch screen. The touch screen is used for

instrument control only. It does not provide data acquisition or data processing functions. An analog output on the rear panel can be connected to a separate data acquisition device.

Windows®Vista or

For communication between the ICS-2100 and Chromeleon, the ICS-2100 is connected to a USB (Universal Serial Bus) port on the computer or a USB hub. For details, see the ICS-2100 installation instructions. Also refer to Installing the

Chromeleon Chromatography Management System with a Dionex Ion Chromatograph (IC) (Document No. 031883).

4 Doc. 065291-01 3/09

1.3 About This Manual

The electronic version (i.e., PDF file) of this 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.

1 • Introduction

If you are not familiar with how to navigate PDF files, refer to the Help system for Adob

e® Acrobat® or Adobe Reader

Chapter 1 Introduction

Introduces ion analysis and the ICS-2100; explains the conventions used in this manual, including safety-related

for assistance

information.

Chapter 2 Features

Provides an overview of ICS-2100 operating features and system components; introduces the Chromeleon user interface.

Chapter 3 Operation and Maintenance

Chapter 4 Troubleshooting

Chapter 5 Service

Appendix A Specifications

Appendix B Touch Screen Operation

Appendix C TTL and Relay Control

Appendix D Reordering Information

Provides operating instructions and describes routine preventive maintenance procedures.

Lists problems, and presents step-by-step procedures for how to isolate and eliminate the cause of each problem.

Provides step-by-step instructions for routine service and parts replacement procedures that the user can perform.

Lists the ICS-2100 specifications and installation site requirements.

Describes the operating features available from the front panel touch screen.

Describes the ICS-2100 TTL and relay control features.

Lists spare parts for the ICS-2100.

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ICS-2100 Ion Chromatography System

Appendix E FAQ

Appendix F

Provides answers to frequently asked questions about ICS2100 operation.

Defines terms commonly used in ion analysis.

Glossary

1.3.1 Safety Messages and Notes

This manual contains warnings and precautionary statements that, when properly followed, can prevent personal injury and/or damage to the instrument. 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, bu t will not c ause injury.

Indicates that the function or process of the instrument may be impaired. Operation does not constitute a hazard.

Messages d'avertissement en français

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

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

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

6 Doc. 065291-01 3/09

1 • Introduction

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.

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.

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ICS-2100 Ion Chromatography System

1.4 Safety and Regulatory Information

The ICS-2100 was manufactured by Dionex Corporation at the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The ICS-2100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. If there is a question regarding appropriate usage, contact Dionex at 1-800-346-6390 before proceeding. Outside the United States, call the nearest Dionex office.

1.4.1 Safety Labels

The TUV T-Mark and cTUVus Mark safety labels and the CE Mark label on the system indicate that it is in compliance with the following standards:

EMC Susceptibility and Emissions

• EN 61326-1:2006

Safety

• CAN/CSA-C22.2 61010-1:2004

• UL 61010-1:2004

• EN 61010-1:2001

The symbols below appear on the ICS-2100 or on labels affixed to the ICS-2100.

Alternating current

Primary protective conductor terminal

Secondary protective conductor terminal

8 Doc. 065291-01 3/09

1 • Introduction

Power supply is on

Power supply is off

Hot surface

Indicates a potential hazard. Refer to the operator’s manual for an explanation of the hazard and how to proceed.

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ICS-2100 Ion Chromatography System

10 Doc. 065291-01 3/09

This chapter describes key ICS-2100 features and introduces the Chromeleon user interface.

2.1 Operating Features

2.1.1 Front Panel

Figure 2-1 illustrates the front panel of the ICS-2100.

Touch

Screen

Power

LED

Injection

Port

2•Features

Injection Port

The sample to be analyzed can be injected manually into the injection port, using a syringe. For automated sample injection, the ICS-2100 must be connected to an autosampler. For more information about sample injection, see

Section 3.10

Touch Screen

The LCD touch screen provides local control of most ICS-2100 functions. Yo u can control many of these functions directly on the touch screen’s

HOME page (see Figure 2-2).

From the also go to a series of pages that provide access to all other locally controlled ICS-2100 operating functions.

HOME page, you can

Figure 2-1. ICS-2100 Front Panel

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ICS-2100 Ion Chromatography System

Summary of Touch Screen Operation

Edit Field

Command

Button

(selected)

Command

Button

(unselected)

Figure 2-2. ICS-2100 Touch Screen Home Page

Status Field

NOTE To adjust the screen contrast, open the front door and

adjust the knurled knob under the screen (see

Figure 2-8

• Edit fields and command buttons have blue text on a shaded

background. Fields that display status information are not shaded.

• Edit fields have square corners, while command buttons are rounded.

• To select a command button or edit a field, touch and release the

command button or edit field with your fingertip.

NOTE When you touch a button or edit field, the action is

taken when you lift your finger. If you unintentionally touch a button or field, you can cancel the action by sliding your finger away from the button or field before lifting.

• Touching a command button (for example, ) executes the

command immediately.

12 Doc. 065291-01 3/09

2 • Features

• Selecting a command button changes the button’s appearance to

white text on a dark backgound (for example, ).

• Touching an edit field (for example, ) opens a page

with a number keypad (see Figure 2-3 desired numerical value for the field and then touch the button.

Touch a

number to

enter the

value.

). Use the keypad to enter the

ENTER

Touch CANCEL to cancel the entry and return to the previous page.

Touch ENTER to confirm the entry and return to the previous page.

Figure 2-3. Number Keypad

Doc. 065291-01 3/09 13

ICS-2100 Ion Chromatography System

• Touching the page name (for example, ) in the

bottom right corner opens a menu of pages (see Figure 2-4

Figure 2-4. ICS-2100 Touch Screen Menu of Pages

Touch a page name to display the page.

• Touching a page name on the menu of p ages displays the selected

page. For example, touching

SUPPRESSOR displays the

14 Doc. 065291-01 3/09

Touch to

return to the

Home page.

2 • Features

SUPPRESSOR page (see Figure 2-5). See Appendix B for details

about each touch screen page.

Touch to select a different option.

Figure 2-5. Suppressor Page

• Touching returns you to the HOME page.

• Touching opens a list of options (see Figure 2-6).

Figure 2-6. Suppressor Page: Selecting an Option

Touch an option to select it.

Doc. 065291-01 3/09 15

ICS-2100 Ion Chromatography System

2.1.2 Top Cover

Figure 2-7 illustrates the top cover of the ICS-2100.

EGC, EPM,

CR-TC, and

Auxiliary

Power

Supply

Connectors

Tubing

Chase

(under

connectors)

EGC Service

Area

Figure 2-7. ICS-2100 (Top View)

EluGen Cartridge and Holder

Second EluGen Cartridge or Reservoir Area

Deionized Water

4 L Reservoir Area

EluGen Cartridge and Reservoir Storage

The top cover holds one or two

EluGen

cartridges and up to two 2-L plastic reservoirs (P/N 044129) or one 4-L plastic reservoir (P/N 039164).

EluGen Cartridges

The EluGen cartridges are installed in holders that fit into the two back reservoir areas. See Section 2.4.4

for details

about the eluent generator.

Tubing Chase

The tubing chase under the EGC and CR-TC connectors routes tubing from the eluent reservoir and EGC holder to the front of the ICS-2100.

EGC, EPM, CR-TC, and Auxiliary Power Supply Connectors

The cable from the EluGen cartridge (EGC) connects to the EGC-1 connector. The cable from the Continuously Regenerated Trap Column (CR-TC) connects to the installed, it connects to the

CR-TC connector. If a second EluGen cartridge is

EGC-2 connector. If the second eluent

generator power supply is configured to power an auxiliary electrolytic device, it connects to the

EGC-2 connector. For details, refer to the ICS-

2100 installation instructions. When operating with an EGC II K

EluGen Cartridge and the EPM

2CO3

Electrolytic pH Modifier, the EluGen cartridge is typically connected to the

EGC-1 connector. The pH modifier, which mounts on the side of the

16 Doc. 065291-01 3/09

2 • Features

EluGen cartridge holder, is connected to the EGC-2 connector. However, the connections can be reversed, if desired.

EGC Service Area

The EGC service area holds the cartridge during installation and replacement. For details, refer to the ICS-2100 installation instructions.

Doc. 065291-01 3/09 17

ICS-2100 Ion Chromatography System

2.1.3 Component Panel

Figure 2-8 shows the use r-accessible components installed on the

component panel behind the ICS-2100 front door.

Pressure Transducer

Leak Sensor

Pump Heads

Injection Valve

Auxiliary Valve

(Optional)

DS6 Conductivity Cell

Suppressor

Column Heater and

Columns

Eluent Valve

Mounting Brackets for

Second Suppressor

Screen Adjustment

Knob (under display) Tubing Chase (2)

Figure 2-8. ICS-2100 Component Panel

18 Doc. 065291-01 3/09

2 • Features

Pressure Transducer

The pressure transducer measures the system backpressure.

Leak Sensor

The leak sensor is installed in the drip tray at the bottom of the component panel. If liquid accumulates in the tray, an error message is logged in the Chromeleon Audit Trail and displayed on the LCD touch screen.

Pump Heads

The ICS-2100 includes a dual-piston serial pump. The flow rate can be set to 0.00 mL/min or to between 0.05 and 5.00 mL/min. However, for optimum performance, set the flow rate to between 0.40 and

2.00 mL/min. Setting the flow rate to 0.00 mL/min turns off the pump. See Section 2.4.3

Injection Valve

The injection valve is a six-port, electrically-activated Rheodyne valve. A 25-μL sample loop (P/N 042857) is installed on the valve at the factory. See Section 2.4.6

for details about the pump.

for details about valve operation.

Auxiliary Valve (Optional)

The auxiliary valve is a two-position, electrically-activated Rheodyne valve (6-Port Valve Kit, P/N 069472; 10-Port Valve Kit, P/N 069473). See Section 2.4.6

DS6 Heated Conductivity Cell

for details about valve operation.

The flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. A heat exchanger inside the cell regulates the temperature, which can be set to between 30 and 55 °C. For optimum performance, set the temperature to at least 7 °C above the ambient temperature and 5 °C above the column oven temperature. See

Section 2.4.10

Doc. 065291-01 3/09 19

for details about the cell.

ICS-2100 Ion Chromatography System

Suppressor

The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity.

Either an AES Suppressor, or MMS

the ICS-2100. See Section 2.4.9

Separator and Guard Columns

Both the separator and guard columns are packed with resin and perform the separation of the sample ions. The main function of the guard column is to trap contaminants and remove particulates that might damage the separator column.

Column Heater

The column heater controls the temperature of the separator and guard columns. The temperature can be set to between 30 and 60 °C; howev er, it must be set to at least 5 °C above the ambient temperature. See

Section 2.4.8

Atlas Electrolytic Suppressor, SRS® Self-Regenerating

™

MicroMembrane™ Suppressor can be used with

for details about the column heater.

for details about the suppressor.

Eluent Valve

The eluent valve controls the flow from the eluent reservoir. The eluent valve opens automatically when the pump is started and closes when the pump is turned off.

Screen Adjustment Knob

Use this knob to change the LCD touch screen contrast.

Tubing Chases

The upper tubing chase routes tubing from the top cover to the component panel. The lower tubing chase routes tubing from the component panel, through the interior of the ICS-2100, to the rear panel.

20 Doc. 065291-01 3/09

2 • Features

2.1.4 Rear Panel

Figure 2-9 illustrates the ICS-2100 rear panel.

Tubing Clips

Analog Output Connector

Power Switch

USB Connectors

Main Power

Receptacle

TTL and Relay Connector Strip

Waste Lines

Figure 2-9. ICS-2100 Rear Panel

Analog Output Connector

The analog output connector outputs conductivity data (as a 0 to 1 V signal) to an integrator or recording device. For connection and setup information, refer to the ICS-2100 installation instructions.

USB Connectors

A USB receptacle is provided to allow connection to the Chromeleon computer. Two USB ports are provided for connecting to other USB devices. For connection instructions, refer to the ICS-2100 installation instructions.

Doc. 065291-01 3/09 21

ICS-2100 Ion Chromatography System

TTL and Relay Connector

The TTL and Relay connector strip provides two TTL outputs, two relay outputs, and four TTL inputs. The outputs can be used to control functions in other TTL- or relay-controllable devices. The inputs can be used to switch the injection valve position, turn on the pump, perform an autozero command, and send an event mark to the analog output. See

Section C.1

Tubing Chases

The lower chase routes tubing from the rear panel to the component panel.

Tubing Clips

The tubing clips hold tubing routed from the top cover in place.

Power Switch

The power switch provides on/off control of power to the ICS-2100.

for connection instructions.

Main Power Receptacle

The power supply cord plugs into the AC power receptacle.

The power supply cord is used as the main disconnec t device. Make sure the socket-outlet is located near the ICS-2100 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.

22 Doc. 065291-01 3/09

2.2 Flow Schematics

• Figure 2-10 illustrates the liquid flow path when the components required for

producing KOH, LiOH, MSA, or NaOH eluent are installed. The required components include the corresponding type of EluGen cartridge and a CRTC.

• Figure 2-11 illustrates the liquid flow path when the components required for

producing carbonate/bicarbonate eluent are installed. The required components include an EGC II K Electrolytic pH Modifier, and an EGC CO

• Figure 2-12 illustrates the liquid flow path when the components required for

producing carbonate eluent are installed. The required components include an EGC II K

EluGen Cartridge and an EGC CO3 Mixer.

2CO3

EluGen Cartridge, an EPM

2CO3

Mixer.

2 • Features

Doc. 065291-01 3/09 23

ICS-2100 Ion Chromatography System

To the pump Degas In

From the

pulse

damper

To the

inject valve

port P(2)

EGC II

KOH, LiOH,

MSA, or

NaOH

Inlet Outlet

EGC

Degas

Degas In

Degas Out

Conductivity

Cell

Cell In

Cell Out

EGC Vent

Eluent

Regen In

CR-TC

Suppressor

Regen In

Deionized

Water

Regen Out

Out

Eluent

Column

Heater

Heat Exchanger

Eluent Out

Back-

pressure

Coil

Sample in

Pulse Damper

Valve

To waste

Pump

Head

Press.

Xducer.

Pump Head

Eluent

Valve

Separator

Guard

To waste

To Gas Separator Assembly

Figure 2-10. ICS-2100 Flow Schematic: KOH, LiOH, MSA, or NaOH Eluent Generation

24 Doc. 065291-01 3/09

2 • Features

Flow Description for KOH, LiOH, MSA, or NaOH Eluent Generation

Refer to Figure 2-10 for the flow path number locations.

• Deionized water from the reservoirn flows first through the pump degas

assembly and then through the eluent valve then pushed through the pressure transducer pressure. From there, the water flows through a pulse damper smooths minor pressure variations from the pump to minimize baseline noise.

o to the pumpp. The water is

q, which measures the system

r, which

• Water then flows into the EluGen cartridge (EGC)s, which generates the

programmed concentration of eluent. Eluent exits the cartridge and flows through the CR-TC degas tubing assembly

t(which traps ionic contaminants), through the EGC

u, and on to the injection valvev.

• After sample is loaded into the sample loopw and the injection valve is

toggled to the Inject position, eluent passes through the sample loop.

• Th e elu e nt/sa mp le mixture is pumped through the heat exchanger , which

heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns and through the suppressor .

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

are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously.

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

where it is the water source for the regenerant chamber.

• Regenerant waste from the suppressor is directed back to the CR-TC , and

then to the EGC degas tubing , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste .

Doc. 065291-01 3/09 25

ICS-2100 Ion Chromatography System

To the pump Degas In

EGC II

2CO3

Inlet Outlet

Eluent Out

Deionized

Water

EGC Vent

Sample in

Pulse Damper

Valve

To waste

EGC

Degas

Degas In

Degas Out

Conductivity

Cell

Cell In

Cell Out

Pump

Head

Eluent

Valve

Regen Out

Press.

Xducer.

Eluent In

Eluent In Regen In

Suppressor

Pump Head

Back-

pressure

Coil

Regen In

Regen Out Eluent Out

EPM

Column

Heater

Heat Exchanger

Guard

EGC CO

Separator

Mixer

To waste

To Gas

Separator Assembly

Figure 2-11. ICS-2100 Flow Schematic: Carbonate/Bicarbonate Eluent Generation

26 Doc. 065291-01 3/09

2 • Features

Flow Description for Carbonate/Bicarbonate Eluent Generation

Refer to Figure 2-11 for the flow path number locations.

• Deionized water from the reservoirn flows first through the pump degas

o to the pumpp. The water is

q, which measures the system

r, which

• Water then flows into the EluGen cartridge (EGC)s, which generates the

programmed concentration of carbonate eluent. Eluent exits the cartridge and flows through the EPM

t, which adjusts the eluent concentration to produce

the carbonate/bicarbonate mixture. The mixture flows through the EGC degas tubing assembly carbonate/bicarbonate mixture), and then on to the injection valve

u to the EGC CO

Mixerv (to ensure a homogenous

• After sample is loaded into the sample loop and the injection valve is toggled

to the Inject position, eluent passes through the sample loop.

• The eluent/sample mixture is pumped through the heat exchanger , which

heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns and through the suppressor .

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

are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously.

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

where it is the water source for the regenerant chamber.

• Regenerant waste from the suppressor is directed back to the EPM , and

then to the EGC degas tubing , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste .

Doc. 065291-01 3/09 27

ICS-2100 Ion Chromatography System

To the pump Degas In

EGC II K

2CO3

Inlet Outlet

EGC

Degas

Deionized

Water

EGC Vent

Degas In

Column

Heater

Heat Exchanger

Degas Out

Conductivity

Cell

Cell In

Eluent I n Regen In

Suppressor

Regen Out Eluent Out

Cell Out

EGC CO

Mixer

Separator Assembly

Sample in

Pulse Damper

Valve

To waste

Pump Head

Eluent

Valve

Press.

Xducer.

Pump

Head

Back-

pressure

Separator

Guard

Coil

Figure 2-12. ICS-2100 Flow Schematic: Carbonate Eluent Generation

To waste

To Gas

28 Doc. 065291-01 3/09

2 • Features

Flow Description for Carbonate Eluent Generation

Refer to Figure 2-12 for the flow path number locations.

• Deionized water from the reservoirnflows first through the pump degas

o to the pumpp. The water is

q, which measures the system

r, which

• Water then flows into the EluGen cartridge (EGC)s, which generates the

programmed concentration of carbonate eluent. Eluent exits the cartridge and flows through the EGC degas tubing assembly EGC CO on to the injection valve

Mixeru (to ensure a homogenous eluent concentration), and then

t. Eluent then goes to the

• After sample is loaded into the sample loopw and the injection valve is

toggled to the Inject position, eluent passes through the sample loop.

• The eluent/sample mixture is pumped through the heat exchanger , which

heats the mixture to the column heater temperature. The mixture then goes to the guard and separator columns and through the suppressor .

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

are detected. A digital signal is sent to Chromeleon software. Analog output can be collected simultaneously.

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

where it is the water source for the regenerant chamber.

• Regenerant waste from the suppressor is directed back to the EGC degas

tubing , where any released hydrogen or oxygen gas is removed before it is sent to the gas separator assembly and then to waste .

Doc. 065291-01 3/09 29

ICS-2100 Ion Chromatography System

2.3 Chromeleon and Chromeleon Xpress

The ICS-2100 is controlled by a PC configured with Chromeleon Chromatography Management System or Chromeleon Xpress. Chromeleon Chromatography Management System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of Dionex chromatography instruments, bu t does not inclu de data management capabilities.

2.3.1 The Panel Tabset

The Chromeleon and Chromeleon Xpress panel tabset provides a centralized location for controlling system functions. A panel tabset for an ICS-2100 system typically includes the following Control panels:

• An ICS-2100 Control panel (see Figure 2-13) provides access to ICS-

2100 functions. The label on the tab for this panel is the name of the timebase in which the ICS-2100 is configured.

Figure 2-13. ICS-2100 Control Panel on the Panel Tabset

30 Doc. 065291-01 3/09

2 • Features

• A Sequence Control panel let s you define and run sequences (groups

of sample injections to be analyzed in the order in which they are listed).

• A Status panel shows the overall system status.

• An Autosampler panel (included if the ICS-2100 is connected to an

AS, AS-DV, or AS-HV Autosampler) provides access to autosampler functions.

To open the panel tabset, use one of the methods below:

• If Chromeleon is installed,

start Chromeleon and click the Default Panel Tabset toolbar button, or select

View > Default Panel Tabset.

• If Chromeleon Xpress is

installed, start the application; this automatically displays the ICS2100 panel tabset.

2.3.2 Software Control Modes

Two modes of software control are available: direct control and programmed control.

• With direct control, you select operating parameters and commands

from the Control panels. Direct control commands are executed as soon as they are entered. See Section 3.11.2 control.

for details about direct

• With programmed control, you create a list of control commands to

be executed in chronological order. Programs can be created automatically (with the help of a software wizard). See Section 3.11.3 for details about programmed control.

2.3.3 System Wellness

System Wellness monitors the overall “health” of a chromatographic system. It provides built-in diagnostic and calibration features that help prevent unscheduled system shutdowns and assure reliable operation of system devices. For details about System Wellness, see Section 5.1

Doc. 065291-01 3/09 31

ICS-2100 Ion Chromatography System

2.4 System Component Details

This section provides details about ICS-2100 system components, including the vacuum degas assembly, pump, eluent generator, injection valve, column heater, suppressor, auxiliary power supply, and conductivity cell.

2.4.1 Vacuum Degas Assembly (Optional)

The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user. The assembly, which must be installed in the ICS-2100 at the factory, consists of:

• A single-channel degas chamber (with degas membranes) with

internal capacity of 17 mL

• A dual-stage diaphragm vacuum pump

• A solenoid valve

• An on-board vacuum sensor

• The electronics required to operate the vacuum pump

• Tubing, fittings, and other accessories

By default, the ICS-2100 monitors the degas pressure reading and turns the degas pump on and off as needed. Different degas operating modes can be selected from the touch screen from Chromeleon.

To select the degas operating options, open the Chromeleon Server Configuration program, right-click the ICS-2100 device in the timebase, and select Properties.

PUMP page (see Section B.7) or

32 Doc. 065291-01 3/09

2 • Features

Select the Options tab (see Figure 2-14).

Figure 2-14. Server Configuration Properties: Degas Options

Degas Options

• Always Off: The degas pump is always off.

• Always On: The degas pump is always on. This setting is for test

purposes by a Dionex Service Representative. Do not use this setting for routine operation.

• Cycle: The degas pump cycles on and off according to the times

specified in the long the degas pump runs during a cycle. between cycles.

Cycle On and Off fields. Cycle On specifies for how

Cycle Off specifies the time

• Monitor: (default mode) The ICS-2100 monitors the degas pressure

reading and turns the degas pump on and off as required.

Doc. 065291-01 3/09 33

ICS-2100 Ion Chromatography System

2.4.2 Eluent V alve

Figure 2-15. Eluent Valve

2.4.3 Pump

The eluent valve controls the flow from the eluent reservoir. The valve opens automatically when the pump is started and closes when the pump is turned off. The valve can also be opened and closed manually from the Chromeleon Control panel (see Section 2.3.1 screen

PUMP page (see Section B.7).

) or the touch

This lets you perform service procedures on pump components without eluent leaks occurring.

The ICS-2100 pump is a microprocessor-based isocratic eluent delivery system. Its variable speed, dual-piston series design ensures pulse-free pumping for the most demanding applications.

Primary Pump Head

The primary pump head pumps eluent into the secondary head (see

Figure 2-16

). The check valves, which prevent reverse flow through the pump, are located on the bottom (inlet) and top (outlet) of the primary pump head. The priming valve is on the front of the pump head.

To open the priming valve, turn the knob one-quarter to one-half turn counterclockwise. When the priming valve is open, liquid can flow into and out of the primary pump head via the port in the front of the valve.

NOTE The priming valve must be open when the pump is

being primed with a syringe or with isopropyl alcohol. For detailed priming instructions, see

Section 5.16

34 Doc. 065291-01 3/09

Secondary

Pump Head

2 • Features

Outlet Check Valve

Primary Pump Head

Waste Valve

Pressure

Transducer

Priming Valve

Inlet Check Valve

Figure 2-16. ICS-2100 Pump Components

Secondary Pump Head

The secondary pump head delivers eluent to the remainder of the chromatography system (the injection valve, column, and detector). The waste valve is located on the front of the secondary pump head (see

Figure 2-16

To open the waste valve, turn the knob one-quarter to one-half turn counterclockwise. When the waste valve is in the open position, all pump flow is directed to waste.

NOTE The waste valve must be open when the pump is

being primed using the Prime button. For detailed priming instructions, see Section 5.16

Doc. 065291-01 3/09 35

ICS-2100 Ion Chromatography System

Pressure Transducer

Flow exiting the secondary pump head is directed to the pressure transducer (see Figure 2-16

Pressure readings indicate that the pumping system is delivering smooth, accurate flow. Pressure readings can be monitored from the Chromeleon Control panel or the touch screen

The system pressure should remain consistent (no more than a 3% difference from one pressure reading to the next). High and low pressure limits can be used to stop the pump flow if a limit is exceeded. The pressure limits can be set from Chromeleon (in the Server Configuration or in the control program) or from the touch screen

Section B.7

). See Section 4.2 for troubleshooting information if a pressure limit is exceeded.

Pulse Damper

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

), which measures the system pressure.

HOME page.

PUMP page (see

Piston Seal Wash

The pump includes a piston seal wash assembly that can be set up to continuously rinse the back of the piston seals to remove salt crystals and prolong the life of the seals. To use this feature, an external water source must be connected. For connection instructions, refer to the ICS-2100 installation instructions.

For continued protection of the pump, replace the piston rinse seals (see

Section 5.7

) and O-rings in the seal wash assembly every 6 months, or

whenever you replace the main piston seals for the ICS-2100 pump.

36 Doc. 065291-01 3/09

2.4.4 Eluent Generator

The eluent generator produces high-purity eluents online, using only deionized water as the carrier. The eluent generator consists of an eluent generator cartridge (EGC) that generates the eluent, and a high-pressure degas tubing assembly that removes electrolysis gases created during eluent generation.

NOTE A gas separator waste tube (P/ N 0 45460) should

be connected to the system waste line during installation (see Section B.10.1

Several types of EluGen cartridges are available for use with the ICS2100 (see Table 2-1) electrolyte concentrate solution for eluent generation.

EluGen Cartridge Part Number Function

EGC II K2CO3 EluGen Cartridge

EGC II KOH EluGen Cartridge

EGC II LiOH EluGen Cartridge

EGC II MSA EluGen Cartridge

EGC II NaOH EluGen Cartridge

2 • Features

. Each cartridge contains 900 mL of the appropriate

058904 Generates carbonate eluent for

anion exchange separations. Note: Produces a carbonate/bicarbonate mixture when installed with the EPM Electrolytic pH Modifier (P/N 063175) and EGC CO Mixer (P/N 061686).

058900 Generates 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.

Table 2-1. EluGen Cartridge Types for the ICS-2100

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

Doc. 065291-01 3/09 37

ICS-2100 Ion Chromatography System

You can select the concentration of eluent to be generated from either the Chromeleon Control panel or from the touch screen

Section B.4

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

Single-Cartridge Configuration

In the single-cartridge configuration, the ICS-2100 contains one EluGen cartridge.

EluGen Cartridge Eluent Concentration Range

K2CO

KOH 0.1 to 100 mM at 0.1 to 1.0 mL/min flow

LiOH 0.1 to 80 mM at 0.1 to 1.0 mL/min flow

MSA 0.1 to 100 mM at 0.1 to 1.0 mL/min flow

NaOH 0.1 to 100 mM at 0.1 to 1.0 mL/min flow

and Table 2-3.

0.1 to 15 mM at 0.1 to 1.0 mL/min flow

0.1 to X mM at 1.0 to 2.0 mL/min flow where X = 15/flow in mL/min

0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow in mL/min

0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 80/flow in mL/min

0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow in mL/min

0.1 to X mM at 1.0 to 3.0 mL/min flow where X = 100/flow mL/min

HOME page (see

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

Configurations

Linked Dual-Cartridge Configuration

In the linked dual-cartridge configuration, the ICS-2100 contains two EluGen cartridges (or one EluGen cartridge and an EPM) that perform as one cartridge. Note that the allowable eluent concentration for a linked cartridge is less than when the cartridge is defined as independent. For

38 Doc. 065291-01 3/09

2 • Features

details, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

EluGen Cartridges

K2CO3/EPM Electrolytic

pH Modifier

KOH/KOH KOH/MSA KOH/NaOH MSA/MSA MSA/NaOH NaOH/NaOH

LiOH/LiOH 0.1 to 40 mM at 0.1 to 1.0 m L/ mi n

Eluent Concentration Range Comment

0.1 to 15 mM at 0.1 to 1.0 mL/min flow

0.1 to X mM at 1.0 to 2.0 mL/min flow X = 15/flow

0.1 to 50 mM at 0.1 to 1.0 mL/min flow

0.1 to X mM at 1.0 to 3.0 mL/min flow X = 50/flow

flow

0.1 to X mM at 1.0 to 3.0 mL/min flow X = 40/flow

The total of the eluent concentrations from both the EluGen cartridge and the EPM must not exceed the specified range. The EPM concentration must not exceed 10 mM. See

“

Generating Carbonate/Bicarbonate Eluent” on page 41 for

details. The eluent

concentration range for each cartridge is cut by 50%.

The eluent concentration range for each cartridge is cut by 50%.

Table 2-3. Eluent Concentration Ranges for Linked

Dual-Cartridge Configurations

EluGen Cartridge Holder

The EluGen cartridge is installed in a cartridge holder, which mounts on the ICS-2100 top cover (see Figure 2-7

). The cartridge holder also houses

the high-pressure degas tubing assembly. The ICS-2100 can control up to two EluGen cartridges. However, when

operating with an EGC II K

EluGen Cartridge and the pH Modifier,

2CO3

only one cartridge can be installed, because the pH Modifier must be connected to the other EGC power supply (

Doc. 065291-01 3/09 39

EGC-1 or EGC-2).

ICS-2100 Ion Chromatography System

Tubing and fittings for plumbing the cartridge, degas assembly, CR-TC, and EPM are included with the holder. For connection instructions, refer to the ICS-2100 installation instructions.

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

OUTLET port. For details, refer to the ICS-2100 installation instructions.

Continuously Regenerated Trap Column (CR-TC)

The CR-TC is a high pressure electrolytically-regenerated trap column. The CR-TC is designed to remove anio nic 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 ICS-2100:

• 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 The IonPac® ATC-HC Trap Column (P/N 059604)

or IonPac CTC-1 Trap Column (P/N 040192) can be used with the ICS-2100. However, both IonPac trap columns require off-line chemical regeneration. Contact Dionex for more information.

40 Doc. 065291-01 3/09

2 • Features

EPM Electrolytic pH Modifier and EGC CO

Mixer

The EGC II K2CO3 EluGen Cartridge can be used with an

EPM Electrolytic pH Modifier (P/N 063175) (see Figure 2-17 and an EGC CO

Mixer

)

EluGen Cartridge

EPM

(P/N 061686 ) to produce a carbonate/ bicarbonate mixture. The carbonate/bicarbonate mixture is used with carbonatebased IonPac columns for anion exchange separations.

Figure 2-17. ICS-2100 with an EluGen Cartridge and EPM Installed

After the cartridge generates carbonate eluent, the pH Modifier adjusts the eluent concentration to produce the carbonate/bicarbonate mixture. The EGC CO

solution of electrolytically-generated K

Mixer provides enough mixing to produce a homogenous

and KHCO3 eluent.

2CO3

For more information about these products, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Re ference Libra ry CD-ROM (P/N 053891).

Generating Carbonate/Bicarbonate Eluent

If a K2CO3 EluGen cartridge and an EPM Electrolytic pH Modifier are installed (connected to EGC-1 and EGC-2, respectively), set EGC-1 to

the concentration of K to the concentration of KHCO K

/KHCO3 eluent mixture, the K2CO3 cartridge must generate the

2CO3

required for your application and set EGC-2

2CO3

required. In order to achieve the desired

total of the two setpoint concentrations. For example, for a 3.50 mM K

/1.00 mM KHCO3 eluent, set EGC-1

2CO3

to 3.50 mM and EGC-2 to 1.00 mM. When the eluent is generated, the K

Doc. 065291-01 3/09 41

cartridge generates 4.50 mM K2CO3, which is then modified by

2CO3

ICS-2100 Ion Chromatography System

the EPM to achieve the desired 3.50 mM K2CO3/1.00 mM KHCO mixture.

2.4.5 Auxiliary Power Supply (Optional)

The EGC-2 power supply can be configured as an auxiliary power supply for the operation of an electrolytic device such as a water purifier. The power supply operates in constant current mode and can be configured from 0 to 200 mA, with a maximum voltage of 35 V.

2.4.6 Injection Va lve

The injection valve (P/N 057968) is a six-port, electrically-activated valve. A 25-μL sample loop (P/N 042857) is installed on the valve at the factory.

The valve has two operating positions: Load and Inject (see Figure 2-18

Sample In

Sample Loop

LOAD POSITION

To Column

Sample In

Sample Loop

INJECT POSITION

To Colum

To Waste

From Pum

To Waste

From Pum

Figure 2-18. Injection Valve Flow Schematics

Eluent flows through either the Load or Inject path, depending on the valve position.

• 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

42 Doc. 065291-01 3/09

2 • Features

syringe or automated sampler 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 3.10 describes how to inject samples.

Figure 2-19

shows the injection valve connections. The injection valve is

plumbed at the factory with all tubing and fittings for connection to the

™

pump, injection port, column, and waste. A 25-μL PEEK

sample loop (P/N 042857) is installed between ports L (1) and L (4). Dionex offers sample loops in various sizes. If necessary, the pre-installed 25-μL loop can be replaced with a loop that has a different sample injection volume.

Figure 2-19. Injection Valve Plumbing

NOTE 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 the system backpressure is too low, install a backpressure coil. Connect one end of the backpressure coil to port P (2) on the injection valve; connect the other end to the for details.

Doc. 065291-01 3/09 43

TO INJ VALVE IN - P line. See Section B.17.1

ICS-2100 Ion Chromatography System

2.4.7 Auxiliary Valve (Optional)

The auxiliary valve is a high-pressure Rheodyne valve. The electricallyactivated, 2-position PEEK valve is offered in both 6-port and 10-port models (6-Port Valve Kit, P/N 069472; 10-Port Valve Kit, P/N 069473). The auxiliary valve enables a variety of sample preparation activities, including:

• Online filtration

• Matrix elimination (for example, the removal of high backgrounds of

chloride or organic material)

• Concentrator-based techniques

• Conditional injections (large loop/small loop applications where the

data system monitors sample concentration and reinjects the sample, using the smaller loop, if the concentration is too high)

• AutoNeutralization

™

• Matrix diversion prior to MS (mass spectrometry) detection

For more information, refer to Installing the ICS-1100/ICS-1600/ICS2100 Auxiliary Valve (Document No. 065288). The manual is provided in

the Auxiliary Valve Kit.

44 Doc. 065291-01 3/09

2.4.8 Column Heater

2 • Features

The column heater provides temperature control for the separator and guard column.

The heater temperature can be set to between 30 °C and 60 °C. However, the set temperature must be at least 5 °C above the ambient temperature. A thermistor mounted in the heater block monitors the temperature. Setting the temperature to 0 °C turns off the column heater.

If the temperature exceeds 65 °C, the column heater is shut off and the error message “Column heater exceeds safe temperature.” is displayed on the touch screen and in the Chromeleon Audit Trail. See Section 4.2 information.

for troubleshooting

For best results with 2-mm columns, a microbore heat exchanger (P/N 060943) should be installed in the column heater (see

Section 5.13

). The tubing connections between the injection valve and column heat exchanger, guard column and separator column, and separator column to detector cell should all use red 0.125-mm, 0.005-in ID PEEK tubing (P/N 044221), rather than the standard black tubing.

Figure 2-20. Column Heater

Doc. 065291-01 3/09 45

ICS-2100 Ion Chromatography System

2.4.9 Suppressor

The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an Atlas Electrolytic Suppressor, Self-Regenerating Suppressor, or MicroMembrane Suppressor can be used with the ICS-2100.

For details about any of the suppressors or for information about selecting a suppressor for your application, refer to the suppressor manuals. The manuals are on the Dionex Reference Library CD-ROM (P/N 053891).

2.4.10 DS6 Heated Conductivity Cell

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

Temperature Control

μL), and low

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.

In ion analysis, the effect of temperature variation is minimized by suppressing eluent conductivity. To further reduce the effect of temperature variation, a heater inside the cell regulates the temperature. The cell heater can be set to between 30 °C and 55 °C. The set temperature must be at least 7 °C above the ambient temperature. Setting the cell temperature to 0 °C turns off the cell heater.

Temperature Compensation

Built-in preset temperature compensation of 1.7% per °C helps minimize changes in the baseline or in peak heights when the operating temperature is different from the temperature at which the cell was calibrated.

46 Doc. 065291-01 3/09

2 • Features

DS6 Heated Conductivity Cell Components

The cell front cover provides CELL IN and CELL OUT fittings for connecting the cell to the suppressor (see Figure 2-8 components are mounted behind the component panel. To replace, the cell remove the screws on the cell front cover and pull the entire cell assembly out through the component panel. See Section 5.10 instructions.

). The remaining cell

for cell replacement

Doc. 065291-01 3/09 47

ICS-2100 Ion Chromatography System

48 Doc. 065291-01 3/09

3 • Operation and Maintenance

This chapter describes routine operating and maintenance procedures for the ICS-

2100. The ICS-2100 is designed for IC (ion chromatography) applications and should

not be used for any other purpose. Operation of the ICS-2100 in a manner not specified by Dionex may result in personal injury.

3.1 Operation Overview

Figure 3-1 illustrates the basic steps for routine operation of the ICS-2100.

Power up the system

Start Chromeleon

Set up the reservoir

(or RFIC-ER system )

Check all

connections

Prime the pump

Set operating

conditio n s

Equilibrate the

system

Prepare samples

Verify operating

status

Process samples

Figure 3-1. Operation Flow Chart

Doc. 065291-01 3/09 49

ICS-2100 Ion Chromatography System

Sample Processing Overview

Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-2 sample processing.

shows the typical steps for manual and batch

Manual Sample

Processing

Using the Front Panel

Load the sample Load the sample

Autozero

Inject the sample

(Optional)

Record data from

the analog output*

*A third-party recording

device must be connected to the analog output.

Manual Sample

Processing

Using Chromeleon

Start data

acquisition

Autozero

Inject the sample

Stop data

acquisition

(Optional)

Save the manual

sequence data

Batch Sample

Processing

Using Chromeleon

Create a sequence

(Sequence Wizard)

Add the sequence

to the batch

Start the batch

Figure 3-2. Sample Processing Overview

50 Doc. 065291-01 3/09

3 • Operation and Maintenance

3.2 Turning On the System Power

Power Switch

Press the power switch on the ICS2100 rear panel (see Figure 3-3

) to turn on the system power. Table 3-4 shows the ICS-2100 conditions at power-up.

Also turn on the power to the computer and the autosampler (if used).

Figure 3-3. ICS-2100 Rear Panel

Feature Power-Up Condition

Pump Off Injection valve Load position Cell Reading current value Suppressor Off* Cell heater Set to the last value used. The default when the ICS-2100

is turned on for the first time is 35 °C.

Column oven temperature Set to the last value used. The default when the ICS-2100

is turned on for the first time is 30 °C. Eluent generator Off* CR-TC Off EPM

* When you start the suppressor, eluent generator, or EPM, the value used last is restored.

Table 3-4. ICS-2100 Power-Up Conditions

Doc. 065291-01 3/09 51

Off

ICS-2100 Ion Chromatography System

3.3 Connecting to Chromeleon

NOTE If you are beginning operation of an ICS-2100 that has

not been configured in a timebase, refer to the ICS-2100 installation instructions for Chromeleon setup instructions.

1. Turn on the PC.

2. Start the Chromeleon Server, if it is not already running. a. Check the Chromeleon Server Monitor icon on the Windows taskbar.

• When the server is running, the icon is gray .

• When the Server is not running, the icon is crossed out in red ).

To start the server, right-click the icon and select Start Server.

b. If the Server Monitor icon is not on the Windows taskbar, click Start >

All Programs > Chromeleon > Server Monitor. The Server Monitor opens. Click Start to start the server.

3. To start the Chromeleon client, click Start and select All Programs > Chromeleon > Chromeleon.

4. If Chromeleon is installed, the main window and Browser appear. Display the panel tabset by selecting View > Default Panel

Tabset or by clicking the Default Panel Tabset toolbar button.

If Chromeleon Xpress is installed, starting the application automatically displays the panel tabset.

5. To display the ICS-2100 Control panel, click the tab labeled with the ICS2100 timebase name (see Figure 3-4

52 Doc. 065291-01 3/09

3 • Operation and Maintenance

Figure 3-4. ICS-2100 Control Panel on the Chromeleon Panel Tabset

Doc. 065291-01 3/09 53

ICS-2100 Ion Chromatography System

3.4 Set Up the Eluent Reservoir

The ICS-2100 does not require pressurized reservoirs. However, if eluent is manually degassed or is sensitive to contamination, Dionex recommends pressurizing the reservoir with helium or nitrogen.

The air regulator accessory bracket and other items needed for pre ssurizing the eluent reservoir must be ordered separately (P/N 060054). For more information, refer to the ICS-2100 installation instructions.

3.4.1 Filter the Deionized Water

Filtering removes small particulates in the deionized water that may contaminate the pump check valves and cause erratic flow rates or loss of prime. An end-line filter (P/N 045987) is provided in the ICS-2100 Ship Kit (P/N 064375) for this purpose.

Install the end-line filter on the end of the deionized water line, inside the reservoir. Verify that the end of the filter extends to the bottom of the reservoir and that the filter is submerged in deionized water . This preven ts air from being drawn through the lines.

3.4.2 Fill the Reservoir

Fill the reservoir with ASTM filtered, Type I (18-megohm) deionized water.

3.4.3 Set the Eluent Level

After filling the reservoir, enter the volume of liquid in the reservoir in one of the following locations:

• On the HOME page in the Eluent Level field (see Figure 3-5)

• In the Eluent Bottle field in the Pump Settings window (accessed

from the ICS-2100

Figure 3-4

The ICS-2100 determines the eluent usage by monitoring the flow rate and the length of time the pump is on, and updates the Eluent Bottle volume as the eluent is depleted. A warning appears if the level falls below 200 mL. Warnings are repeated at 100 mL and 0 mL.

54 Doc. 065291-01 3/09

)

Control panel on the Chromeleon panel tabset (see

3 • Operation and Maintenance

In order for the level displayed in the Eluent Bottle box and gauge to be accurate, you must enter the level when the reservoir is fil led. The ICS-2100 does not automatically detect when the reservoir is filled, nor when it is empty.

Enter the volume of

liquid in the reservoir

Enter the volume

of liquid in the

reservoir (in liters)

Note: The Eluent Level field is updated as the liquid is depleted.

Figure 3-5. Home Page: Setting the Eluent Level

Note: The Eluent Bottle field and slider gauge are updated as the liquid is depleted.

Figure 3-6. Pump Settings Windows: Setting the Eluent Level

The STATUS page (see Figure 3-7) also displays the amount of liquid remaining in the reservoir and an estimate of how many hours remain before the eluent reservoir is empty.

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ICS-2100 Ion Chromatography System

See Section B.6 for details about the STATUS PAGE.

Figure 3-7. Status Page

3.4.4 Connect the Reservoir

If it is not already connected, connect the

OUT

line from the reservoir cap to the which extends from the plumbing and cable chase on the top of the ICS-2100 (see

Figure 3-8

ELUENT BOTTLE

ELUENT IN line,

ELUENT BOTTLE

OUT

ELUENT

Figure 3-8. Reservoir Connections

56 Doc. 065291-01 3/09

3.5 Check All Connections

(

)

1. Make sure the eluent reservoir is filled and the tubing connecting the reservoir

to the ICS-2100 tubing is securely connected (see Figure 3-8

2. Make sure the eluent generator electrical cable (blue) is connected to the

EGC-1 connector.

3 • Operation and Maintenance

3. Make sure the CR-TC electrical cable (black) is connected to the

connector.

3.6 Prime the Pump

If you changed eluent or if the eluent lines are dry, prime the lines first with a syringe before following the procedure below to prime the pump. See Section 5.16.1 syringe.

1. Verify that the priming valve on the primary pump head (see Figure 3-9) is

closed (turned all the way clockwise).

2. Open the waste valve on the secondary pump head by turning the knob one-

quarter to one-half turn counterclockwise. Opening the valve directs the eluent flow path to waste and eliminates backpressure.

Secondary

Pump Head

Waste Valve

(open)

CR-TC

for instructions on priming the lines with a

Primary

Priming Valve

Pump Hea

Figure 3-9. Priming the Pump

3. Press

Doc. 065291-01 3/09 57

Prime on the Chromeleon Control panel or the ICS-2100 touch screen

HOME page. Confirm that the waste valve is open by pressing OK when the

ICS-2100 Ion Chromatography System

reminder message appears. The pump will begin pumping at approximately 3mL/min.

4. Continue priming the ICS-2100 until all air and previous eluent are purged and no air bubbles are exiting the waste line.

5. Press

Pump Off.

6. Close the waste valve. Do not overtighten. The pump is now ready for operation.

3.7 Set System Operating Conditions

NOTE This section is an overview of the steps needed to start

up the system and begin running samples. Actual operating parameters (flow rate, cell heater temperature, suppressor current, etc.) depend on the application to be run. Refer to the column manual for the required parameters for your application.

Set or verify system operating parameters from either the Chromeleon Control panel or from the touch screen automatically by loading a Chromeleon sequence.

NOTE Clicki ng the System Startup button on the Chromeleon

Control panel starts the pump and suppressor. The flow rate and suppressor current settings that were in effect when the system was shut down are restored.

HOME page. Operating parameters can also be set

NOTE Clicki ng the System Startup button on the Chromeleon

Control panel starts the pump, suppressor, eluent generator, and CR-TC. The flow rate, suppressor current, and eluent concentration settings that were in effect when the system was shut down are restored.

1. Verify that the pump is on and set to the correct flow rate.

2. Verify that the suppressor current is on and that the setting is correct.

3. Verify that the eluent generator is turned on and the correct concentration is set. Verify that the CR-TC is turned on.

4. Verify that the cell heater is set to the correct value.

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3 • Operation and Maintenance

5. Verify that the column heater is set to the correct value.

Automatically Turning on the Suppressor and Eluent Generator

You can set up the ICS-2100 to turn on the suppressor, eluent generator, and CR-TC automatically when the pump is turned on. To do this:

• For the suppressor, select the Automatically turn on with pump option from

SUPPRESSOR page.

the

• For the eluent generator and CR-TC, select the option from the ELUENT

GENERATOR

NOTE The suppressor, eluent generator, and CR-TC are

page.

always turned off automatically when the pump is turned off.

3.8 Equilibrate the System and Verify Operational Status

NOTE You can monitor system functions (conductivity,

pressure, cell temperature, etc.) from the Chromeleon Control panel or from the touch screen

HOME page.

1. Allow the system to equilibrate. During equilibration, the Chromeleon Control panel displays the background conductivity (the conductivity of the eluent before sample injection) and the system backpressure.

2. Monitor the background conductivity. Refer to the column manual for the appropriate background conductivity for your applicat ion.

3. Offset the background and zero the reading by clicking the Autozero on the Chromeleon Control panel (see Figure 3-4

button

4. Monitor the system pressure from the Control panel to make sure it is at the expected pressure for the installed column (refer to the column manual for details) and is stable.

• If the pressure is less than the expected amount, gas may be trapped in the

system. T o release the gas, remove the pump fitting on the injection valve port, labeled

P (2). Allow the air to escape and then reconnect the fitting.

• If the pressure fluctuates by more than about 0.13 MPa (20 psi), prime the

pump. See Section 4.3

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for additional troubleshooting information.

ICS-2100 Ion Chromatography System

• If the pressure is too high, there may be a restriction in the system

plumbing. See Section 4.7

5. Verify that the baseline conductivity is at the expected reading for your application and is stable. In general, it should be <30 for anion analyses and <2

Section 4.12

See Section 4.13

for troubleshooting information if the conductivity is too high.

if the baseline is drifting or has excessive “noise” (large

fluctuations in readings).

6. Verify that the cell heater is at the set point and is stable. The temperature is at equilibrium when the Set Temperature and the Current Temperature readings on the Control panel are the same, or when the “ displayed next to the

Column Heater temperature on the HOME page.

7. Verify that the column heater temperature is at the se t point and stable. The temperature is at equilibrium when the Set Temperature and the Current Temperature readings on the Control panel are the same, or when the “ symbol is displayed next to the Column Heater temperature on the HOME page.

The system is now ready for sample processing.

for troubleshooting information.

μS for a system set up for cation analyses. See

μS for a system set up

=” symbol is

=”

3.9 Prepare Samples

NOTE Sample preparation can be performed while the system

is equilibrating.

3.9.1 Collecting and Storing Samples

Collect samples in high density polyethylene containers that have been thoroughly cleaned with deionized (DI) water. Do not clean containers with strong acids or detergents because these can leave traces of ions on the container walls. The ions may interfere with the analysis.

If samples will not be analyzed on the day they are collected, filter them through clean 0.45 μm filters immediately after collection; otherwise, bacteria in the samples may cause the ionic concentrations to change over time. Refrigerating the samples at 4 eliminate, bacterial growth.

60 Doc. 065291-01 3/09

° C (39° F) will reduce, but not

Analyze samples containing nitrite or sulfite as soon as possible. Nitrite oxidizes to nitrate, and sulfite to sulfate, thus increasing the measured concentrations of these ions in the sample. In general, samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant changes in anion concentrations.

3.9.2 Pretreating Samples

Analyze rainwater, drinking water, and air particulate leach solutions directly with no sample preparation (other than filtering and possibly diluting).

Filter groundwater and wastewater samples through 0.45 μm filters before injection, unless samples were filtered after collection.

Before injection, pretreat samples that may contain high concentrations of interfering substances by putting them through Dionex OnGuard

cartridges. Refer to Installation and Troubleshooting Guide for OnGuard Cartridges (Document No. 032943) for instructions.

3 • Operation and Maintenance

3.9.3 Diluting Samples

Because the concentrations of ionic species in different samples can vary widely from sample to sample, no single dilution factor can be recommended for all samples of one type. In some cases (for example, many water samples), concentrations are so low that dilution is not necessary.

Use eluent or ASTM filtered, Type I (18-megohm) deionized water to dilute the sample. When using carbonate eluents, diluting with eluent minimizes the effect of the water dip at the beginning of the chromatogram. If you dilute the sample with eluent, also use eluent from the same lot to prepare the calibration standards. This is most important for fluoride and chloride, which elute near the water dip.

To improve the accuracy of early eluting peak determinations, such as fluoride, at concentrations below 50 ppb, dilute standards in eluent or spike the samples with concentrated eluent to minimize the water dip. For example, spike a 100 mL sample with 1.0 mL of a 100 X eluent concentrate.

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ICS-2100 Ion Chromatography System

3.10 Loading and Injecting Samples

NOTE Samples can be injected using either the standard

injection valve or the optional auxiliary valve, if installed. For more information, see the Chromeleon Help or user’s manual.

The two techniques for loading samples into the sample loop are: (1) with an autosampler or (2) with a syringe or vacuum syringe through the injection port on the ICS-2100 front door.

For autosampler injections, the injection port tubing is disconnected from the ICS2100 injection valve and replaced by the autosampler outlet tubing. Other setup requirements depend upon the model of autosampler.

Setup for an AS Autosampler

To use an AS Autosampler with the ICS-2100, the following requirements must be met:

• The ICS-2100 injection valve (or the auxiliary valve, if installed) must be

specified as the injection valve and must be linked to the AS in the Chromeleon timebase.

• An injection valve should not be installed in the AS.

See the ICS-2100 installation instructions for AS connection instructions.

NOTE The ICS-2100 and the AS ca n be set up for stand-alone

(front panel) operation. This requires a TTL cable connection between the ICS-2100 and the AS. See

Section D.3

Setup for an AS-DV Autosampler

for stand-alone setup instructions.

To use an AS-DV Autosampler with the ICS-2100, the following requirements must be met:

• The ICS-2100 injection valve must be linked to the AS-DV in the

Chromeleon timebase.

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3 • Operation and Maintenance

Setup for an AS-HV Autosampler

For setup information for the AS-HV Autosampler, see the AS-HV Autosampler Operator’s Manual (Document No. 065125). The manual is provided on the

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

3.10.1 Loading Samples with a Syringe

1. Make sure the injection port on the ICS-2100 front door (see

Figure 2-1

(see Figure 3-10

) is connected to sample port S (5) on the injection valve

Figure 3-10. Injection Valve Connections

2. Fill the 1 cc syringe (P/N 016388) provided in the ICS-2100 Ship Kit (P/N 064375) with a calibration standard or sample.

3. Insert the syringe into the injection port on the ICS-2 10 0 front door (see Figure 2-1

4. Verify that the injection valve is in the Load position.

5. Overfill the sample loop with several sample loop volumes. Excess sample will exit through the injection valve waste line.

6. Leave the syringe in the port.

7. Switch the injection valve to the Inject position (see Section 3.10.4

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ICS-2100 Ion Chromatography System

3.10.2 Loading Samples with a Vacuum Syringe

1. Disconnect the waste line from port W (6) of the injection valve (see

Figure 3-10

PEEK or Teflon

2. Place the free end of the line into the sample.

3. Verify that the injection valve is in the Load position.

4. Insert the 1 cc syringe (P/N 016388) provided in the ICS-2100 Ship Kit (P/N 064375) into the injection port on the ICS-2100 front door (see Figure 2-1 injection valve.

) and attach a shorter line: 25 to 30 cm (10 to 12 inches) of

tubing.

) and pull out the plunger to draw the sample into the

5. Switch the injection valve to the Inject position (see Section 3.10.4

3.10.3 Loading Samples with an Autosampler

1. V erify that the autosampler output line is connected to port S (5) of the ICS-2100 injection valve.

2. Prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions.

3. The sample loading process depends on the autosampler. Refer to the autosampler manual for detailed instructions. In general, use one of the following methods:

• Include the commands for controlling sample loading in a

Chromeleon program. (If necessary, refer to the Chromeleon Help or user manual for assistance.)

• Enter the commands for loading the sample on the autosampler

front panel.

4. Switch the injection valve to the Inject position (see Section 3.10.4

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3.10.4 Injecting Samples

After loading the sample in the sample loop, use one of the following methods to switch the injection valve to the Inject position:

• Manually: Click the Inject button on the Chromeleon Control panel

(see Figure 3-4

) or touch the Inject button on the HOME page.

• Automatically: Include the Inject command in a Chromeleon

program. (If necessary, refer to the Chromeleon Help or user manual for assistance.)

3.11 Processing Samples

Samples can be run manually (one at a time) or else they can be grouped and run automatically in batches.

3.11.1 Manual Sample Processing

T o process samples manually, select operating parameters and commands from the touch screen pages, or from the Chromeleon menu bar , too lbars, and Control panel. Commands are executed as soon as they are entered.

3 • Operation and Maintenance

NOTE When you run samples manually from the front

panel (without using only temporarily in the ICS-2100 memory. For a permanent record of the data, connect a recording device (chart recorder, integrator, etc.) to the analog output. See Section B.21 connection instructions.

Chromeleon), the data is saved

for analog output

1. Complete the instructions in Section 3.2 through Section 3.8 to prepare the ICS-2100 for operation and to prepare the sample for processing.

2. Load the sample, using a syringe, vacuum syringe, or autosampler (see Section 3.10

3. In Chromeleon, select Control > Acquisition On. Chromeleon records the signal supplied by the detector and displays the signal plot on the Control panel.

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ICS-2100 Ion Chromatography System

4. Click the Autozero button on the Control panel or the touch screen

HOME page.

5. Inject the sample (see Section 3.10.4

6. In Chromeleon, monitor the chromatogram on the Control panel and

select Control > Acquisition Off when sample data is collected.

NOTE Data from Chromeleon manual processing is

saved in the MANUAL sequence folder under the local datasource. This data is overwritten each time a new manual sample is processed. To save the data from a manual run, select the MANUAL folder, select File > Save As, and enter a new name for the sequence.

7. If you are controlling the ICS-2100 from the touch screens, select the

PLOT button on the HOME page to view a plot of the conductivity

data.

3.11.2 Automatic (Batch) Sample Processing

You can use Chromeleon or Chromeleon Xpress to create a list of samples (a sequence) to be processed automatically. For each sample, the sequence includes the following:

• A program with commands and parameters for controlling the ICS-

2100 and autosampler (if used), and for acquiring sample data.

• A quantification method for peak identification and area

determination.

• Additional sample processing parameters (sample name, sample type,

injection volume, etc.).

After creating the sequence, you can start batch processing.

66 Doc. 065291-01 3/09

3 • Operation and Maintenance

Summary of Automatic Sample Processing

1. Complete the instructions in Section 3.2 through Section 3.8 to prepare the ICS-2100 for operation and to prepare the sample for processing.

2. If an autosampler is installed, prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions. Autosampler manuals are provided on the Dionex Reference Library CD-ROM (P/N 053891).

3. If an autosampler is not installed, load the sample into the injection valve sample loop through the sample port on the ICS-2100 front door (see Section 3.10.1

4. Use the Application Wizard to specify a program and quantitation method, and create a sequence:

a. On the Sequence Control panel, click Application Wizard.

b. Select an application template from the list (see Figure 3-11

Figure 3-11. Application Wizard

Doc. 065291-01 3/09 67

ICS-2100 Ion Chromatography System

c. Click Next > and select the in a new sequence via Sequence

Wizard option.

d. Click Next > to go to the Sequence Wizard. e. Complete the steps in the Sequence Wizard, adding the desired

number of samples and standards to the list. For help, click the Help button on the Sequence Wizard page.

After you click Finish, a sequence is created and a program appropriate for the selected application is copied to the sequence. If you are using Chromeleon, a quantification method is also copied to the sequence

5. Load the sequence and start batch processing:

a. On the Sequence Control panel, click Load Sequence.

b. Select the sequence created in Step 4 c. Click Start Batch.

3.12 Maintenance

This section describes routine maintenance procedures that users may perform. All other maintenance procedures must be performed by Dionex personnel.

As Needed

• Regularly check the eluent reservoir and refill when needed.

Daily

• Check the ICS-2100 component panel (see Figure 2-8) for leaks or spills.

Wipe up spills. Isolate and repair leaks (see Section 4.3 eluent with deionized water.

• Check the waste container daily and empty when needed.

Weekly

• Once a week, check fluid lines for crimping or discoloration. Replace any

pinched lines. Replace damaged lines.

• Check the junctions between the pump heads and the pump casting for

evidence of liquid leaks. If the piston seal wash tubing is not connected, check the drain tubes at the rear of the pump heads for evidence of moisture. Normal

and click Open.

). Rinse off any dried

68 Doc. 065291-01 3/09

3 • Operation and Maintenance

friction and wear may gradually result in small liquid leaks around the piston seal. If unchecked, these leaks can gradually contaminate the piston housing, causing the pump to operate poorly. If leaks occur, replace the piston seals (see Section 5.7

• Check the end-line filter (P/N 045987) and change if needed. When new, end-

line filters are pure white. If the system is in continuous operation, change the end-line filter weekly, or whenever it becomes discolored. Replace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent.

NOTE It is especially important to regularly replace end-line

filters when using aqueous eluents, which may contaminate the filter with bacteria or algae. The bacterial buildup may not be visible.

Every Six Months

• Calibrate the cell (see Section 5.1.3).

• Calibrate the vacuum degas assembly (see Section 5.1.5).

• Replace the pump piston rinse seals and piston seals (see Section 5.7).

Yearly

• Dionex recommends performing preventive maintenance annually, as well as

before scheduled Performance Qualification tests. An ICS-2100 Preventive Maintenance Kit (P/N 057954) is available for this purpose.

• Rebuild the auxiliary valve, if installed (see Section 5.4).

• If an AS Autosampler is installed, perform the preventive maintenance

procedure. The AS Preventive Maintenance Kit (P/N 060581) is available for this purpose.

• If an AS-DV Autosampler is installed, replace the tip and tubing. The AS-DV

Preventive Maintenance Kit (P/N 055647) contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve. Instructions are included with the kit.

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ICS-2100 Ion Chromatography System

70 Doc. 065291-01 3/09

This chapter is a guide to troubleshooting minor issues that may arise during operation of the ICS-2100. Turn to the section of this chapter that best describes the operating problem or symptom that has been observed. Each section lists possible causes of the problem or symptom in order of probability. A systematic troubleshooting approach is the most effective way to determine the root cause.

If you are unable to resolve a problem by following the instructions here, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office. Please have this chapter at hand when talking with Technical Support personnel.

4.1 Error Messages

The Moduleware (the instrument control firmware installed in each ICS-2100 module) periodically checks the status of certain parameters. If a problem is detected, it is displayed on the touch screen.

Error messages are also reported to Chromeleon and logged in the Audit Trail. Each error message is preceded by an icon that identifies the seriousness of the underlying problem (see the table below). You can change the severity level assigned to a problem whenever appropriate.

4 • Troubleshooting

Icon Severity Level Description

Warning A message is displayed in the Audit Trail, but the

current run is not interrupted.

Error A message is displayed in the Audit Trail, and the

system attempts to correct the problem (sometimes by using an alternative parameter). An Error never interrupts the current analysis; however, if it occurs during the Ready Check, the analysis will not be started.

Abort A message is displayed in the Audit Trail, and the

running batch is aborted.

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ICS-2100 Ion Chromatography System

The table below lists the most frequently observed ICS-2100 error messages. For troubleshooting assistance, refer to the page indicated in the table.

Alarms and Error Conditions See Auxiliary power supply disconnected

Auxiliary power supply over current Auxiliary power supply over voltage Auxiliary power supply stopped for zero flow Column heater exceeds safe temperature Column heater open circuit Column heater short circuit CR-TC over current CR-TC stopped for zero flow rate Degas calibration failed EGC board not present EGC-1 calibration error EGC-1 disconnected error EGC-1 invalid concentration EGC-1 invalid concentration vs. flow rate EGC-1 invalid flow rate EGC-1 over current EGC-1 over voltage EGC-2 calibration error EGC-2 disconnected error EGC-2 invalid concentration EGC-2 invalid concentration vs. flow rate EGC-2 invalid flow rate EGC-2 over current EGC-2 over voltage Hardware not present Leak sensor wet Load/Inject valve error

page 74 page 74 page 75 page 75 page 75 page 76 page 76 page 76 page 77 page 77 page 77 page 78 page 78 page 78 page 78 page 79 page 79 page 79 page 78 page 78

page 78 page 79 page 79 page 79 page 80 page 80 page 80

Table 4-5. Alarms and Error Messages Summary

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4 • Troubleshooting

Alarms and Error Conditions See Option not installed

Pressure slope calibration error Pump motor lost control Pump over pressure Pump pressure hardware error Pump stopped due to lost USB communication error Pump under pressure Second valve error Suppressor not connected Suppressor over current Suppressor over power Suppressor over voltage Suppressor stopped for zero flow rate

Table 4-5. Alarms and Error Messages Summary (Continued)

page 81 page 81 page 81 page 82 page 82 page 82 page 83 page 83 page 84 page 84 page 85 page 85 page 85

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ICS-2100 Ion Chromatography System

4.2 Troubleshooting Error Messages

AUXILIARY POWER SUPPLY DISCONNECTED

This error occurs when the auxiliary power supply is configured as active, but no device is connected.

To troubleshoot:

1. Connect the cable for the auxiliary device to the connector.

2. If there is no auxiliary device, open the Chromeleon Server Configuration program and remove this option from the ICS-2100 timebase.

AUXILIARY POWER SUPPLY OVER CURRENT

This error occurs when the device connected to the auxiliary power supply is attempting to draw more current than is allowed (200 mA) or is 20% higher than the set current.

To troubleshoot:

1. Check the cable connecting the device to the power supply for damage or a faulty connection.

2. If the error persists, refer to the manual provided by the device vendor for assistance.

EGC-2 power supply

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4 • Troubleshooting

AUXILIARY POWER SUPPLY OVER VOLTAGE

This error occurs when the device connected to the auxiliary power supply is attempting to operate at a higher voltage than is allowed (35 V).

To troubleshoot:

1. Check the cable connecting the device to the power supply for damage or a faulty connection.

2. If the error persists, refer to the manual provided by the device vendor for assistance.

AUXILIARY POWER SUPPLY STOPPED FOR ZERO FLOW RATE ERROR

When the pump flow stops, the auxiliary power supply automatically turns off (to prevent damage to the electrolytic device) and this error occurs.

To troubleshoot:

If the pump stopped unexpectedly, see Section 4.6

for pump troubleshooting

information.

COLUMN HEATER EXCEEDS SAFE TEMPERAT URE

This error occurs when the column heater temperature is higher than the maximum allowed. This error may occur if the ICS-2100 is operating in an extreme environment (greater than 40 °C (104 °F)).

To troubleshoot:

Refer to Section A.3

for environmental specifications.

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ICS-2100 Ion Chromatography System

COLUMN HEATER OPEN CIRCUIT

This error occurs when the column heater is unplugged from the component panel.

To troubleshoot:

1. Check that the column heater is plugged into the component panel.

2. If the error persists, the column heater may be faulty. Replace the column heater (see Section 5.12

COLUMN HEATER SHORT CIRCUIT

This error occurs when there is a short circuit on the thermistor input used to measure the column heater temperature. This error indicates a faulty column heater.

To troubleshoot:

Replace the column heater (see Section 5.12

CR-TC OVER CURRENT ERROR

This error occurs when the current applied to the CR-TC exceeds the maximum current allowed.

To troubleshoot:

1. Check the CR-TC cable connection.

2. If the error persists, contact Dionex for assistance. There may be a malfunction in the CR-TC control electronics

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4 • Troubleshooting

CR-TC STOPPED FOR ZERO FLOW RATE

This message appears when you click the Shutdown button on the Chromeleon Control panel. The message also appears when you turn off the pump flow while the EGC current (and CR-TC) are on. The CR-TC is automatically turned off.

To troubleshoot:

If the pump stopped unexpectedly, see Section 4.6

for pump troubleshooting

information.

DEGAS CALIBRATION FAILED

This error occurs when the degas vacuum does not reach the expected level during calibration.

To troubleshoot:

1. Retry the calibration.

2. If calibration still fails, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance.

EGC BOARD NOT PRESENT

This error occurs if Chromeleon sends a command to the IC related to the eluent generator, but the eluent generator controller board is either not installed or the ICS-2100 does not recognize the installed board.

To troubleshoot:

Contact Dionex for assistance. The electronics components cannot be serviced by the user.

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ICS-2100 Ion Chromatography System

EGC-1 CALIBRATION ERROR EGC-2 CALIBRATION ERROR

This error occurs if the measured current is outside the expected range when running the eluent generator calibration procedure.

To troubleshoot:

1. Review the procedure to verify that you set up the ICS-2100 correctly and then rerun the calibration.

2. If the error message reappears, contact Dionex for assistance.

EGC-1 DISCONNECTED ERROR EGC-2 DISCONNECTED ERROR

This error occurs when Chromeleon sends a command to set an eluent generator parameter when the EGC is disconnected. The error also can occur if you attempt to run the EGC verification test when the EGC is disconnected.

To troubleshoot:

1. Verify that the EluGen cartridge cable is connec ted to the

EGC-1

connector on the ICS-2100 top cover (see Figure 2-7).

2. If the error persists, contact Dionex for assistance. There may be a malfunction in the EGC control electronics.

EGC-1 INVALID CONCENTRATION VS. FLOW RATE ERROR EGC-2 INVALID CONCENTRATION VS. FLOW RATE ERROR

The maximum eluent concentration that can be set for a particular application depends on the suppressor type, the EGC type, and the flow rate. This error occurs when the selected concentration is too high for the current flow rate.

To troubleshoot:

Refer to the column manual, which is included on the Dionex Reference Library CD-ROM (P/N 053891), for the concentration of eluent to use with

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4 • Troubleshooting

your application. Reset the eluent concentration and/or the flow rate to the recommended values.

EGC-1 INVALID FLOW RATE ERROR EGC-2 INVALID FLOW RATE ERROR

This error occurs if the flow rate is set to a value not supported by the eluent generator. The ICS-2100 allows a flow rate range of 0.00 to 5.00 mL/min without an eluent generator. With an eluent generator, the allowed range is

0.10 to 3.00 mL/min.The recommended operating range is 0.40 to

2.00 mL/min.

To troubleshoot:

Set the flow rate to a value within the allowed range.

EGC-1 OVER CURRENT EGC-2 OVER CURRENT

This error occurs when the current applied to the EluGen cartridge exceeds the maximum current allowed. Under these conditions, the EGC current is turned off to prevent damage to the EGC. This error may occur if the liquid flow to the cartridge is interrupted.

To troubleshoot:

See Section 4.6

for troubleshooting when there is no flow from the pump.

EGC-1 OVER VOLTAGE EGC-2 OVER VOLTAGE

This error occurs when the current applied to the EluGen cartridge exceeds the maximum current allowed. The EGC current is turned off to prevent damage to the EGC. This error may occur if the liquid flow to the cartridge is interrupted.

To troubleshoot:

See Section 4.6

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for troubleshooting when there is no flow from the pump.

ICS-2100 Ion Chromatography System

HARDWARE NOT PRESENT

This error indicates a problem in the ICS-2100 electronics.

To troubleshoot:

Contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user.

LEAK SENSOR WET

The leak sensor is installed in the drip tray at the bottom of the component panel (see Figure 2-8 problem and this error message appears.

To troubleshoot:

1. Locate the source of the leak by visually inspecting the tubing, fittings, and components on the component panel. Refer to Section 4.3

). If liquid accumulates in the tray , the sensor signals the

2. Tighten fittings or replace tubing and fittings as required. Refer to

Section 4.3

for detailed troubleshooting of various types of leaks.

3. After fixing the leak, dry the drip tray thoroughly to prevent the leak sensor from triggering additional error messages.

LOAD/INJECT VALVE ERROR

If the injection valve fails to switch position within 1 second of being toggled, the ICS-2100 Moduleware reports an error to Chromeleon and this error message appears.

To troubleshoot:

1. If a sequence is being executed, terminate the sequence by selecting Batch > Stop in Chromeleon.

2. Try to toggle the valve from Load to Inject by clicking the Load

and

Inject buttons on the ICS-2100 Control panel in Chromeleon or on the touch screen

80 Doc. 065291-01 3/09

HOME page.

4 • Troubleshooting

3. Turn off the ICS-2100 power briefly and then restart.

4. If the problem persists, repeat Step 2

5. If the problem persists, contact Dionex for assistance.

OPTION NOT INSTALLED

This error occurs if a command is issued to control an option that is not installed.

To troubleshoot:

Check the Chromeleon Server Configuration program to verify that the option is enabled.

PRESSURE SLOPE CALIBRATION ERROR

This error occurs if you try to calibrate the pressure slope when the pressure is less than 3 MPa (500 psi).

To troubleshoot:

Contact Dionex for assistance

PUMP MOTOR LOST CONTROL

This error indicates a problem in the pump controller electronics.

To troubleshoot:

Contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user.

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ICS-2100 Ion Chromatography System

PUMP PRESSURE HARDWARE ERROR

This error indicates a problem in the pump controller electronics.

To troubleshoot:

Contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user.

PUMP OVER PRESSURE

If the system pressure exceeds the set limit for at least 0.5 second, this error message appears and the pump stops. Pressure limits can be set in the Chromeleon Server Configuration or in the control program. The limits can also be set on the touch screen

To troubleshoot:

1. Check for blockages in the liquid lines by working your way backward from the cell to the pump. See Section 2.2

PUMP page (see Section B.7.1).

for the system flow schematics.

2. Check that the flow rate is set to the correct value.

3. Check that the high pressure limit is set to the correct value.

4. Restart the pump.

PUMP STOPPED DUE TO LOST USB COMMUNICATION ERROR

This error occurs if the ICS-2100 loses communication with Chromeleon.

To troubleshoot:

Verify that the USB cable is connected correctly from the ICS-2100 rear panel to the Chromeleon PC.

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4 • Troubleshooting

PUMP UNDER PRESSURE

If the system pressure falls below the low pressure limit, the pump stops and this error message appears. Pressure limits can be set in the Chromeleon Server Configuration or in the control program. The limits can also be set on the touch screen

To troubleshoot:

1. Make sure the eluent reservoir is full.

PUMP page (see Section B.7.1).

2. Check for liquid leaks (see Section 4.3

3. Check that the waste valve is closed.

4. Prime the pump (see Section 5.16

5. Restart the pump.

SECOND VALVE ERROR

If the auxiliary valve fails to switch position within 1 second of being toggled, the ICS-2100 Moduleware reports an error to Chromeleon and this error message appears.

To troubleshoot:

1. If a sequence is being executed, terminate the sequence by selecting

Batch > Stop in Chromeleon.

2. Try to toggle the valve from position A to position B by clicking the corresponding buttons on the ICS-2100 Control panel in Chromeleon (or by clicking the Valve_2 commands under Pump_ECD in the Commands dialog box).

3. Turn off the ICS-2100 power briefly and then restart.

4. If the problem persists, repeat Step 2

5. If the problem persists, contact Dionex for assistance.

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ICS-2100 Ion Chromatography System

SUPPRESSOR NOT CONNECTED

This error occurs if you turn on the suppressor and the ICS-2100 cannot establish a connection with the suppressor.

To troubleshoot:

1. Check the suppressor cable connection (see Section 5.11

2. If the error persists, contact Dionex for assistance. There may be a problem in the suppressor controller electronics. The ICS-2100 electronics components cannot be serviced by the user.

SUPPRESSOR OVER CURRENT

This error may be caused by an expended or dirty suppressor or by a malfunction in the suppressor controller electronics.

To troubleshoot:

1. Follow the instructions in the suppressor manual to regenerate the suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

2. Follow the instructions in the suppressor manual to clean the suppressor.

3. If a malfunction in the suppressor controller is suspected, contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user.

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4 • Troubleshooting

SUPPRESSOR OVER POWER

This error occurs when, in order to maintain the selected current, the ICS2100 is required to apply a higher voltage than the suppressor can support.

To troubleshoot:

1. Reduce the flow rate.

2. Rehydrate the suppressor. Refer to the suppressor manual for instructions. Suppressor manuals are included on the Dionex Reference Library CDROM (P/N 053891).

3. If the error persists, replace the suppressor (see Section 5.11

SUPPRESSOR OVER VOLTAGE

This error occurs if you turn on the suppressor but the ICS-2100 cannot establish a connection with the suppressor.

To troubleshoot:

1. Check the suppressor cable connection (see Section 5.11

2. If the error persists, replace the suppressor (see Section 5.11

SUPPRESSOR STOPPED FOR ZERO FLOW RATE

This error message appears when you click the Shutdown button on the ICS2100 Control panel in Chromeleon. The message also appears anytime you turn off the pump flow while the suppressor is on. The suppressor is automatically turned off to prevent damage to the suppressor.

To troubleshoot:

• If the pump stopped unexpectedly, see Section 4.6 for pump

troubleshooting information.

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ICS-2100 Ion Chromatography System

4.3 Liquid Leaks

• Leaking fitting

Locate the source of the leak. Tighten or, if necessary, replace the liquid line connection (see Section 5.3 Fittings (Document No. 031432) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

• Broken liquid line

Replace the line and fittings with the same length and internal diameter tubing (see Section 5.3

• Blocked or improperly installed line

Make sure the lines are not crimped or otherwise blocked. Also, if the b locked line is a waste line, make sure it is not elevated at any point after it exits the ICS-2100. If a line is blocked, replace it (see Section 5.2

• Loose pump check valve

1. Make sure the check valves are firmly seated in the pump head. If they are not, tighten them carefully with an open-end wrench just until the leak stops.

). Refer to Installation of Dionex Liquid Line

2. If the leak persists, replace the check valve (see Section 5.6

• Leaking seal wash port

Leaking from the seal wash port indicates a leaking piston seal. Replace the seal (see Section 5.7

• Damaged pump piston seal

1. Replace the piston seal (see Section 5.7

2. If the leak persists, replace the piston (see Section 5.8

• Pump head not tight against casting

Carefully tighten the pump head mounting nuts just until the leak stops. DO NOT OVERTIGHTEN!

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4 • Troubleshooting

• Leaking pressure transducer

1. Make sure the liquid line connections into the pressure transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No.

031432) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings.

2. If the pressure transducer continues to leak, contact Dionex for assistance. The pressure transducer cannot be serviced by the user.

• Leaking pump head waste valve

Make sure the waste valve is closed. To close the valve, turn the knob clockwise, and tighten fingertight. DO NOT OVERTIGHTEN!

Overtightening may damage the valve and the pump head.

If the leak persists, replace the waste valve O-ring (see Section 5.9

• Leaking suppressor

Refer to the suppressor manual for troubleshooting procedures. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

• Leaking injection valve or auxiliary valve

1. Make sure the liquid line connections to the transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings.

2. Liquid leaks from behind the valve stator may indicate a scratched rotor seal. Rebuild the valve (see Section 5.4

• Leaking detector cell

1. Check the waste lines for blockage; trapped particles can plug the lines and cause a restriction and/or leak. If necessary, clear the waste lines by reversing the direction of flow.

2. Make sure the plumbing downstream from the cell is clear; a blockage may overpressurize the cell, causing it to leak. If the problem continues, contact Dionex for assistance.

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ICS-2100 Ion Chromatography System

4.4 Pump Difficult to Prime or Loses Prime

Excessive pressure fluctuations (more than 3% difference from one pressure reading to the next) indicate that the pump is out of prime.

• Empty eluent reservoir and/or no eluent connected

Fill the reservoir. Make sure all connections are secure.

• Eluent improperly or insufficiently degassed

Check the vacuum degas settings:

1. Open the Chromeleon Server Configuration program. Right-click the

ICS-2100 device in the timebase and select Properties.

2. Select the Options tab (see Figure 4-1

Figure 4-1. ICS-2100 Server Configuration Properties: Options

3. Verify that the Degas check box is selected.

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Oritron ICS-2100 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1.1 Introduction to Ion Chromatography (IC)

1.2 Overview of the ICS-2100

1.3 About This Manual

1.3.1 Safety Messages and Notes

1.4 Safety and Regulatory Information

1.4.1 Safety Labels

2.1 Operating Features

2.1.1 Front Panel

2.1.2 Top Cover

2.1.3 Component Panel

2.1.4 Rear Panel

2.2 Flow Schematics

2.3 Chromeleon and Chromeleon Xpress

2.3.1 The Panel Tabset

2.3.2 Software Control Modes

2.3.3 System Wellness

2.4 System Component Details

2.4.1 Vacuum Degas Assembly (Optional)

2.4.2 Eluent V alve

2.4.3 Pump

2.4.4 Eluent Generator

2.4.5 Auxiliary Power Supply (Optional)

2.4.6 Injection Va lve

2.4.7 Auxiliary Valve (Optional)

2.4.8 Column Heater

2.4.9 Suppressor

2.4.10 DS6 Heated Conductivity Cell

3.1 Operation Overview

3.2 Turning On the System Power

3.3 Connecting to Chromeleon

3.4 Set Up the Eluent Reservoir

3.4.1 Filter the Deionized Water

3.4.2 Fill the Reservoir

3.4.3 Set the Eluent Level

3.4.4 Connect the Reservoir

3.5 Check All Connections

3.6 Prime the Pump

3.7 Set System Operating Conditions

3.8 Equilibrate the System and Verify Operational Status

3.9 Prepare Samples

3.9.1 Collecting and Storing Samples

3.9.2 Pretreating Samples

3.9.3 Diluting Samples

3.10 Loading and Injecting Samples

3.10.1 Loading Samples with a Syringe

3.10.2 Loading Samples with a Vacuum Syringe

3.10.3 Loading Samples with an Autosampler

3.10.4 Injecting Samples

3.11 Processing Samples

3.11.1 Manual Sample Processing

3.11.2 Automatic (Batch) Sample Processing

3.12 Maintenance

4.1 Error Messages

4.2 Troubleshooting Error Messages

4.3 Liquid Leaks

4.4 Pump Difficult to Prime or Loses Prime