Dionex ICS-900 Operator's Manual

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ICS-900 Ion Chromatography System

Operator’s Manual

Document No. 065215

Revision 02

September 2009

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

DISCLAIMER OF WARRANTY AND LIMITED WARRANTY

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

TRADEMARKS

AES, AMMS, Chromeleon, CMMS, and SRS are registered trademarks of Dionex Corporation. MMS, MicroMembrane, and OnGuard are trademarks of Dionex Corporation. Teflon and Tefzel are registered trademarks of E.I. du Pont de Nemours and Company. Microsoft, Windows 2000, and Windows XP are registered trademarks of Microsoft Corporation.

PRINTING HISTORY

Revision 01, March 2008 Revision 02, September 2009

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

1.1 Overview of the ICS-900 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.2 The ICS-900 Operator’s Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.2.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.3 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

1.3.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

1.3.2 Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

1.3.3 Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

2•Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.1.1 Front Door and Top Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.1.2 Component Mounting Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

2.1.3 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.2 Fluid Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.3 System Component Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

2.3.1 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

2.3.2 Pressure Transducer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

2.3.3 Injection Valve with Sample Loop . . . . . . . . . . . . . . . . . . . . . . 18

2.3.4 MMS 300 MicroMembrane Suppressor . . . . . . . . . . . . . . . . . . 19

2.3.5 Displacement Chemical Regeneration (DCR) . . . . . . . . . . . . . 20

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2.3.6 Conductivity Cell and DS5 Detection Stabilizer . . . . . . . . . . . .21

2.4 Chromeleon and Chromeleon Xpress Software . . . . . . . . . . . . . . . . . . .23

2.4.1 The Panel Tabset . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23

2.4.2 Software Control Modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .24

2.4.3 System Wellness and Predictive Performance . . . . . . . . . . . . .25

3 • Operation and Maintenance . . . . . . . . . . . . . . . . . . . . . . . .27

3.1 Operation Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27

3.2 Turning On the ICS-900 Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28

3.3 Connecting to Chromeleon or Chromeleon Xpress . . . . . . . . . . . . . . . .28

3.4 Preparing the Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29

3.5 Preparing the Regenerant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30

3.6 Priming the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .32

3.7 Equilibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35

3.8 Verifying Operational Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35

3.9 Configuring Standby Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .36

3.10 Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.10.1 Collecting and Storing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.10.2 Pretreating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.10.3 Diluting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38

3.11 Processing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39

3.11.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39

3.11.2 Manually Processing Samples . . . . . . . . . . . . . . . . . . . . . . . . . .40

3.11.3 Automatically Processing Samples (Batch Processing) . . . . . .42

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Contents

3.11.4 Loading and Injecting Samples with an Autosampler . . . . . . . 44

3.11.5 Loading and Injecting Samples with a Syringe . . . . . . . . . . . . 46

3.11.6 Example Chromeleon Commands for Loading and

Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48

3.12 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49

4 • Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

4.1 Alarms and Error Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51

4.2 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

4.3 Pump Difficult to Prime or Loses Prime . . . . . . . . . . . . . . . . . . . . . . . . 58

4.4 Pump Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

4.5 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

4.6 Erratic Flow/Pressure Reading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

4.7 Excessive System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

4.8 Peak “Ghosting” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

4.9 Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . . . 61

4.10 Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . . . 61

4.11 No Detector Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

4.12 High Detector Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62

4.13 Baseline Noise or Drift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63

5•Service. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

5.1 Diagnostics and Calibrations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

5.1.1 Opening the Wellness Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

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5.1.2 Wellness Panel Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .67

5.1.3 Calibrating the Pressure Transducer . . . . . . . . . . . . . . . . . . . . .69

5.1.4 Calibrating the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .70

5.1.5 Calibrating the Flow Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . .72

5.2 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73

5.3 Isolating a Restriction in the Liquid Plumbing . . . . . . . . . . . . . . . . . . . .74

5.4 Cleaning Eluent Bottles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .76

5.5 Changing the Sample Loop . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .76

5.6 Cleaning and Replacing Pump Check Valves . . . . . . . . . . . . . . . . . . . .77

5.7 Replacing a Pump Piston Seal and Backup Seal . . . . . . . . . . . . . . . . . .80

5.8 Replacing a Pump Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .86

5.9 Replacing the Waste Valve Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .87

5.10 Rebuilding the Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .88

5.11 Replacing the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .90

5.12 Replacing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .91

5.13 Changing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .92

A • Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93

A.2 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93

A.3 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93

A.4 Front and Rear Panel LEDs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .94

A.5 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .94

A.6 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95

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Contents

A.7 Suppressors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

A.8 Column Heater/Thermostat . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96

A.9 Conductivity Detector and Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . 96

A.10 Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

A.11 System Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

B • Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99

C • TTL and Relay Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

C.1 Connecting a TTL or Relay . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

C.2 Selecting TTL Input Control Modes and Functions . . . . . . . . . . . . . . 103

C.3 Configuring Relay Output 1 or 2 to Respond to the Pump Flow . . . . 106

C.4 Controlling TTL and Relay Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . 108

C.5 Controlling an AS40 Automated Sampler with a Relay . . . . . . . . . . . 110

D•FAQ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113

D.1 How do I connect to an autosampler? . . . . . . . . . . . . . . . . . . . . . . . . . 113

D.2 How often should I perform calibrations? . . . . . . . . . . . . . . . . . . . . . . 113

D.3 Why are the retention times moving? . . . . . . . . . . . . . . . . . . . . . . . . . 113

D.4 How do I adjust retention times? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

D.5 When should I remake standards? . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

D.6 When should I remake eluents? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

D.7 How do I start Chromeleon or Chromeleon Xpress? . . . . . . . . . . . . . 114

D.8 How do I back up data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

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D.9 How do I delete data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .114

D.10 How do I shut off the system? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115

D.11 How do I store columns? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115

D.12 How do I know when a column is dirty? . . . . . . . . . . . . . . . . . . . . . . .115

D.13 How do I clean a column? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115

D.14 Why is the conductivity high? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .115

E • Introduction to Ion Chromatography (IC) . . . . .117

F • Glossary. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .119

Index

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1.1 Overview of the ICS-900

The Dionex ICS-900 Ion Chromatography System (ICS-900) performs isocratic ion analyses using suppressed conductivity detection. The ICS-900 is an integrated ion chromatography system consisting of a pump, an injection valve, and a conductivity cell. Other system components (guard column, separator column, and suppressor) are ordered separately.

1 • Introduction

The ICS-900 is controlled with a PC running Windows and the Chromeleon later) or Chromeleon Xpress. The Chromeleon System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of Dionex chromatography instruments, but does not include data management capabilities.

For communication between the ICS-900 and the PC on which Chromeleon or Chromeleon Xpress is installed, the ICS-900 must be connected to a USB (Universal Serial Bus) port on the PC or a USB hub. For details, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document No.

065214). The manual is provided on the Dionex Reference Library CD-ROM (P/N 053891) and in the ICS-900 Ship Kit (P/N 067768).

NOTE For an introduction to basic ion chromatography

® Chromatography Management System (version 6.8 SP4 or

Chromatography Management

concepts, see Appendix E

® XP or Windows® 2000

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ICS-900 Operator’s Manual

1.2 The ICS-900 Operator’s Manual

1.2.1 Overview

The electronic version (i.e., PDF file) of the ICS-900 operator’s manual contains numerous hypertext links that can take you to other locations within the file. These links include:

• Table of contents entries

• Index entries

• Cross-references (underlined in blue) to sections, figures, tables, etc.

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

e® Acrobat® or Adobe Reader® for assistance.

Chapter 1 Introduction

Chapter 2 Description

Chapter 3 Operation and Maintenance

Chapter 4 Troubleshooting

Chapter 5 Service

Appendix A Specifications

Appendix B Reordering Information

Introduces the ICS-900; explains the conventions used in this manual, including safety-related information.

Describes ICS-900 operating features, the chromatographic flow path, and the software required for ICS-900 control.

Provides operating instructions for the ICS-900 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.

Provides specifications and installation site requirements for the ICS-900.

Lists spare parts for the ICS-900.

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1 • Introduction

Appendix C TTL and Relay Control

Appendix D FAQ

Appendix E Introduction to Ion Chromatography

Appendix F Glossary

Describes the ICS-900 TTL and relay control features.

Provides answers to frequently asked questions about ICS-900 operation.

Describes basic ion chromatography concepts.

Provides definitions of terms commonly used in ion chromatography.

1.3 Safety and Regulatory Information

The ICS-900 was manufactured by Dionex Corporation at the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The ICS-900 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of an ICS-900 in a manner not specified by Dionex may result in personal injury.

If there are questions regarding appropriate usage, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

1.3.1 Safety Messages and Notes

This manual contains warnings and precautionary statements that can prevent personal injury and/or damage to the ICS-900 when properly followed. Safety messages appear in bold type and are accompanied by icons, as shown below.

Indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury.

Indicates a potentially hazardous situation which, if not avoided, could result in death or serious injury.

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Indicates a potentially hazardous situation which, if not avoided, may result in minor or moderate injury. Also used to identify a situation or practice that may seriously damage the instrument, but will not cause injury.

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

Messages d'avertissement en français

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

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

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

Warnhinweise in Deutsch

Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen.

Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen.

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

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Notes

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

NOTE NOTES call attention to certain information. They

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

1.3.2 Safety Symbols

These symbols appear on the ICS-900 or on ICS-900 labels:

Alternating current

Primary protective conductor terminal

1 • Introduction

Secondary protective conductor terminal

Power supply is on

Power supply is off

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

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1.3.3 Declaration of Conformity

The cETLus and CE marks on the ICS-900 model/data label indicate that the ICS-900 is in compliance with the following standards.

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2.1 Operating Features

2.1.1 Front Door and Top Cover

Figure 2-1 illustrates the front door and top cover of the ICS-900 Ion

Chromatography System (ICS-900).

2 • Description

Status LEDs

Injection

Port

Figure 2-1. ICS-900 Ion Chromatography System

Eluent Bottle

Regenerant Bottle

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LEDs

Three status LEDs (described below) are on the ICS-900 front door.

LED Label If On (Green) If Flashing

Power ICS-900 power is on Does not flash Ready System check passed, but

sequence not yet started (LED stays on until run starts or sequence is aborted)

Run Running/acquiring data Error/alarm/fault (including

System check failed (occurs if system check executes for 10 minutes without success)

injection valve position)

Other status information and alarm messages are displayed in the Audit Trail in Chromeleon or Chromeleon Xpress. For a description of these messages, see Section 4.1

Injection Port

The injection port can be connected to the injection valve inside the ICS-900. The sample to be analyzed is injected into the injection port using a syringe. For automated sample injections, the ICS-900 injection valve can be connected to an autosampler, instead of to the injection port. For more information about sample injection, see Section 3.11.5

Eluent and Regenerant Bottles

The ICS-900 top cover is molded to hold one eluent bottle assembly (P/N 062510) and one regenerant bottle assembly (anion, P/N 068222; cation, P/N 068223).

• Eluent carries the sample through the ICS-900 and facilitates the ion

separation process. The type of eluent used depends on the analyses

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performed. For example, an ICS-900 configured for anion analyses

uses carbonate eluent, while an ICS-900 configured for cation analyses uses methanesulfonic acid (MSA) eluent.

• Regenerant renews the suppressor’s ability to suppress eluent

conductivity. An ICS-900 configured for anion analyses uses dilute sulfuric acid regenerant. An ICS-900 configured for cation analyses uses tetrabutylammonium hydroxide (TBAOH) regenerant. For more information about suppressor regeneration, see Section 2.3.5

2.1.2 Component Mounting Panel

Figure 2-2 shows the components installed on the component panel

behind the ICS-900 front door.

2 • Description

Conductivity Cell

(Housed in DS5 Detection Stabilize

MMS 300

Suppressor

Separator Column

Pump Heads

Pressure

Transducer

Injection Valve

Tubing Chase

Guard Column

Backpressure

Tub ing

Figure 2-2. ICS-900 Component Mounting Panel

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Conductivity Cell

The flow-through heated conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. A heat exchanger inside the cell regulates the temperature to 40 °C (104 °F). The cell is housed inside a DS5 Detection Stabilizer (P/N 067761). For details about the conductivity cell and DS5 Detection Stabilizer, see

Section 2.3.1

MMS™ 300 MicroMembrane Suppressor

The MMS 300 suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. For details about the MMS 300 suppressor, see Section 2.3.4

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.

Pressure Transducer

The pressure transducer measures the system backpressure. See

Section 2.3.2

Pump Heads

for details about the pressure transducer.

The ICS-900 includes a dual-piston serial pump. The flow rate can be set from 0.01 mL/min to 5.00 mL/min. However, for optimum performance, set the flow rate to between 0.20 and 3.00 mL/min. Setting the flow rate to 0.00 mL/min turns off the pump. For details about the pump, see

Section 2.3.1

Injection Valve

The injection valve is a six-port, electrically-activated valve. For details about the injection valve, see Section 2.3.3

10 Doc. 065215-02 9/09

Tubing Chase

The tubing chase routes tubing from the component panel, through the ICS-900 interior, to the rear panel.

2.1.3 Rear Panel

Figure 2-3 illustrates the ICS-900 rear panel.

2 • Description

USB Connector

Link LED

TTL and Relay

Connector

Fuse Holder,

Power Switch, and Power Receptacle

Plumbing and

Waste Lines

Figure 2-3. ICS-900 Rear Panel

USB Connector

The USB connector connects the ICS-900 to the PC on which Chromeleon or Chromeleon Xpress is installed. For the standard system configuration of one ICS-900 connected to a PC, connect a USB cable between the USB connector on the ICS-900 and a USB port on the PC. For detailed connection instructions, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document

Doc. 065215-02 9/09 11

ICS-900 Operator’s Manual

No. 065214), provided on the Dionex Reference Library CD-ROM (P/N 053891) and in the ICS-900 Ship Kit (P/N 067768).

Link LED

The Link LED indicates the communication status between the ICS-900 and the PC on which

Link

Chromeleon or Chromeleon Xpress is installed.

LED Status Description

On The ICS-900 and the PC are linked, but no data is currently

being transmitted or received

Flashing The ICS-900 and the PC are linked and data is being

transmitted

Off The ICS-900 and the PC are not currently linked

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 the pump on and off, and perform an autozero command. For connection instructions, see

Appendix C

Fuse Holder, Power Switch, and Power Receptacle

• The fuse holder contains two fast-blow IEC 127 fuses rated 3.15 A

(P/N 954745). For instructions on how to change the fuses, see

Section 5.13

• The power switch provides on/off control of power to the ICS-900.

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

The power supply cord is used as the main disconnect device. Make sure the socket-outlet is located near the ICS-900 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.

12 Doc. 065215-02 9/09

2 • Description

Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht zugänglich ist.

Plumbing and Waste Lines

The following lines exit the ICS-900 through the tubing chase on the lower left corner of the rear panel.

• Eluent

• Regenerant

• Cell outlet

• Waste (sample, regenerant, and pump priming)

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ICS-900 Operator’s Manual

2.2 Fluid Schematic

Figure 2-4 shows the flow path through the ICS-900.

To pump inlet

From cell outlet

Backpressure Coil

(1 or 2, depending on flow rate)

Conductivity Cell

(in DS5 Detection Stabilizer)

Regen Out Eluent Out

Eluent In

Secondary

MMS 300

Pulse Damper

Primary

Pump

Heads

Regen In

Transducer

Eluent

To cell inlet

To MMS Regen In

Pressure

Injection

Valve

Regenerant

Eluent in from pulse damper

Sample in

To Waste

Figure 2-4. ICS-900 Flow Schematic

14 Doc. 065215-02 9/09

2 • Description

Liquid flows through the ICS-900 along the following flow path. Refer to

Figure 2-4

for the flow path number locations.

• Eluent from the eluent bottle is drawn into the pump . The pump pushes

the eluent through the pressure transducer , which measures the system pressure, and through a pulse damper , which smooths minor pressure

1 2

variations from the pump to minimize baseline noise.

• The eluent then flows into the injection valve . After sample is loaded into

the sample loop and the injection valve is toggled to the Inject position, eluent passes through the sample loop pushing the sample into the eluent stream.

• The eluent/sample mixture is pumped through the guard and separator

columns , where the ions are separated by the ion exchange process.

• The eluent/sample mixture then flows through the suppressor , which

suppresses the conductivity of the eluent and enhances the conductivity of the analyte. Regenerant flows continuously through the suppressor, restoring the ion exchange sites to their original state.

• The eluent/sample mixture then flows through the conductivity cell , where

the analytes are detected. A signal is produced and sent to Chromeleon or Chromeleon Xpress software.

• Finally, the eluent flows out of the cell and into the regenerant bottle , where

it pressurizes the regenerant and forces it into the suppressor.

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ICS-900 Operator’s Manual

2.3 System Component Details

2.3.1 Pump

The ICS-900 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 2-5

pump, are located on the bottom (inlet) and top (outlet) of the primary pump head.

Secondary

Pump Head

). The check valves, which prevent reverse flow through the

Outlet Check Valve

Primary Pump Head

Waste Valve

Inlet Check Valve

Figure 2-5. ICS-900 Pump Components

Secondary Pump Head

The secondary pump head delivers eluent to the pressure transducer. The waste valve is located on the front of the secondary pump head (see

Figure 2-5

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

16 Doc. 065215-02 9/09

2.3.2 Pressure Transducer

The pressure transducer measures the system pressure at the point that the eluent flows from the pump head outlet check valve. Pressure readings indicate that the pumping system is delivering smooth, accurate flow. Pressure readings can be monitored from Chromeleon or Chromeleon Xpress.

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 Properties dialog box or in the Chromeleon or Chromeleon Xpress program). For troubleshooting information if a pressure limit is exceeded, see Section 4.7

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.

2 • Description

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ICS-900 Operator’s Manual

2.3.3 Injection Valve with Sample Loop

The injection valve is a six-port, electrically-activated Rheodyne valve. A 10 μL sample loop (P/N 042949) is installed on the valve at the factory. The valve has two operating positions: Load and Inject. Eluent flows through either the Load or Inject path, depending on the valve position.

From Pump

To Column

Figure 2-6

LOAD POSITIONINJE

shows flow schematics for the valve.

T POSITION

From Pump

Sample Loop

Sample In

Figure 2-6. Injection Valve Flow Schematics

To Waste

= Sample

= Eluent

Sample InTo Column

To Waste

• In the Load position, sample is loaded into the sample loop, where it

is held until injection. Eluent flows from the pump, through the valve, and to the column, bypassing the sample loop. Sample flows from the syringe or autosampler line (if installed), through the valve, and into the sample loop. Excess sample flows out to waste.

• In the Inject position, sample is swept to the column for analysis.

Eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it.

Section 3.11.2 Section 3.11.3

18 Doc. 065215-02 9/09

describes how to inject samples manually; describes how to inject samples with an autosampler.

2.3.4 MMS 300 MicroMembrane Suppressor

The MMS 300 suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity.

2 • Description

As illustrated in Figure 2-7

, a constant flow of regenerant over the membrane continually restores the suppression ability of the MMS 300.

A process called Displacement Chemical Regeneration (DCR) pushes regenerant from the regenerant bottle through the suppressor. See

Section 2.3.5

for details.

For more information about the MMS 300, refer to the suppressor manual. Suppressor manuals are included on the Dionex Reference Library CDROM (P/N 053891).

Figure 2-7. MMS 300 Suppressor Flow

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ICS-900 Operator’s Manual

2.3.5 Displacement Chemical Regeneration (DCR)

Displacement Chemical Regeneration (DCR) is the process that restores the ability of the MMS 300 suppressor to suppress eluent. In DCR, the eluent that exits the cell is pumped into the regenerant bottle. The eluent pressurizes the bottle and pushes the regenerant into the suppressor. However, because the eluent is a different density than the regenerant, it remains separate.

In the anion DCR process (see Figure 2-8

), the eluent is less dense than the regenerant and it remains on the top of the bottle, forcing the regenerant into the regenerant line at the bottom of the bottle and out into the suppressor.

In the cation DCR process (see Figure 2-9

), the eluent is denser than the regenerant and it flows to the bottom of the bottle. This displaces the regenerant, pushing regenerant out of the regenerant line at the top of the bottle and out into the suppressor.

Regen In

Used eluent out to regenerant reservoir

(in DS5 Detection Stabilizer)

Regen Out Eluent Out

Eluent In

Conductivity Cell

AMMS 300

Regen In

Eluent out to cell

Regenerant in from reservoir

Used

Regen Bottle Out

Eluent

Anion

Regenerant

Eluent in from column

Regenerant out to waste

Figure 2-8. Anion ICS-900 Displacement Chemical Regeneration (DCR)

20 Doc. 065215-02 9/09

Regen In

2 • Description

Used eluent out to regenerant reservoir

Conductivity Cell

(in DS5 Detection Stabilizer)

Regen Out Eluent Out

Eluent In

Regenerant out to waste

CMMS 300

Regen In

Eluent in from column

Eluent out to cell

Regenerant in from reservoir

Cation

Regenerant

Regen Bottle Out

Used

Eluent

Figure 2-9. Cation ICS-900 Displacement Chemical Regeneration (DCR)

Connections to the regenerant bottle differ depending on whether the system will run an anion or a cation application. Regenerant bottles for each type of application are available (anion regenerant bottle assembly, P/N 068222; cation regenerant bottle assembly, P/N 068223). For detailed installation instructions, refer to the DCR Kit Installation Instructions (Document No. 031664), provided on the Dionex Reference Library CDROM (P/N 053891).

2.3.6 Conductivity Cell and DS5 Detection Stabilizer

The flow-through heated conductivity cell contains two 316 stainless steel electrodes that are permanently sealed into the PEEK cell body. The cell measures the electrical conductance of analyte ions as they pass through the cell.

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.

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ICS-900 Operator’s Manual

In ion analysis, the effect of temperature variation is minimized by suppressing eluent conductivity. Built-in preset temperature compensation also ensures that there is no major change in the baseline or in peak heights. Temperature compensation stability.

Direct conductive heating is used in the ICS-900 conductivity cell to provide temperature control and compensation. A heat exchanger inside the ICS-900 cell regulates the temperature. All data is collected at 40 °C (104 °F).

The cell is housed inside a DS5 Detection Stabilizer (P/N 067761) (see

Figure 2-10

temperature.

), which helps to insulate the cell from fluctuations in ambient

further improves baseline

Cell Inlet

From suppressor

Cell Outlet

To r egenerant reservoir

Conductivity Cell

Connector to component

mounting panel

ELUENT OUT por

Figure 2-10. Conductivity Cell and DS5 Detection Stabilizer

The conductivity cell has two detection limit ranges: 0 to 500 10,000 for the application. The default range of 0 to 500

μS. Select the range depending on the expected detector readings

μS is appropriate for

μS or 0 to

most applications. The detection limit range is set in the Properties dialog box of the Chromeleon Server Configuration program. For details, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document No. 065214), provided on the Dionex Reference Library CDROM (P/N 053891) and in the ICS-900 Ship Kit (P/N 067768).

22 Doc. 065215-02 9/09

2 • Description

2.4 Chromeleon and Chromeleon Xpress Software

The ICS-900 is controlled by a PC configured with Chromeleon Chromatography Management System or Chromeleon Xpress. Chromeleon Management System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of Dionex chromatography instruments, but does not include data management capabilities.

2.4.1 The Panel Tabset

The Chromeleon and Chromeleon Xpress panel tabset provides a centralized location for controlling system functions. A panel tabset for an ICS-900 system typically includes the following Control panels:

• An ICS-900 Control panel (see Figure 2-11) provides access to

ICS-900 functions. The label on the tab for this panel is the name of the timebase in which the ICS-900 is configured.

Chromatography

Figure 2-11. ICS-900 Panel on the Panel Tabset

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ICS-900 Operator’s Manual

• A Sequence Control provides controls for defining and running

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 provides access to autosampler functions.

This panel is present only if the timebase in which the ICS-900 is configured includes an autosampler.

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 Tab se t.

• If Chromeleon Xpress is

installed, start the application; this automatically displays the ICS-900 panel tabset.

2.4.2 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.

24 Doc. 065215-02 9/09

2 • Description

2.4.3 System Wellness and Predictive Performance

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

Predictive Performance provides functions for monitoring the usage of replaceable parts and for planning service procedures. Predictive Performance lets you monitor the following functions:

• The number of hours the ICS-900 has been in use

• The number of times the injection valve has cycled

• The number strokes performed by the pump pistons

• The estimate of the amount of wear to the piston seal

• The volume of eluent pumped through the suppressor and column

You can set limits for injection valve cycles, piston strokes, piston seal wear, suppressor usage, and column usage. Two limits can be set for each parameter. When the first limit is reached, a warning message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail. When the second limit is reached, an error message is displayed in the Audit Trail. After replacing a part, reset the limit counters to zero.

Different applications cause different rates of wear on the consumable parts in your instrument. Experience will help you determine the appropriate limits to set to predict when the next maintenance will be required.

Predictive Performance commands and parameters are available in the Commands dialog box in Chromeleon or Chromeleon Xpress. To open the Commands dialog box, press F8. Expand the list of commands under Pump_ECD and scroll to the Predictive Performance commands

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ICS-900 Operator’s Manual

(InjectValveCycles, PumpPistonStrokes, SealWear, SuppressorVolume, ColumnVolume) (see Figure 2-12

Figure 2-12. Predictive Performance Commands: InjectValveCycles

If you do not wish to receive these warning or error messages, you can disable them by setting the Warning and Limit parameter for each Predictive Performance function to Off.

26 Doc. 065215-02 9/09

3 • Operation and Maintenance

This chapter describes routine operating and maintenance procedures for the ICS900 Ion Chromatography System (ICS-900).

3.1 Operation Overview

Figure 3-1 illustrates the basic steps for routine operation of the ICS-900.

Turn on the ICS-900

power

Connect to

Chromeleon

Prepare the eluent

and regenerant

Prime the pump

Equilibrate the

system

Prepare samples

Process samples

Figure 3-1. ICS-900 Operation Flow Chart

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ICS-900 Operator’s Manual

3.2 Turning On the ICS-900 Power

Press the power switch on the ICS-900 rear panel (see Figure 2-3) to turn on the system power. These are the conditions at power-up:

• The pump is off.

• The injection valve is in the Load position.

• The conductivity detector begins reading the current conductivity.

3.3 Connecting to Chromeleon or Chromeleon Xpress

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 and

select All Programs (or 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 (or Programs) > Chromeleon > Chromeleon.

4. If Chromeleon is installed, 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-900 Control panel, select the tab labeled with the ICS-900 timebase name (see Figure 3-2

28 Doc. 065215-02 9/09

3 • Operation and Maintenance

Figure 3-2. ICS-900 Control Panel on Panel Tabset

3.4 Preparing the Eluent

1. Prepare the eluent. For instructions refer to the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N

053891).

2. Fill the eluent bottle with the prepared eluent, insert the stopper assembly tubing into the bottle, and hand tighten the cap.

Set the Eluent Level

After filling the bottle, move the Eluent Remaining slider on the ICS-900 Control panel (see Figure 3-3) to indicate the volume of liquid in the bottle.

The ICS-900 determines the eluent usage by monitoring the flow rate and the length of time the pump is on. As the eluent is used up, the ICS-900 updates the

Eluent Remaining slider and gauge. A warning appears in the Audit Trail when

the level falls below 200 mL, and then again when the level falls bellow 100 mL.

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ICS-900 Operator’s Manual

For the eluent level to be accurate, you must enter the level each time the bottle is filled.

Figure 3-3. Setting the Eluent Level

3.5 Preparing the Regenerant

After filling the eluent bottle, move the slider to indicate the volume of liquid in the bottle

Note: The Eluent Remaining slider and gauge are updated as the liquid is used up.

The type of regenerant used with the ICS-900 depends on the type of analysis to be run. A dilute sulfuric acid regenerant is used for anion analyses; a tetrabutylammonium hydroxide (TBAOH) regenerant is used for cation analyses. Follow the instructions below to prepare either anion or cation regenerant.

Use ASTM Type I (18 megohm-cm) filtered and deionized water to prepare the regenerant.

1. Verify that you have the correct regenerant bottle assembly (P/N 068222 for anion analyses; P/N 068223 for cation analyses):

• For anions, verify that the cap is labeled ANION and the REGEN BOTTLE

line extends to the bottom of the bottle.

OUT

• For cations, verify that the cap is labeled CATION and the REGEN BOTTLE

OUT line extends only about 1 cm (0.4 in) into the bottle.

2. Rinse the regenerant bottle with deionized water.

3. Fill the bottle about halfway with deionized water.

30 Doc. 065215-02 9/09

3 • Operation and Maintenance

4. Determine the regenerant concentration required for the application. To estimate the regenerant concentration required for an eluent strength, use the following formulas:

Anion Regenerant Concentration = (mM eluent) x 2 Cation Regenerant Concentration = (mM eluent) x 5

For example, if you are using 20 mM methanesulfonic acid (MSA) as the eluent for cation analysis, use a regenerant concentration of 100 mM tetrabutylammonium hydroxide (TBAOH).

For additional details, refer to the Displacement Chemical Regeneration (DCR) kit installation instructions and the suppressor manual.

5. Empty the required amount of concentrate (sulfuric acid for anions; TBAOH for cations) into the bottle.

For acid concentrates (such as the anion regenerant), always pour the concentrate into deionized water, not into the empty bottle.

Pour les concentrés acides (comme le régénérant anionique), versez toujours le concentré dans de l'eau désionisée et non dans le réservoir vide.

Gießen Sie säurehaltige Konzentrate (beispielsweise den Anionregenerenten) das Konzentrat immer in entionisiertes Wasser und nicht in den leeren Behälter.

6. Fill the bottle almost to the top with deionized water and then place the bottle in the tray on the top of the ICS-900.

NOTE To avoid staining the ICS-900, be careful not to spill

TBAOH on the instrument.

7. Using the concentrate bottle, pour additional deionized water into the bottle until it is completely filled to the top. If a few drops spill over, then it is full enough.

The regenerant bottle must be filled all the way to the top at all times.

8. Insert the stopper assembly tubing into the bottle and hand-tighten the cap.

9. Invert the bottle three or four times to disperse the concentrate.

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ICS-900 Operator’s Manual

After the analysis begins, do not mix the contents of the regenerant bottle.

10.Verify that the liquid lines from the ELUENT and REGEN bottles are

connected to the corresponding lines from the ICS-900 (see Figure 3-4

ELUENT Bottle Out

Figure 3-4. Eluent and Regenerant Bottle Liquid Line Connections

3.6 Priming the Pump

Prime the pump if the eluent has been changed, the eluent line contains air, or the pump heads are dry (for example, after servicing).

NOTE If the eluent line is empty or the pump heads are

completely dry, you can use a 10 cc syringe (P/N 054578) to prime the pump (see page 34

REGEN

Bottle In

REGEN Bottle Out

1. Verify that the ELUENT and REGEN bottles are filled, the bottle caps are

installed and hand-tightened, and the liquid lines are connected to the bottles.

2. Verify that the waste lines are directed to a waste container.

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3 • Operation and Maintenance

3. Open the waste valve on the secondary (left) pump head by turning the knob one-half turn counterclockwise (see Figure 3-5 eluent flow path to waste and eliminates backpressure.

Secondary

Pump Head

Waste Valve

(Open)

Figure 3-5. Priming the Pump

). Opening the valve directs the

4. Click

Prime on the ICS-900 Control panel (see Figure 3-2), or open the

Commands dialog box (press F8), select the Pump command, and select the Prime option. The pump will begin pumping at approximately 3 mL/min.

5. Continue priming the ICS-900 until no air bubbles are exiting the pump waste line.

6. Click

Pump Off.

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

NOTE A convenient way to verify that the waste valve is closed

is to select the pump flow rate required for your application, turn on the pump, and then close the valve. The pressure should rise to the value expected for the application and quickly stabilize.

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Priming the Eluent Line with a Syringe (Optional)

A syringe can be used to facilitate priming when the eluent line is empty or the pump heads are completely dry.

1. Verify that the pump is turned off.

2. Disconnect the waste line from the luer fitting on the secondary (left) pump head and connect a 10 mL syringe (P/N 054578) to the luer fitting (see

Figure 3-6

Secondary

Pump Head

Waste Valve

(Open)

Luer Fitting

Figure 3-6. Priming the Eluent Lines

10 mL Syringe (P/N 054578)

3. Open the waste valve by turning it one-half turn counterclockwise.

4. Draw the syringe back to begin removing air from the flow path.

NOTE When the line already contains liquid, the syringe will be

difficult to draw back. In this case, prime with the prime command only (see Section 3.6

5. When a small amount of liquid enters the syringe, remove the syringe from the luer fitting, and reconnect the waste line to the luer fitting.

6. Follow the instructions in Section 3.6

34 Doc. 065215-02 9/09

to finish priming.

3.7 Equilibrating the System

1. Turn on the pump and run at the flow rate recommended for the column.

2. Allow the system to equilibrate. The ICS-900 Control panel displays the background conductivity (the conductivity of the eluent without the offset performed by the autozero command).

3. Offset the background and zero the conductivity reading by clicking the

Autozero

4. Monitor the system pressure to make sure it is at the expected pressure for the installed column (refer to the column manual for details) and is stable. Column manuals typically provide pressure specifications for systems that do not include a guard column. Expect the ICS-900 system pressure (with a guard column) to be 15% to 20% higher than the specification in the column manual.

• If the pressure is less than expected, air may be trapped in the system.

button on the ICS-900 Control panel.

Release the air by temporarily removing the pump fitting (P) on the injection valve. Allow the air to escape, and then reconnect the fitting.

3 • Operation and Maintenance

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

plumbing. Refer to the Section 4.7

5. Check for leaks in the regenerant bottle.

6. Check that liquid is flowing out of the suppressor

7. Monitor the baseline conductivity. In general, it should be <30 set up for anion analyses, and <2 Equilibration time varies and it can take some time to reach these expected values.

If the conductivity is too high, see Section 4.12 information. If the baseline is drifting or has excessive “noise” (large fluctuations in readings), see Section 4.13

μS for a system set up for cation analyses.

3.8 Verifying Operational Status

After the system has equilibrated, verify the actual pump pressure and stability by monitoring the pump pressure. Record the short-term pressure fluctuations; they should be less than 0.13 MPa (20 psi). If the pressure fluctuates by more than this amount, prime the pump (see Section 3.6

for troubleshooting information.

REGEN OUT waste line.

μS for a system

for troubleshooting

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ICS-900 Operator’s Manual

3.9 Configuring Standby Mode

You can configure the ICS-900 to enter standby mode after a period of inactivity (a period of time in which no data collection and no input from Chromeleon or Chromeleon Xpress has occurred). In standby mode, the pump flow rate is reduced.

To configure standby mode:

1. Start the Chromeleon Server Configuration program (click Start on the Windows taskbar and select All Programs (or Programs) > Chromeleon > Server Configuration).

2. Right-click the ICS-900 device in the timebase and select Properties.

3. Click Options (see Figure 3-7

Figure 3-7. ICS-900 Properties Dialog Box: Options Tab Page

4. Enter the desired Standby Flow Rate and select the Inactivity Time Out Period. If you select (0, Off), the ICS-900 does not enter standby mode when

it is idle.

To cancel standby mode and return the pump to the normal flow rate, either turn on the pump from the ICS-900 Control panel or start a new sequence.

36 Doc. 065215-02 9/09

3.10 Preparing Samples

NOTE Sample preparation can be performed while the system

is equilibrating.

3.10.1 Collecting and Storing

Collect samples in high density polyethylene containers that have been thoroughly cleaned with ASTM Type I (18 megohm-cm) filtered and deionized water. Do not clean containers with strong acids or detergents because these will 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.

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 • Operation and Maintenance

°C (39 °F) will reduce, but not

3.10.2 Pretreating

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.

A Dionex High Pressure Inline Filter (P/N 044105) is available for removing particulates down to 0.45 micron from samples. Connect the inline filter between the autosampler outlet and the sample inlet port on the injection valve. For details, see the printed installation instructions provided with the inline filter.

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

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cartridges. For instructions, refer to Installation and Troubleshooting Guide for OnGuard Cartridges (Document No. 032943). The manual is

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

3.10.3 Diluting

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 Type I (18 megohm-cm) filtered and 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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3.11 Processing Samples

3.11.1 Overview

Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-8 manual and batch sample processing.

3 • Operation and Maintenance

shows the typical steps for

Manual Sample

Processing

Load the sample

Autozero

Start data

acquisition

Inject the sample

Monitor

chromatogram

Stop data

acquisition

Batch Sample

Processing

Create a program*

Create a sequence

Load the

sequence

Start the batch

*Includes commands

for sample loading, autozero, injection, and data acquisition.

Figure 3-8. Sample Processing Overview

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ICS-900 Operator’s Manual

3.11.2 Manually Processing Samples

To manually process a sample, select operating parameters and commands from the Chromeleon or Chromeleon Xpress panel tabset. Commands are executed as soon as they are entered.

Summary of Manual Sample Processing

1. Complete the instructions in Section 3.2 through Section 3.10 to prepare the ICS-900 for operation and to prepare the sample for processing.

2. Load the sample into the injection valve sample loop with an autosampler (see Section 3.11.4

) or a syringe (see Section 3.11.5).

3. On the ICS-900 Control panel, click the Autozero

button.

4. On the Sequence Control panel, click the Acq On button (or click the Acquisition On/Off button on the Chromeleon toolbar).

5. Switch the injection valve to the Inject position. The method used to switch the injection valve depends on whether you are using an autosampler (see Section 3.11.4

) or a syringe (see Section 3.11.5).

6. The signal plot is displayed on the ICS-900 Control panel (see

Figure 3-9

). Monitor the chromatogram and when sample data has

been collected, click the Acq Off button on the Sequence Control

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3 • Operation and Maintenance

panel (or click the Acquisition On/Off button on the Chromeleon toolbar).

Figure 3-9. Manual Data Acquisition

Saving Manual Data

NOTE Chromeleon Xpress does not allow data to be saved.

If you are using Chromeleon, data from manual processing is saved in the manual sequence under the timebase folder in the local datasource.

To save the data from a manual run:

1. Select the manual folder and select File>Save As.

2. Enter a new name for the sequence.

3. Select the Save raw data check box.

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ICS-900 Operator’s Manual

4. Click Save.

3.11.3 Automatically Processing Samples (Batch 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-900 and autosampler (if installed), and for acquiring sample data.

• A quantification method for peak identification and area

determination. The quantification method is not included with Chromeleon Xpress.

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

injection volume, etc.).

After creating the sequence, you can start batch processing.

Summary of Automatic Sample Processing

1. Complete the instructions in Section 3.2 through Section 3.10 to prepare the ICS-900 for operation and to prepare the samples 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-900 front door (see Section 3.11.5

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.

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3 • Operation and Maintenance

b. Select an application template from the list (see Figure 3-10).

Figure 3-10. Application Wizard

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

and click Open.

c. Click Start Batch.

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3.11.4 Loading and Injecting Samples with an Autosampler

1. Verify that the autosampler output line is connected to port S (5) on the injection valve. Direct the injection valve waste line as required for the installed autosampler model.

For details about connecting an autosampler, refer to the ICS-900 Installation Instructions (Document No. 065214) and the autosampler operator’s manual. The manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). The ICS-900 Installation Instructions are also included in the ICS-900 Ship Kit (P/N 067768).

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. Use one of the following methods to load sample into the injection valve sample loop and inject it onto the column:

• Automatically: Include the Load and Inject commands in a

Chromeleon or Chromeleon Xpress program. See the examples in

Section 3.11.6

processing samples.

. See Section 3.11.3 for details about automatically

• Manually with an AS40: Start the AS40 load cycle (either

manually or with a relay). When the AS40 load cycle is complete, click the Inject button on the ICS-900 Control panel (see

Figure 3-11

processing samples.

Figure 3-11. ICS-900 Control Panel Load and Inject Buttons

). See Section 3.11.2 for details about manually

• Manually with an AS or AS-DV: Click the Inject icon on the

Chromeleon tool bar or select Control>Inject. On the Inject dialog box, enter the Position and Vo lu me and click OK.

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3 • Operation and Maintenance

Autosampler Setup Notes

Follow the steps below to verify that the ICS-900 injection valve is controlled by the correct device.

1. Open the Chromeleon Server Configuration program.

2. Open the ICS-900 Properties dialog box and click Inject Valve.

3. Under Controlled by, check the device selected for Pump_InjectValve:

• For an AS or AS-DV, verify that the AS is shown (see

Figure 3-12

Figure 3-12. ICS-900 Properties: Inject valve controlled by AS

• For an AS40, verify that the ICS-900 is shown (see Figure 3-13).

Figure 3-13. ICS-900 Properties: Inject Valve Controlled by ICS-900

4. To change the controlling device, select the Pump_InjectValve name and press the F2 key. On the Device Configuration dialog box, select the correct device from the Controlled By list. Click OK.

5. For an AS40, also verify that there is a relay connection from the AS40 Load relay to the ICS-900 RELAY OUT 1. Refer to the connection instructions in Section C.5

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for details.

ICS-900 Operator’s Manual

3.11.5 Loading and Injecting Samples with a Syringe

This section describes two methods for loading sample into the injection valve sample loop with a syringe:

• Loading sample with a syringe through the sample loading port on the

front of the ICS-900 (push method)

• Loading sample with a vacuum syringe through the sample loading

port on the front of the ICS-900 (pull method)

NOTE For instructions on how to load and inject

samples with an autosampler, see Section 3.11.4

Loading Samples with a Syringe (Push Method)

1. Verify that the sample loading port on the front of the ICS-900 is connected to sample port

Figure 3-14

2. Fill a syringe with a calibration standard or sample.

S (5) on the injection valve (see

3. Insert the syringe into the sample loading port on the front of the ICS-900.

4. Verify that the injection valve is in the Load position. If it is not, click the Load button on the ICS-900 Control panel (see Figure 3-11

5. Overfill the sample loop with five sample loop volumes. Remember that the line from the syringe to the valve must be filled first before the sample loop can be filled. Excess sample will exit through the injection valve waste line.

6. Leave the syringe in the port. This prevents the sample from siphoning out of the loop before injection.

7. Use one of the following methods to inject the sample onto the column:

• Manually: Click the Inject button on the ICS-900 Control panel.

See Section 3.11.2

for details about manually processing samples.

• Automatically: Include the Inject command in a Chromeleon or

Chromeleon Xpress program. See the examples in Section 3.11.6 See Section 3.11.3 samples.

for details about automatically processing

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3 • Operation and Maintenance

Loading Samples with a Vacuum Syringe (Pull Method)

1. Verify that the sample loading port on the front of the ICS-900 is connected to sample port

Figure 3-14

S (5) on the injection valve (see

2. Disconnect the waste line from port

W (6) on the injection valve and

attach a shorter line: 25 to 30 cm (10 to 12 in) of PEEK or Teflon® tubing (see Figure 3-14

3. Place the free end of this line into the sample.

4. Verify that the injection valve is in the Load position. If it is not, click the Load button on the ICS-900 Control panel (see Figure 3-11

5. Insert a syringe into the sample loading port on the front door and pull out the plunger to draw the sample into the injection valve. Draw at least five times the sample loop volume. Remember that the line from the sample to port

W (6) on the injection valve must be filled first

before the sample loop can be filled.

Syringe

Sample

Loading Port

(on front door)

(4)(5)

(3)

(2)

Sample

(6)

(1)

Injection Valve

Figure 3-14. Loading Sample with a Vacuum Syringe (Pull Method)

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ICS-900 Operator’s Manual

6. Use one of the following methods to inject the sample onto the column:

• Manually: click the Inject button on the ICS-900 Control panel.

See Section 3.11.2

for details about manually processing samples.

• Automatically: Include the Inject command in a Chromeleon or

Chromeleon Xpress program. See the examples in Section 3.11.6 See Section 3.11.3

for details about automatically processing

samples.

3.11.6 Example Chromeleon Commands for Loading and Injecting Samples

The following examples show commands for loading and injecting samples using an AS, AS-DV, or AS40 autosampler.

Example AS Program Commands

0.000 Pump_ECD.Autozero ;Zero the baseline.

Load ;Switch the valve to Load.

Wait CycleTimeState ;Wait for cycle time (if any).

Inject ;Switch the valve to Inject.

Wait InjectState ;Wait for injection to complete.

ECD_1.AcqOn ;Start data acquisition.

14.000 ECD_1.AcqOff ;Stop data acquisition.

Example AS-DV Program Commands

Sampler.LoadPosition ;Switch the valve to Load.

DeliverSample ;Deliver sample to the valve.

0.000 Autozero ;Zero the baseline.

Wait CycleTimeState ;Wait for cycle time (if any).

Inject ;Switch the valve to Inject.

ECD_1.AcqOn ;Start data acquisition.

14.000 ECD_1.AcqOff ;Stop data acquisition.

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3 • Operation and Maintenance

Example AS40 Program Commands

-2.300 Pump_ECD_Relay_1.Closed Duration=138.00 ;Note 1

0.000 Pump_ECD.Autozero ;Note 2

ECD_1.AcqOn ;Note 3

Pump_InjectValve.InjectPosition Duration=30.00 ;Note 4

30.00 ECD_1.AcqOff ;Note 5

AS40 Program Command Notes:

1. Close the ICS-900 RELAY OUT 1, which is connected to the AS40

LOAD relay. This signals the AS40 to load the sample.

2. Zero the baseline.

3. Start data acquisition.

4. Switch the valve to Inject for 30 seconds.

5. Stop data acquisition.

3.12 Maintenance

This section describes routine maintenance procedures for the ICS-900 that users may perform. All other maintenance procedures must be performed by Dionex personnel.

As Needed

• Make fresh eluent.

• Regularly check the eluent bottle and refill it when needed.

• Every time you refill the eluent bottle, also empty the regenerant bottle, rinse

it, and refill it with fresh regenerant. Reset the Eluent Remaining slider on the ICS-900 Control panel (see page 29

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ICS-900 Operator’s Manual

Daily

• Check the ICS-900 component mounting panel (see Figure 2-2) for leaks or

spills. Wipe up spills. Isolate and repair leaks (see Section 4.2 dried eluent or regenerant with deionized water.

• Check the waste container and empty when needed.

Weekly

• Check fluid lines for crimping or discoloration. Relocate any pinched lines.

Replace damaged lines.

• Check the back of the pump head and underneath the head for evidence of

liquid leaks. Normal 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

Annually

• Change the pump seals (see Section 5.7).

• Rebuild the injection valve (see Section 5.10).

). Rinse off any

• If an AS or AS-DV autosampler is installed, perform the preventive

maintenance procedure. Kits are available for this purpose: AS Preventive Maintenance Kit (P/N 060581), AS-DV Preventive Maintenance Kit (P/N 072678).

• If an AS40 Automated Sampler is installed, replace the sample tip and tubing.

The ASM/AS40 Sample Tip Replacement Kit (P/N 040835) contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve. For instructions on how to replace the sampling tip, see the AS40 Automated Sampler Operator’s Manual (Document No.

034970). The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

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This chapter is a guide to troubleshooting problems that may occur while operating the ICS-900 Ion Chromatography System (ICS-900).

• Section 4.1 describes the error messages displayed in the Chromeleon or

Chromeleon Xpress Audit Trail.

• Section 4.2 through Section 4.13 describe other operating problems and how

to resolve them.

If you are unable to eliminate a problem, contact Dionex for help. In the U.S., call Dionex Technical Support at 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

4.1 Alarms and Error Conditions

If any of the following alarm conditions occurs, an error message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail. Each error message is preceded by an icon that identifies the seriousness of the underlying problem (see the table below).

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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The table below lists the ICS-900 error messages. For troubleshooting assistance, refer to the page indicated in the table

Alarms and Error Conditions See Conductivity exceeds limit.

Flow rate calibration error. Load/inject valve error. Module data buffer overflow. Data may have been lost. Pump motor lost control. Pump pressure hardware error. Pump pressure slope calibration error. Remaining eluent below 200 mL. The system pressure is below the low pressure limit. The system pressure has exceeded the high pressure limit.

Conductivity exceeds limit.

page 52

page 53

page 54

page 55

page 56

This message may appear at when the ICS-900 power is turned on. If the message appears at other times, it indicates a problem.

To troubleshoot:

1. Perform the suppressor inline quick start procedure:

a. Disconnect the separator column outlet line from the suppressor

ELUENT IN port and disconnect the cell inlet line from the suppressor ELUENT OUT port. Use a union to connect these two lines.

b. Turn on the pump flow and allow the suppressor to regenerate for

10 minutes.

c. Turn off the pump and allow the suppressor to hydrate for 20 minutes.

d. Reconnect the separator column outlet line and cell inlet line to the

suppressor ports.

2. If the high background persists:

• Prepare fresh eluent (see Section 3.4).

• Prepare fresh regenerant (see Section 3.5).

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4 • Troubleshooting

• Verify the cell calibration by pumping deionized water through the

cell (bypassing the column(s) and suppressor). The total background should be less than 1.0

μS.

• Perform the suppressor off-line regeneration procedure.

a. Disconnect the liquid lines from the suppressor and remove the

suppressor from the ICS-900.

b. Use a syringe to push the following types and amounts of fluid

into the suppressor ports:

• AMMS® 300: Push about 3 mL of 100 mM H

ELUENT OUT port and about 5 mL of 100 mM H REGEN IN port.

through the

2SO4

through the

• CMMS® 300: Push about 3 mL of 200 mM NaOH through the

ELUENT OUT port and about 5 mL of 200 mM NaOH through the REGEN IN port.

c. Allow the suppressor to sit for at least 20 minutes to fully hydrate

it.

• If the problem persists, replace the suppressor (see Section 5.12).

Flow rate calibration error.

This error occurs if you try to calibrate the flow rate when the pump is off, or it is on, but the flow rate is not 1 mL/min.

To troubleshoot:

• Before calibrating the flow rate, be sure to press the Start Calibration

button on the Wellness panel. This will automatically start the pump and set the flow rate to 1 mL/min. For flow rate calibration instructions, see

Section 5.1.5

Load/inject valve error.

If the injection valve fails to switch positions within 1 second of being toggled, the ICS-900 Moduleware reports an error to Chromeleon or Chromeleon Xpress and this error message is displayed.

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ICS-900 Operator’s Manual

To troubleshoot:

1. If a sequence is being executed, terminate the sequence by selecting Stop on the Batch menu.

2. Turn off the ICS-900 power briefly and then restart.

3. Try to toggle the valve from Load to Inject by clicking the Inject button on the ICS-900 Control panel.

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

Module data buffer overflow. Data may have been lost.

Various electronics-related problems can cause this error message to be displayed.

If this warning appears, contact Dionex for assistance. The ICS-900 electronics components cannot be serviced by the user.

Pump motor lost control.

This error indicates a problem in the pump controller electronics.

To troubleshoot:

• Contact Dionex for assistance. The ICS-900 electronics components

cannot be serviced by the user.

Pump pressure hardware error.

This error indicates a problem in the pump controller electronics.

To troubleshoot:

• Contact Dionex for assistance. The ICS-900 electronics components

cannot be serviced by the user.

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4 • Troubleshooting

Pump 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:

• Verify that the pump is on and the flow rate is at the rate required for the

application.

• Verify that the pressure gauge is working correctly.

• Verify that the correct number and type of backpressure coils are

installed. Refer to the tables on page 63

• Check for liquid leaks (see Section 4.2).

Remaining eluent below 200 mL.

-or-

Remaining eluent below 100 mL.

These errors occur when the ICS-900 determines that the eluent bottle contains less than the volume specified in the message.

To troubleshoot:

• The ICS-900 determines the eluent usage by monitoring the flow rate and

the length of time the pump is on. For the eluent level to be accurate, you must enter the level on the ICS-900 Control panel each time the bottle is filled. After filling the bottle, move the Eluent Remaining slider on the ICS-900 Control panel (see Figure 3-3 the bottle.

) to indicate the volume of liquid in

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ICS-900 Operator’s Manual

The system pressure is below the low pressure limit.

If the system pressure falls below the minimum pressure limit for 0.5 second, Chromeleon or Chromeleon Xpress stops the pump and displays this error message. The minimum pressure limit can be set to between 0 and 33.7 MPa (0 and 4900 psi) in the Chromeleon Server Configuration Properties dialog box or the Chromeleon or Chromeleon Xpress program.

To troubleshoot:

1. Make sure the eluent bottle is full.

2. Check for liquid leaks (see Section 4.2

3. Prime the pump (see Section 3.6

4. Restart the pump from the ICS-900 Control panel (see Section 3.6

For additional troubleshooting information about pump priming, see

Section 4.3

The system pressure has exceeded the high pressure limit.

If the system pressure exceeds the maximum pressure limit for 0.5 second, Chromeleon or Chromeleon Xpress stops the pump and display this error message. The maximum pressure limit can be set to between 0.7 and

34.4 MPa (100 and 5000 psi) in the Chromeleon or Chromeleon Xpress

Server Configuration or control program.

To troubleshoot:

1. Check for blockages in the liquid lines by working your way backward from the cell to the pump (see Figure 2-4

2. Restart the pump from the ICS-900 Control panel.

For additional troubleshooting information about system pressure, see

Section 4.7

for the flow schematic).

56 Doc. 065215-02 9/09

4.2 Liquid Leaks

• Leaking fitting

Locate the source of the leak. Tighten or, if necessary, replace the liquid line connection (see Section 5.2 Installation of Dionex Liquid Line Fittings (Document No. 031432), provided on the Dionex Reference Library CD-ROM (P/N 053891).

• Broken liquid line

4 • Troubleshooting

). For tightening requirements, refer to the

Replace the line and fittings (see Section 5.2

• Blocked or improperly installed line

Make sure the lines are not crimped or otherwise blocked. Also, if the blocked line is a waste line, make sure it is not elevated at any point after it exits the ICS-900. If a line is blocked, replace it (see Section 5.2

• Loose pump check valve housing

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.

• Damaged pump piston seal

1. Replace the piston seal (see Section 5.7

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

• Pump head not tight

Carefully tighten the pump head mounting screws just until the leak stops.

DO NOT OVERTIGHTEN!

• Leaking pressure transducer

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

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• Leaking pump head waste valve

Make sure the waste valve is closed. To close the valve, turn the knob clockwise, just until tight. DO NOT OVERTIGHTEN! Overtightening

may damage the valve and the pump head.

Inspect the pump head. If the waste valve is the source of the leak, replace the waste valve seal (see Section 5.9

• Leaking MMS 300

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

Make sure the liquid line connections to the valve are tight. Replace any damaged fittings. 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).

Liquid leaks from behind the valve stator may indicate a scratched rotor seal. Rebuild the injection valve (see Section 5.10

• Leaking conductivity cell

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.

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.

4.3 Pump Difficult to Prime or Loses Prime

• Empty eluent bottle and/or no eluent connected

Fill the bottle. Make sure all connections are secure.

• Dirty check valve

Clean or replace the pump check valve (see Section 5.6

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4 • Troubleshooting

• Liquid leaks at junction between pump head and pump housing

Replace the piston seal (see Section 5.7

4.4 Pump Does Not Start

• No power (front door Power LED indicator fails to light)

Check that the power cord is plugged in.

Check the main power fuses and replace if needed (see Section 5.13

• No communication between ICS-900 and Chromeleon or Chromeleon

Xpress (

The USB cable is not connected correctly. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No. 065214), provided on the Dionex Reference Library CD-ROM (P/N

053891) and in the ICS-900 Ship Kit (P/N 067768).

Link LED on rear panel fails to light)

4.5 No Flow

• Pump not primed

Prime the pump (see Section 3.6

• Broken pump piston

Replace the piston (see Section 5.8

4.6 Erratic Flow/Pressure Reading

• Pump needs priming

Prime the pump (see Section 3.6

• Damaged piston seal

Replace the piston seal (see Section 5.7

• Dirty pump check valve

Clean or replace the check valve (see Section 5.6

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4.7 Excessive System Backpressure

• Restriction in system plumbing

Check all liquid lines for crimping or blockage. Make sure the ferrule fittings are not overtightened onto tubing. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for details. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

• Plugged or damaged fitting

Isolate the faulty fitting by loosening fittings, one by one, until the pressure returns to normal. Repair or replace the fitting (see Section 5.2

• Flow rate through columns too high

Check the pump flow rate.

• Clogged column bed supports

Refer to the instructions in the column manual for troubleshooting guidance. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

• Contaminated columns

Clean the columns as instructed in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

• Plugged Injection valve passages

Rebuild the injection valve (see Section 5.10

4.8 Peak “Ghosting”

Ghosting is the appearance of extraneous peaks in a chromatogram. These may be late-eluting peaks from a previous injection or they may result from a contaminated, malfunctioning, or incorrectly installed injection valve. These peaks may co-elute with peaks of interest, resulting in nonreproducible peak heights/areas.

• Insufficient time between sample injections

Wait until the previous sample has been completely eluted before making another injection.

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4 • Troubleshooting

• Insufficient flush between samples

Flush the sample loop with at least 10 loop volumes of deionized water or sample between sample injections.

• Incorrect or contaminated standards

Remake standards.

• Incorrect or contaminated eluent

Remake the eluent (see Section 3.4

• Malfunctioning injection valve

Contact Dionex for assistance.

4.9 Nonreproducible Peak Height or Retention Time

• Column overloading

Dilute the sample (see Section 3.10.3

• Liquid leaks

Locate and eliminate the leaks (see Section 4.2

• Incomplete or imprecise filling of the sample loop

1. Fill the sample loop until excess sample exits the waste line.

2. Inspect the 1 cc syringe (P/N 016388) and replace if damaged.

• Pump not primed properly

Prime the pump (see Section 3.6

4.10 Abnormal Retention Time or Selectivity

• Contaminated or incorrect eluent

Remake the eluent, using concentrated eluent and ASTM Type I (18megohm) filtered and deionized water (see Section 3.4

• Contaminated or degraded sample

Take appropriate precautions when preparing and storing samples to prevent contamination and degradation (see Section 3.10

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• Contaminated column

1. Clean the column as instructed in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

2. If cleaning is unsuccessful, replace the column.

4.11 No Detector Response

• Cell not properly installed

Check that the cell is plugged into the component mounting panel and the cell housing is screwed down until the bottom of the housing is flush against the sheet metal panel (see Figure 2-2

• No flow from pump

and Figure 2-10).

Several conditions may cause this condition; see Section 4.4 for details.

• Cell electronics malfunctioning

Use the Wellness panel to test the electronics with a dummy cell (see

Section 5.1

reading with the dummy cell is outside the tolerance range, the electronics are malfunctioning. Contact Dionex for assistance.

and the Chromeleon Help for instructions). If the conductivity

4.12 High Detector Output

• Background not suppressed by suppressor

Conductivity exceeds limit is displayed in the Chromeleon or Chromeleon

Xpress Audit Trail, follow the instructions in Section 4.1 troubleshooting guidance, refer to the suppressor manual. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

• Sample concentration too high

Dilute the sample (see Section 3.10.3

• Wrong eluent or regenerant

Check that you are using the correct eluent and regenerant for your system (see Section 3.4

and Section 4.5

. For additional

62 Doc. 065215-02 9/09

• Cell out of calibration

4 • Troubleshooting

Recalibrate the cell from the Wellness panel (see Section 5.1

4.13 Baseline Noise or Drift

• Flow system leak; erratic baseline

Check all fittings and liquid lines for leaks. Tighten or, if necessary, replace all liquid line connections. 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).

• Trapped gases

Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them. Also loosen and retighten the fittings to and from the MMS eluent ports.

• Pump not properly primed

Prime the pump (see Section 3.6

• Contaminated or incorrect eluent and/or regenerant

Remake the eluent and regenerant (see Section 3.4

• Rapid changes in ambient temperature

If the ambient temperature does not meet the specification of 10 to 35 °C (50 to 95 °F), verify that air conditioning and heating vents are directed away from the ICS-900 and the ICS-900 front door is closed.

• Insufficient conductivity cell backpressure

Verify that the correct backpressure coils are installed:

Standard bore systems: Use one or two black backpressure coils (P/N 045877) supplied in the ICS-900 Ship Kit (P/N 067768).

Flow Rate Number of Coils

1.5 to 3.0 mL/min

0.5 to 1.5 mL/min

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1 (black)

2 (black)

ICS-900 Operator’s Manual

Microbore systems: Use one or two red backpressure coils (P/N 045878) supplied in the microbore tubing kit (P/N 052324).

Flow Rate Number of Coils

0.3 to 0.5 mL/min

Less than 0.3 mL/min

Install the tubing between the cell outlet and the regenerant bottle inlet. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No. 065214), provided on the Dionex Reference Library CD-ROM (P/N 053891) and in the ICS-900 Ship Kit (P/N 067768).

• Insufficient system equilibration following changes to operating

parameters; especially apparent when operating at high sensitivities

Allow a longer system equilibration time (up to 3 hours) before starting to inject samples.

• Incorrect suppressor operating conditions

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

1 (red)

2 (red)

• Cell above or below temperature

Contact Dionex for assistance.

• Damaged piston seal

Replace the piston seal (see Section 5.7

• DCR backpressure tubing not installed or incorrectly installed

Install the tubing on the end of the suppressor waste line. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No. 065214), provided on the Dionex Reference Library CD-ROM (P/N 053891) and in the ICS-900 Ship Kit (P/N 067768).

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This chapter describes ICS-900 Ion Chromatography System (ICS-900) service and repair procedures that users may perform. Procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call 1800-346-6390. Outside the U.S., call the nearest Dionex office.

Before replacing any part, refer to the troubleshooting information in Chapter 4 correctly identify the cause of the problem.

Substituting non-Dionex parts may impair system performance, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information.

5.1 Diagnostics and Calibrations

The Wellness panel (see Figure 5-2) provides controls for performing diagnostic and calibration functions. This section provides an overview of Wellness panel features. For calibration procedures, see the following sections:

• “Calibrating the Pressure Transducer” (Section 5.1.3)

• “Calibrating the Cell” (Section 5.1.4)

• “Calibrating the Flow Rate” (see Section 5.1.5)

5.1.1 Opening the Wellness Panel

1. In the Chromeleon Browser, expand the Dionex Templates\Panels\Wellness folder.

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2. Double-click Dionex_ICS-900_wellness.pan (see Figure 5-2).

Figure 5-1. Opening the Wellness Panel

The Wellness panel opens (see Figure 5-2

Figure 5-2. ICS-900 Wellness Panel

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3. If the controls on the Wellness panel are disabled, select Connect to timebase on the Control menu and select the ICS-900 timebase.

5.1.2 Wellness Panel Features

The Wellness panel provides the following features:

System Status • The check box indicates whether the ICS-900 is connected to

Chromeleon or Chromeleon Xpress. When there is no connection, the check box is clear and the remaining controls on the Wellness panel are disabled.

• Click the Pump button to turn the pump on and off.

• Click the Log Serial # button to record the ICS-900 serial

number in the Audit Trail.

• The Calibration or Diagnostic box is green while a

calibration or diagnostic procedure is running.

• The current total system Pressure, pump Flow rate, and

electrochemical detector (ECD) conductivity are displayed.

Audit Trail

Reset Calibration Parameters

• The Audit Trail displays an account of every event that occurs

during ICS-900 operation. This includes errors, status messages, operational events, etc.

• Click the View/Reset Cal Values button to open a window

that shows the current calibration values, the previous values, and the factory-set values. You can reset the current calibration values to the previous or factory-set values from the window.

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Calibration

Diagnostic

• Pressure Transducer

• Use the Calibrate Offset and Calibrate Slope buttons

when performing the pressure transducer calibration procedure (see Section 5.1.3

• The Offset and Slope values and the date of the last

calibration are displayed.

• Conductivity Cell

• Use the Calibrate Offset and Calibrate Slope buttons

when performing the cell calibration procedure (see

Section 5.1.4

• The Offset and Slope values and the date of the last

calibration are displayed.

• Pump Flow Rate Calibration

• Click Calibration Procedure to perform the calibration

(see Section 5.1.5

• Click Log to record the calibration value in the Audit

Trail.

• The Pump and Conductivity Cell Variance values are a

measure of the noise of the respective channels. The values of these measurements will vary with differing eluents, pump seal age and wear, background conductivity, and so on. When values (obtained under the same conditions) are compared they can be used as a relative measure of the performance of the system.

• The Variance, Minimum, and Maximum readings for the

last time the Pump and Conductivity Cell diagnostic tests were run are displayed.

Dummy Cell Test

• The Dummy Cell Test connects a fixed resistance in place of

the conductivity cell. A measured value outside the typical range of the test indicates a failure in the detector electronics.

• Click Log to perform the test and record the value in the

Audit Trail. Clicking Log enables the dummy cell, logs the value, and then disables the dummy cell.

• The Dummy Cell On check box enables and disables the

dummy cell.

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5.1.3 Calibrating the Pressure Transducer

1. Toggle the injection valve position a few times by clicking the Load and Inject buttons on the ICS-900 Control panel. This removes any air or contaminant buildup in the injection valve loop.

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Pressure

Transducer

2. Wait about 10 minutes and then continue to Step 3

3. Open the ICS-900 Wellness panel (see Section 5.1

4. Under Pressure Transducer, click the Calibrate Offset button (see

Figure 5-2

). A panel with instructions and command buttons will

open.

5. Follow the instructions on the panel to complete the transducer offset calibration procedure. The new offset is determined and stored as the current value.

NOTE To open the waste valve on the front of the

secondary pump head (see Figure 5-3 knob one-half turn counterclockwise.

), turn the

Waste Valve

Figure 5-3. ICS-900 Interior Components

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6. Close the waste valve.

7. Under Pressure Transducer, click the Calibrate Slope panel with instructions and command buttons will open.

8. Follow the instructions on the panel to complete the transducer slope calibration procedure. The new slope is determined and stored as the current value.

9. Turn off the pump.

10. Disconnect the pressure gauge and backpressure coil.

11. Reconnect the pressure transducer to the pump.

5.1.4 Calibrating the Cell

Calibrate the cell every 6 months or after installing a new conductivity cell.

Items Needed Description

1.00 mM KCl solution Prepare by dissolving 0.0746 g of reagent-

Backpressure tubing to provide at least 7 MPa (1000 psi)

button. A

grade KCl in one liter of ASTM Type I (18 megohm-cm) filtered and deionized (DI) water (use a volumetric flask).

Use 0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715).

1. Use an Allen wrench to remove the two screws securing the conductivity cell housing to the ICS-900 component mounting panel (see Figure 5-4

Figure 5-4. ICS-900 Interior Components: Removing the Conductivity Cell Housing

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). Save the screws.

Remove Screws

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2. Pull the cell housing straight out from the component mounting panel to unplug the cell from its electronics. Let the cell housing hang by the tubing.

3. Open the ICS-900 Wellness panel (see Section 5.1

4. Under Conductivity Cell, click the Calibrate Offset button (see

Figure 5-2

). A panel with instructions and command buttons will

open.

5. Follow the instructions on the panel to complete the conductivity cell offset calibration procedure. The new offset is determined and stored as the current value.

NOTE To reinstall the cell, on the mounting panel,

align the 9-pin connectors on the cell housing with the component mounting panel and plug the cell back into the electronics. Replace the mounting screws (removed in Step 1 tighten.

) and

6. Under Conductivity Cell, click the Calibrate Slope button. A panel with instructions and command buttons will open.

7. Follow the instructions on the panel to complete the conductivity cell slope calibration procedure. The new slope is determined and stored as the current value.

NOTE After calibration, the conductivity reading

should be 147.00 ± 2 μS/cm. If this is not the case, call Dionex for assistance.

8. Flush the KCl solution from the system by pumping DI water through the cell. When the conductivity drops to near zero, stop the pump flow.

9. Reconnect the pump to the injection valve and reconnect the line from the suppressor to the cell inlet.

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5.1.5 Calibrating the Flow Rate

Calibrate the flow rate if the Operational Qualification or Performance Qualification flow rate accuracy and precision test fails.

Items needed:

• 0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715) to create

14 ± 2 MPa (2000 ± 300 psi) of backpressure (if needed)

• High purity ASTM Type I (18 megohm-cm) filtered and deionized

water

• Balance capable of weighing more than 10 g with 0.001 g readability

• Tared beaker

To calibrate:

1. Open the ICS-900 Wellness panel (see Section 5.1).

2. Under Pump Flow Rate Calibration, click Calibration Procedure. A panel with instructions and command buttons will open.

3. Follow the instructions on the panel to complete the conductivity cell slope calibration procedure. The new slope is determined and stored as the current value.

NOTE Enter the weight of the collected water (in

grams, to the nearest milligram).

4. Click Log to record the new calibration value in the Audit Trail. This value is stored as the current value.

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5.2 Replacing Tubing and Fittings

The ICS-900 is plumbed with the tubing and tubing assemblies listed below.

Tubing Size and Type Used For

0.125-mm (0.005-in) ID PEEK, red (P/N 044221)

0.25-mm (0.010-in) ID PEEK, black (P/N 042690)

0.50-mm (0.020-in) ID Tefzel®, light blue (P/N 035519)

0.75-mm (0.030-in) ID PEEK, green (P/N 044777)

1.6-mm (0.062-in) ID Teflon®, natural (P/N 014157)

Microbore tubing kit (P/N 052324) Tubing for exchanging black 0.25-mm

Connection from pump pulse damper to pressure transducer

Connections between all other system components

Connection from injection port on door to injection valve

Connections from injection valve to waste, injection valve to pump pulse damper, and cell to regenerant bottle

Connections from suppressor to regenerant bottle, pump to eluent bottle, and pump to waste

(0.010-in) ID PEEK lines with red 0.125-mm (0.005-in) ID lines (to reduce delay volumes).

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Regen In port

Regen Out to waste,

• 10-32 fittings (P/N 062980) and ferrules (P/N 043276) are used for most

tubing connections. For tightening requirements, refer to Installation of Dionex Liquid Line Fittings (Document No. 031432). The manual is included

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

• 1/8-in fittings (P/N 052267) and ferrules (P/N 048949) are used for

connections to the MMS 300 regen ports and the eluent and regenerant bottles.

• 1/16-in fittings (P/N 052230) and ferrules (P/N 052231) are used for

connections from the front door injection port to the injection valve.

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5.3 Isolating a Restriction in the Liquid Plumbing

A restriction in the liquid plumbing will cause excessive system backpressure.

1. Begin pumping eluent through the system (including the columns).

2. Follow the ICS-900 flow schematic (see Figure 2-4 through the system, beginning at the cell exit. One at a time, loosen each fitting and observe the pressure. The connection at which the pressure drops abnormally indicates the point of restriction.

If the restriction has caused such high pressure that the system cannot be operated, you must work forward through the flow schematic, adding parts one at a time until an abnormal pressure increase (and hence, the restriction) is found.

3. If the restriction is in the tubing or fitting, remove the restriction by back flushing or by replacing the tubing or fitting.

) and work backward

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To pump inlet

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From cell outlet

Backpressure Coil

(1 or 2, depending on flow rate)

Conductivity Cell

(in DS5 Detection Stabilizer)

Regen Out Eluent Out

Eluent In

Pulse Damper

Secondary

Pump

Heads

To Waste

MMS 300

Primary

Regen In

Transducer

Eluent

To cell inlet

To MMS Regen In

Pressure

Injection

Valve

To Waste

Regenerant

Eluent in from pulse damper

Sample in

Figure 5-5. ICS-900 Flow Schematic

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5.4 Cleaning Eluent Bottles

Before preparing new eluent, all eluent bottles should be rinsed thoroughly (inside and out) with ASTM Type I (18 megohm-cm) filtered and deionized water. If a bottle still appears dirty, or has a slimy film on the inside, clean it as instructed below.

1. Dispose of any remaining chemicals according to municipal regulations.

2. Rinse the bottle (inside and out) with ASTM Type I (18 megohm-cm) filtered and deionized water.

3. Rinse the inside of the bottle with isopropyl alcohol or methanol.

4. If algae or bacteria have left a slimy film on the bottle, use an algicide or disinfectant (dilute hydrogen peroxide, etc.).

5. Rinse cleaning chemicals out of the bottle with ASTM Type I (18 megohmcm) filtered and deionized water.

6. Dry the bottle with clean, particulate-free air.

5.5 Changing the Sample Loop

A 10 μL PEEK sample loop (P/N 042949) is installed on the injection valve at the factory. Unless you are using a 2 mm column, replace the sample loop with another 10 μL PEEK sample loop. If you are using a 2 mm column, refer to the column manual for the size of loop required. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891)

1. Turn off the pump from the ICS-900 Control panel.

2. Open the ICS-900 front door.

3. Disconnect the sample loop from ports the injection valve (see

Figure 5-6

L and L on

Figure 5-6. ICS-900 Injection Valve

Sample Loop

76 Doc. 065215-02 9/09

4. Install the new sample loop between the two ports.

5. Make sure the loop is tightly coiled, so that the door can close securely.

6. Turn on the pump from the ICS-900 Control panel.

7. Check for leaking fittings and tighten if required.

8. Close the door.

5.6 Cleaning and Replacing Pump Check Valves

A dirty check valve causes erratic flow rates and pressures. In addition, it may cause the pump to lose prime and/or be difficult to reprime. If possible, replace dirty check valves. If new check valves are not available, follow the instructions for cleaning.

To replace the check valves:

1. Turn off the ICS-900 power switch and disconnect the power cord.

2. To prevent contamination of pump parts, put on a pair of powder-free gloves before disassembling the pump head.

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3. Disconnect the tube fittings from the inlet and outlet check valve assemblies on the primary pump head (see Figure 5-7

4. Use a 1/2-inch wrench to loosen both check valve assemblies. Remove the check valve assemblies from the pump head.

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Outlet Check Valve

Secondary

Pump Head

Figure 5-7. Pump Heads

NOTE The inlet check valve assembly housing has a 1/4-28 port.

The outlet check valve assembly housing has a 10-32 port.

5. Inspect the new inlet check valve assembly (P/N 045722) to verify that the double-hole end of the cartridge is visible (see Figure 5-8

Primary Pump Head

Inlet Check Valve

Inlet Check Valve Outlet Check Valve

1/4-28 Port

10-32 Port

If the double-hole end is not visible, remove the cartridge from the housing and install it correctly.

Double-hole

Single-hole

6. Inspect the new outlet check valve assembly (P/N 045721) to verify that the

Flow

single-hole end of the cartridge is visible.

If the single-hole end is not visible, remove the cartridge from the housing and install it correctly.

78 Doc. 065215-02 9/09

Flow

Figure 5-8. Check Valve Assemblies

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NOTE The pump will not operate properly unless the cartridge

is installed in the housing in the correct orientation. Liquid flows through the check valve in the large single hole and out the small double holes.

7. Install the inlet check valve assembly on the bottom of the primary pump head. Install the outlet check valve assembly on the top of the head. Tighten the check valves fingertight, and then use a wrench to tighten an additional one-quarter to one-half turn.

Overtightening may damage the pump head and check valve housing and crush the check valve seats.

8. Reconnect the liquid lines and the power cord. Turn on the ICS-900 main power.

9. Prime the pump (see Section 3.6

10. When the ICS-900 is at operating pressure, check for leaks from the check valves. Tighten a check valve a little more only if it leaks.

To clean the check valves:

1. Follow Step 1 through Step 4 in the check valve replacement procedure to remove the check valve cartridges from the valve housings.

2. Place the check valve housings and cartridges in a beaker with methanol. Sonicate or agitate the parts for several minutes.

3. Rinse each check valve housing and cartridge thoroughly with filtered deionized water.

4. Follow Step 5

through Step 10 in the check valve replacement procedure to

reinstall the check valves.

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5.7 Replacing a Pump Piston Seal and Backup Seal

A damaged seal allows leakage past the piston, as well as leakage from the piston seal wash housing. The pump may be difficult to prime, flow rates may be unstable, and there may be baseline noise.

Preparation:

1. Rinse the pump flow path with deionized water. Direct the flow to waste by opening the waste valve on the secondary pump head (see Figure 5-7 open the valve, turn the knob one-half turn counterclockwise.

2. After rinsing, close the waste valve.

3. To prevent contamination of pump parts, put on a pair of rubber gloves before disassembling the pump head.

To remove the head and piston:

1. Turn off the power switch and disconnect the power cord.

2. Disconnect all tubing connections to the pump head.

). To

3. Using a 7/64-in hex key (P/N 068227), loosen the two screws on the pump head with the defective seal. Remove the screws, and then carefully remove the head and place it on a clean surface.

4. Slowly pull the head and allow it to separate from the housing. Carefully disengage the head from the piston by pulling the head straight off and away from its mounting studs.

Lateral motion while disengaging the pump head from the piston may break the piston.

Un mouvement latéral pendant la séparation de la tête et du piston peut casser le piston.

Vermeiden Sie Seitwärtsbewegungen, wenn Sie den Pumpenkopg vom Kolben lösen. Andernfalls kann der Kolben brechen.

5. Place the head (front end down) on a clean work surface

6. The piston does not come off as part of the pump head assembly because it is captured by a magnetic retention system. After removing the pump head, hold

80 Doc. 065215-02 9/09

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(

)

(

)

the shaft of the piston (near the base), tilt the piston slightly, and pull the piston away from the pump.

Refer to Figure 5-9 pump head.

(P/N 014895)

Spacer with Drain

(P/N 067705)

Backup Piston Seal

(P/N 063382)

or Figure 5-10 when disassembling and reassembling the

Outlet Check Valve Assembly (P/N 045721)

Piston Seal

(P/N 055870)

O-Ring

Primary Pump Head (P/N 067702)

Inlet Check Valve Assembly (P/N 045722)

Seal Holder

Piston

P/N 052840

Figure 5-9. Primary Pump Head

(P/N 067706)

Piston Seal

(P/N 055870)

(P/N 014895)

Spacer with Drain

(P/N 067705)

Backup Piston Seal

(P/N 063382)

Piston

P/N 052840

O-Ring

Seal Holder (P/N 067706)

(P/N 063382)

eal

Prime Valve (P/N 063968)

Secondary Pump Head (P/N 067704)

Figure 5-10. Secondary Pump Head

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To install the new backup piston seal:

1. Lift the spacer off the pump head.

2. To remove the seal holder from the spacer, use one of the following methods:

• With the seal holder facing up, cup the spacer

in your hand and blow clean laboratory air at the spacer to dislodge the seal holder.

• Insert a thin object or pointed tool into the

small notch on the spacer and carefully pry out the seal holder. Be careful not to scratch the spacer.

3. To remove the backup piston seal from the spacer, insert a thin object (for example, the straightened end of a paper clip) and carefully pry out the backup piston seal. Be careful not to scratch the spacer.

4. To install the new backup piston seal:

Grooved side

a. Hold the new backup piston seal

(P/N 063382) with the grooved side facing down, and insert the shaft of the piston through the seal.

b. Insert the piston into the center hole in

the spacer.

c. Push the piston into the spacer until

the top of the piston is flush with the spacer. A clicking sound indicates that the seal is correctly seated.

Spacer

of backup

piston seal

Notch

Seal Holder

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The piston backup piston seal is made of soft plastic. Do not press on the seal with anything hard or sharp, including your fingernail. If the seal is nicked or gouged, it will not seal properly and may result in leaks.

d. Pull out the piston. The top of the seal should

be flush with the surface of the spacer.

e. Press the seal holder onto the spacer.

To remove the old piston seal from the head:

1. Fill the head cavity with deionized water by injecting the liquid through the piston opening.

2. Reinsert the piston approximately 3 mm (0.125 inch) into the seal.

3. If this is the primary pump head, install a 10-32 fitting plug (P/N 042772) on the outlet check valve. Tighten the plug.

4. If this is the secondary pump head, install a 10-32 fitting plug (P/N 042772) in both the inlet and outlet ports. Tighten the plugs.

5. Push the piston into the head. (This should hydraulically unseat the seal from the head.) Remove the piston and pull off the seal.

NOTE If the piston seal is not removed, make sure the 10-32

fitting plug(s) are tight and add more water. Make sure the head contains no air bubbles, and then repeat Steps

and 5.

6. Remove the 10-32 fitting plug(s).

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To install the new piston seal:

1. If this is the secondary pump head, open the waste valve knob by turning the knob one-half turn counterclockwise.

2. Lubricate the seal and the pump head opening with a small amount of isopropyl alcohol to facilitate insertion.

3. Push the piston through the spacer and then through the new piston seal.

4. Insert the piston and seal into the pump head.

Piston Seal

Piston

Spacer

5. To seat the seal, push down on the spacer until it is flush with the head. A clicking sound indicates that the seal is correctly seated.

84 Doc. 065215-02 9/09

6. Remove the spacer and piston and verify that the seal is flush with the surface of the pump head.

7. Verify that the O-ring is installed in the spacer.

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To reinstall the head and piston:

Dionex recommends reinstalling the head and piston as a single assembly, so that the piston centers itself onto the magnetic follower.

1. Hold the assembled spacer and guide with the drain tube aligned vertically and press the spacer into the head until it is flush with the indented surface of the head.

2. Insert the piston so that about 1/4 inch of the shaft is exposed. This ensures that the magnet in the follower picks up the piston. (The follower is the cylinder that holds the piston in place as it moves in and out of the pump head assembly.)

3. Reinstall the head and piston assembly; tighten the screws evenly.

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To complete the procedure:

1. Reconnect all liquid lines to the pump head.

2. Close the waste valve knob.

3. Turn on the ICS-900 power switch.

4. Prime the pump (see Section 3.6

5. Reset the seal wear counter in Chromeleon or Chromeleon Xpress:

a. Press F8 to open the Commands dialog box.

b. Expand the list of commands under Pump_ECD and scroll to the

ResetSealWear command (see Figure 5-11

c. Select the command and click Execute.

Figure 5-11. Resetting the Seal Wear Counter

5.8 Replacing a Pump Piston

Continued leaking of the piston seal after installation of a new seal (assuming the pump head is tight) indicates a dirty, scratched, or broken piston.

Follow the instructions in Section 5.7 piston seal (P/N 055870). Always replace the piston seal when replacing a piston. After replacing the piston and seal, reset the seal wear and pump piston stroke counters.

86 Doc. 065215-02 9/09

to install a new piston (P/N 052840) and

5.9 Replacing the Waste Valve Seal

A damaged seal causes leakage around the base of the waste valve knob.

1. Turn off the ICS-900 power switch.

5•Service

2. To remove the waste valve from the pump head (see Figure 5-12

), turn the knob counterclockwise until it is loose, and then pull the knob straight out of the cavity in the pump head.

Waste Valve

Figure 5-12. Waste and Priming Valves

3. If the seal is removed with the valve knob in Step 2

, pull the seal off the end of the

knob (see Figure 5-13

). If the seal is not

Valve Knob

removed with the valve knob, insert a thin object (for example, the straightened end of a paper clip) into the cavity in the

Seal

pump head and carefully pull out the seal.

Do not scratch the cavity.

Figure 5-13. Waste Valve Seal Replacement

Scratches in the cavity will cause leaks around the base of the knob while the pump is being primed.

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4. Orient the new seal (P/N 063382) with the grooved side away from the valve and slide it over the end of the valve.

5. Insert the valve with the new seal into the pump head opening and turn the knob clockwise. Tighten fingertight.

6. Turn on the ICS-900 power switch.

7. Prime the pump (see Section 3.6

5.10 Rebuilding the Injection Valve

Dionex recommends rebuilding the injection valve annually. The Injection Valve Rebuild Kit (P/N 057896) contains all required replacement parts.

NOTE Substitution of non-Dionex parts may impair valve

performance and void the product warranty.

1. Turn off the pump.

2. Open the front door of the ICS-900.

3. Disconnect each liquid line connected to the injection valve.

4. Follow the instructions provided in the Injection Valve Maintenance Kit to replace the rotor seal, isolation seal, and stator face.

5. Reconnect all liquid lines to the injection valve.

6. Close the ICS-900 front door.

7. Turn on the pump from the ICS-900 Control panel.

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8. Reset the injection valve cycle counter in Chromeleon or Chromeleon Xpress:

a. Press F8 to open the Commands dialog

box.

b. Expand the list of commands under

Pump_ECD and scroll to the ResetInjValveCounter command (see

Figure 5-14

c. Select the command and click Execute.

Figure 5-14. Resetting the Injection Valve Counter

5•Service

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ICS-900 Operator’s Manual

(

)

5.11 Replacing the Conductivity Cell

1. Turn off the ICS-900 power switch.

1. Disconnect the power cord.

2. Open the ICS-900 front door.

3. Disconnect the black suppressor (see Figure 5-15

CELL OUT (orange) to CELL OUT

Figure 5-15. Conductivity Cell Assembly

4. Disconnect the orange

CELL OUT line.

black

ELUENT OUT line from the ELUENT OUT port on the

ELUENT OUT to suppresso

Connector to component mounting panel

black

CELL OUT line from the union that connects it to the

5. Use an Allen wrench to remove the two screws on the top of the cell housing.

6. Remove the cell by unplugging it from the component mounting panel.

7. Plug the new conductivity cell (P/N 067761) into its mounting location.

8. Replace the screws on the top of the cell housing and tighten.

9. Attach the orange

CELL OUT line. Attach the ELUENT OUT line to the ELUENT OUT port on

black the suppressor.

CELL OUT line from the cell to the union attached to the

10. Close the front door.

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11. Reconnect the power cord and turn on the ICS-900 power.

5•Service

12. Calibrate the cell (see Section 5.1.4

5.12 Replacing the Suppressor

Refer to the suppressor manual for guidance about when to replace a suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

1. Turn off the pump.

2. Open the front door of the ICS-900.

3. Disconnect the four eluent and regenerant lines from the suppressor.

4. Slide the suppressor to the left to detach it from the component mounting panel.

5. Slide the new suppressor to the right until it locks into place on the mounting panel.

6. Connect the four eluent and regenerant lines to the new suppressor.

7. Close the ICS-900 front door.

8. Prime the pump (see Section 3.6

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ICS-900 Operator’s Manual

5.13 Changing the Main Power Fuses

1. Turn off the ICS-900 power switch.

2. Disconnect the power cord.

HIGH VOLTAGE—Disconnect the main power cord from its source and also from the rear panel of the ICS-900.

HAUTE TENSION—Débranchez le cordon d'alimentation principal de sa source et du panneau arrière du ICS-900.

HOCHSPANNUNG—Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des ICS-900.

3. The fuse drawer is located above the power switch (see Figure 5-16 tab locks the fuse drawer in place. Using a small screwdriver, press the tab in and then up to release the fuse drawer.

). A small

Fuse Drawer

Tab

4. Pull the fuse drawer out of the rear panel and remove the old fuses.

5. Replace the two fuses with new fast-blow IEC 127 fuses rated 3.15 A (P/N 954745). Dionex recommends always replacing both fuses.

Figure 5-16. Fuse Drawer

6. Insert the fuse drawer into the rear panel and press until the drawer snaps into place.

7. Reconnect the main power cord and turn on the power.

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Dionex ICS-900 Operator's Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1.1 Overview of the ICS-900

1.2 The ICS-900 Operator’s Manual

1.2.1 Overview

1.3 Safety and Regulatory Information

1.3.1 Safety Messages and Notes

1.3.2 Safety Symbols

1.3.3 Declaration of Conformity

2.1 Operating Features

2.1.1 Front Door and Top Cover

2.1.2 Component Mounting Panel

2.1.3 Rear Panel

2.2 Fluid Schematic

2.3 System Component Details

2.3.1 Pump

2.3.2 Pressure Transducer

2.3.3 Injection Valve with Sample Loop

2.3.4 MMS 300 MicroMembrane Suppressor

2.3.5 Displacement Chemical Regeneration (DCR)

2.3.6 Conductivity Cell and DS5 Detection Stabilizer

2.4 Chromeleon and Chromeleon Xpress Software

2.4.1 The Panel Tabset

2.4.2 Software Control Modes

2.4.3 System Wellness and Predictive Performance

3.1 Operation Overview

3.2 Turning On the ICS-900 Power

3.3 Connecting to Chromeleon or Chromeleon Xpress

3.4 Preparing the Eluent

3.5 Preparing the Regenerant

3.6 Priming the Pump

3.7 Equilibrating the System

3.8 Verifying Operational Status

3.9 Configuring Standby Mode

3.10 Preparing Samples

3.10.1 Collecting and Storing

3.10.2 Pretreating

3.10.3 Diluting

3.11 Processing Samples

3.11.1 Overview

3.11.2 Manually Processing Samples

3.11.3 Automatically Processing Samples (Batch Processing)

3.11.4 Loading and Injecting Samples with an Autosampler

3.11.5 Loading and Injecting Samples with a Syringe

3.11.6 Example Chromeleon Commands for Loading and Injecting Samples

3.12 Maintenance

4.1 Alarms and Error Conditions

4.2 Liquid Leaks

4.3 Pump Difficult to Prime or Loses Prime

4.4 Pump Does Not Start

4.5 No Flow

4.6 Erratic Flow/Pressure Reading

4.7 Excessive System Backpressure

4.8 Peak “Ghosting”

4.9 Nonreproducible Peak Height or Retention Time

4.10 Abnormal Retention Time or Selectivity

4.11 No Detector Response

4.12 High Detector Output

4.13 Baseline Noise or Drift

5.1 Diagnostics and Calibrations

5.1.1 Opening the Wellness Panel

5.1.2 Wellness Panel Features

5.1.3 Calibrating the Pressure Transducer

5.1.4 Calibrating the Cell

5.1.5 Calibrating the Flow Rate

5.2 Replacing Tubing and Fittings

5.3 Isolating a Restriction in the Liquid Plumbing

5.4 Cleaning Eluent Bottles

5.5 Changing the Sample Loop

5.6 Cleaning and Replacing Pump Check Valves

5.7 Replacing a Pump Piston Seal and Backup Seal

5.8 Replacing a Pump Piston

5.9 Replacing the Waste Valve Seal

5.10 Rebuilding the Injection Valve

5.11 Replacing the Conductivity Cell

5.12 Replacing the Suppressor

5.13 Changing the Main Power Fuses