Dionex ICS-1000 Operator's Manual

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ICS-1000 ION CHROMATOGRAPHY SYSTEM

OPERATOR’S MANUAL

Document No. 031879

Revision 01 March 2003

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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

MMS™ MicroMembrane™ Suppressor is a trademark of Dionex Corporation.

AES® Atlas Electrolytic Suppressor, Chromeleon®, OnGuard®, and SRS® SelfRegenerating Suppressor are registered trademarks of Dionex Corporation.

Teflon® is a registered trademark of E.I. duPont de Nemours & Co.

Windows® is a registered trademark of Microsoft Corporation.

PRINTING HISTORY

Revision 01, March 2003

Page 3

1 • Introduction

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

1.2 Overview of the ICS-1000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4

1.3 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-5

1.3.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . .1-6

1.3.2 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-8

2 • Features

2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

2.1.1 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

2.1.2 Top Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-3

2.1.3 Component Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4

2.1.4 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7

2.2 Flow Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-9

2.3 The Chromeleon Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-11

2.3.1 The Chromeleon Main Window and Browser . . . . . . . . . . . .2-12

2.3.2 The ICS-1000 Control Panels . . . . . . . . . . . . . . . . . . . . . . . . .2-13

2.4 System Component Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-19

2.4.1 Vacuum Degas Assembly (Optional) . . . . . . . . . . . . . . . . . .2-19

2.4.2 Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-21

2.4.3 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-21

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ICS-1000 Ion Chromatography System

2.4.4 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-24

2.4.5 Column Heater (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-26

2.4.6 Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-27

2.4.7 DS6 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . 2-27

3 • Operation and Maintenance

3.1 Operation Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.2 Power Up the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3

3.3 Start Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4

3.4 Set Up the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6

3.4.1 Prepare the Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6

3.4.2 Degas the Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6

3.4.3 Filter the Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7

3.4.4 Fill the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8

3.4.5 Set the Eluent Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8

3.4.6 Connect the Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8

3.5 Check All Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9

3.6 Prime the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9

3.7 Set System Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10

3.8 Equilibrate the System and Verify Operational Status . . . . . . . . . . . 3-11

3.9 Prepare Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.9.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . 3-12

3.9.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.9.3 Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13

ii Doc. 031879-01 3/03

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3.10 Loading and Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-14

3.10.1 Loading Samples with a Syringe . . . . . . . . . . . . . . . . . . . . . .3-15

3.10.2 Loading Samples with a Vacuum Syringe . . . . . . . . . . . . . . .3-16

3.10.3 Loading Samples with an Autosampler . . . . . . . . . . . . . . . . .3-16

3.10.4 Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-17

3.10.5 Example Chromeleon Commands for Loading and Injecting Samples 3-17

3.11 Process Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-18

3.11.1 Manual Sample Processing . . . . . . . . . . . . . . . . . . . . . . . . . .3-18

3.11.2 Automatic (Batch) Sample Processing . . . . . . . . . . . . . . . . . .3-19

3.12 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-21

4 • Troubleshooting

Contents

4.1 Alarms and Error Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-3

4.2 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-9

4.3 Pump Difficult to Prime or Loses Prime . . . . . . . . . . . . . . . . . . . . . . .4-11

4.4 Pump Does Not Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-13

4.5 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-14

4.6 Erratic Flow/Pressure Reading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-15

4.7 Excessive System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-15

4.8 Peak “Ghosting” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-16

4.9 Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . .4-17

4.10 Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . .4-17

4.11 No Cell Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-18

4.12 High Cell Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-18

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ICS-1000 Ion Chromatography System

4.13 Baseline Noise or Drift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19

4.14 Vacuum Degas Assembly Does Not Run . . . . . . . . . . . . . . . . . . . . . . 4-20

5•Service

5.1 Diagnostic and Calibration Procedures . . . . . . . . . . . . . . . . . . . . . . . . 5-1

5.1.1 Chromeleon Wellness Panel Overview . . . . . . . . . . . . . . . . . . 5-2

5.1.2 Calibrating the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . 5-4

5.1.3 Calibrating the Flow Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6

5.1.4 Calibrating the Vacuum Degas Assembly . . . . . . . . . . . . . . . . 5-7

5.2 Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . . . 5-7

5.3 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9

5.4 Rebuilding the Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10

5.5 Cleaning and Replacing the Pump Check Valves . . . . . . . . . . . . . . . 5-11

5.6 Replacing a Pump Piston Seal and Piston Rinse Seal . . . . . . . . . . . . 5-13

5.7 Replacing a Pump Piston . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17

5.8 Replacing the Waste Valve or Priming Valve O-Ring . . . . . . . . . . . . 5-18

5.9 Replacing the Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20

5.10 Replacing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22

5.11 Replacing the Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23

5.12 Replacing the Column Heater Heat Exchanger . . . . . . . . . . . . . . . . . 5-25

5.13 Replacing the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-26

5.14 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-28

5.15 Priming with Isopropyl Alcohol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-29

5.16 Changing Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-30

iv Doc. 031879-01 3/03

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A • Specifications

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

A.2 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

A.3 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

A.4 Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2

A.5 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2

A.6 Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3

A.7 Conductivity Cell with Heat Exchanger . . . . . . . . . . . . . . . . . . . . . . . A-3

A.8 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3

A.9 Vacuum Degas Assembly (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . A-3

A.10 Column Heater (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4

Contents

B • Installation

B.1 Facility Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1

B.2 Unpacking the ICS-1000 System . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2

B.2.1 Unpacking the Computer (North America only). . . . . . . . . . . B-4

B.2.2 Unpacking the Computer (outside North America) . . . . . . . . B-4

B.3 Installing Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5

B.4 Installing the Chromeleon Software License . . . . . . . . . . . . . . . . . . . B-6

B.5 Connecting the ICS-1000 to the Chromeleon PC . . . . . . . . . . . . . . . . B-9

B.5.1 Connecting the ICS-1000 to the PC . . . . . . . . . . . . . . . . . . . . B-9

B.5.2 Connecting Additional USB Devices . . . . . . . . . . . . . . . . . . B-10

B.6 Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-11

B.7 Turning On the ICS-1000 Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-12

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ICS-1000 Ion Chromatography System

B.8 Setting Up Chromeleon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-13

B.8.1 Assigning the ICS-1000 to a Timebase . . . . . . . . . . . . . . . . .B-13

B.8.2 Assigning DX-LAN Devices to the Timebase (Optional) . . . B-16

B.9 Installing and Plumbing the Columns and Suppressor . . . . . . . . . . . .B-19

B.9.1 Column Heater Setup (Optional) . . . . . . . . . . . . . . . . . . . . . .B-19

B.9.2 Installing the Columns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-20

B.9.3 Installing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-21

B.10 Connecting the Waste Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-23

B.10.1 Installing the Gas Separator Waste Tube . . . . . . . . . . . . . . . .B-23

B.11 Setting Up the Eluent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-25

B.12 Setting Up a Chromeleon Application . . . . . . . . . . . . . . . . . . . . . . . . B-26

B.12.1 Verifying Chromeleon Communication. . . . . . . . . . . . . . . . .B-35

B.13 Setting the Eluent Level . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-35

B.14 Priming the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-36

B.14.1 Priming the Eluent Lines with a Syringe . . . . . . . . . . . . . . . .B-36

B.14.2 Priming with the Prime Button. . . . . . . . . . . . . . . . . . . . . . . .B-38

B.15 Equilibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-39

B.16 Verifying Operational Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-39

B.17 Connecting an AS50 Autosampler (Optional) . . . . . . . . . . . . . . . . . .B-40

B.17.1 AS50 Configuration Requirements . . . . . . . . . . . . . . . . . . . .B-40

B.17.2 AS50 Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-41

B.17.3 Enable AS50 Control of the Injection Valve . . . . . . . . . . . . .B-43

B.18 Connecting an AS40 Automated Sampler (Optional) . . . . . . . . . . . .B-44

B.19 Analog Output Connection (Optional) . . . . . . . . . . . . . . . . . . . . . . . .B-46

B.20 Pressurizing the Eluent Reservoir (Optional) . . . . . . . . . . . . . . . . . . .B-46

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B.20.1 Connecting the Gas Source (Optional) . . . . . . . . . . . . . . . . . B-47

B.20.2 Pressurizing the Eluent Reservoir (Optional) . . . . . . . . . . . . B-48

B.21 Pump Continuous Seal Wash Connections (Optional) . . . . . . . . . . . B-49

B.22 Manually Connecting to a Control Panel . . . . . . . . . . . . . . . . . . . . . B-51

B.23 Installation Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-53

C • TTL and Relay Control

C.1 TTL and Relay Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1

C.1.1 Selecting TTL Input Functions and Control Types. . . . . . . . . C-3

C.2 Controlling TTL and Relay Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . C-5

C.3 Example Setup for Stand-Alone Operation . . . . . . . . . . . . . . . . . . . . . C-7

Contents

D • Reordering Information

E•FAQ

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

E.2 How do I print? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1

E.3 Why are the retention times moving? . . . . . . . . . . . . . . . . . . . . . . . . . E-1

E.4 How do I adjust retention times? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-1

E.5 When should I remake standards? . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.6 When should I remake eluents? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.7 How do I start Chromeleon? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.8 How do I delete data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.9 How do I back up data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

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ICS-1000 Ion Chromatography System

E.10 How do I shut off the system? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.11 How do I store columns? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-2

E.12 How do I know when a column is dirty? . . . . . . . . . . . . . . . . . . . . . . .E-3

E.13 How do I clean a column? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .E-3

E.14 Why is the conductivity high? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E-3

F • Glossary

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1 • Introduction

1.1 Introduction to Ion Chromatography (IC)

The Dionex ICS-1000 Ion Chromatography System (ICS-1000) performs ion analyses using suppressed or non-suppressed conductivity detection. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system.

Before running a sample, the ion chromatography system is calibrated using a standard solution. By comparing the data obtained from a sample to that obtained from the known standard, sample ions can be identified and quantitated. The data collection system, typically a computer running chromatography software, produces a chromatogram (a plot of the detector output vs. time). The chromatography software converts each peak in the chromatogram to a sample concentration and produces a printout of the results.

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ICS-1000 Ion Chromatography System

A typical IC analysis consists of 6 stages (see Figure 1-1).

. Data Analysis

Conductivity

Cell

Suppressor

5. Detectio

1. Eluent

Eluent

Delivery

Pump

2. Sample Injection

Figure 1-1. Ion Analysis Process

1. Eluent Delivery

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

sample through the ion chromatography system. The ICS-1000 is an isocratic delivery system. This means that the eluent composition and concentration remain constant throughout the run.

2. Sample Injection

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

automatically (if an automated sampler is installed). When triggered, the ICS-1000 injects the sample into the eluent stream.

Injection

Val ve

Guard Column

Sample Loop

Separator

Column

4. Suppression

3. Separation

Sample

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

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

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3. Separation

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

the sample ions are separated. In the ICS-1000, the mode of separation is called ion exchange. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites.

4. Suppression

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

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

5. Detection

• A conductivity cell measures the electrical conductance of the sample

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

6. Data Analysis

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

1 • Introduction

• The data collection system (for the ICS-1000, this is Chromeleon®)

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

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ICS-1000 Ion Chromatography System

1.2 Overview of the ICS-1000

The ICS-1000 is an integrated ion chromatography system containing a pump, injection valve, column heater, and conductivity detector. Other system components, including a guard column, separator column, and suppressor vary, depending on the analyses to be performed.

The ICS-1000 can optionally be configured with a column heater for temperature control of the column.

ICS-1000 operation is controlled remotely by a personal computer running Windows later). Chromeleon also provides data acquisition and data processing functions.

For communication between the ICS-1000 and Chromeleon, the ICS-1000 is connected to a USB (Universal Serial Bus) port on the computer or a USB hub. For installation instructions, see Section B.5 Chromeleon IC System (Document No. 031883).

® 2000 or Windows XP and Chromeleon software (version 6.5 SP2 or

and also refer to Installing the

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1.3 About This Manual

1 • Introduction

Chapter 1 Introduction

Chapter 2 Features Overview

Chapter 3 Operation and Maintenance

Chapter 4 Troubleshooting

Chapter 5 Service

Appendix A Specifications

Appendix B Installation

Appendix C TTL and Relay Control

Introduces ion analysis and the ICS-1000; explains the conventions used in this manual, including safety-related information.

Provides an overview of ICS-1000 operating features and system components; introduces the Chromeleon user interface.

Provides operating instructions and describes routine preventive maintenance procedures.

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

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

Lists the ICS-1000 specifications and installation site requirements.

Describes how to install the ICS-1000.

Describes the ICS-1000 TTL and relay control features.

Appendix D Reordering Information

Appendix E FAQ

Appendix F Glossary

Doc. 031879-01 3/03 1-5

Lists spare parts for the ICS-1000.

Provides answers to frequently asked questions about ICS-1000 operation.

Defines terms commonly used in ion analysis.

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ICS-1000 Ion Chromatography System

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-1000 when properly followed. Safety messages appear in bold type and are accompanied by icons, as shown below.

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

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

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

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

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.

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1 • Introduction

Warnhinweise in Deutsch

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

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

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

Notes

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

NOTE NOTES call attention to certain information. They alert

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

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ICS-1000 Ion Chromatography System

1.3.2 Safety Labels

The ICS-1000 meets EN 61010-1:1993 (safety), CAN/CSA-C22.2 No.

1010.1-92 (safety), UL 3101-1/10.93 (safety), EN 50082-1:1992 (susceptibility), EN 55011:1991 (emissions). The TUV GS, C, US Mark safety labels and the CE Mark label on the ICS-1000 attest to compliance with these standards.

The symbols below appear on the ICS-1000 or on ICS-1000 labels.

Alternating current

Protective conductor terminal (earth ground)

Power supply is on

Power supply is off

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This chapter describes key ICS-1000 features and introduces the Chromeleon user interface.

2.1 Operating Features

2.1.1 Front Panel

Figure 2-1 illustrates the front panel of the ICS-1000.

Power

LED

Status LEDs

Injection Port

2•Features

Injection Port

The sample to be analyzed can be injected manually into the injection port, using a syringe. For automated sample injection, the ICS-1000 must be connected to an autosampler. For more information about sample injection, see

Section 3.10

LEDs

The status LEDs (see

Figure 2-2

of various system functions. See Table 2- 1 of each LEDs function. The power LED indicates whether the ICS-1000 power is on.

) indicate the status

for a description

Figure 2-1. ICS-1000 Front Panel

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ICS-1000 Ion Chromatography System

INJECT VALVE

Load

Inject

ALARM

STATUS

Module Connected

Acquiring Data

Pump

Suppressor

Column Heater

Figure 2-2. Status LEDs

LED Label If On (Green) If Flashing

Load

Injection valve is in Load

Valve error.

position.

Inject

Injection valve is in Inject

Valve error.

position.

Alarm

No “on” (green) state. Error detected. Check the Chromeleon

Audit Trail for the cause.

Module Connected

ICS-1000 is connected to a Chromeleon timebase.

Does not flash.

Acquiring Data

Pump

Sequence or manual data

Sequence has stopped due to an error.

acquisition is in progress.

Pump is on. High or low pressure limit is exceeded.

The pump is turned off

Suppressor

Column Heater

Suppressor is on and current is being applied to it.

Column heater is at set temperature.

Continuity check failed or suppressor is over the voltage, current, or power limit. The suppressor is turned off

Column heater is transitioning to a new temperature.

Table 2-1. ICS-1000 Status LED States

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2.1.2 Top Cover

Figure 2-3 illustrates the top cover of the ICS-1000.

Figure 2-3. ICS-1000 (Top View)

2 • Features

Reservoir Storage

The ICS-1000 top cover has room for up to three 2-L plastic reservoirs (P/N 044129).

Tubing Chase

The tubing chase under the top cover routes tubing to the front of the ICS-1000.

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ICS-1000 Ion Chromatography System

2.1.3 Component Panel

Figure 2-4 shows the user-accessible components installed on the

component panel behind the ICS-1000 front door.

Eluent Valve

Leak Sensor

Pump Heads

Pressure Transducer

Injection Valve

Columns

Connector for

optional column heater

Suppressor

DS6 Conductivity

Cell

Mounting brackets

for a second suppressor

Tubing Chase (2)

Figure 2-4. ICS-1000 Component Panel

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2 • Features

Eluent Valve

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

Leak Sensor

The leak sensor is installed in the drip tray at the bottom of the component panel. If liquid accumulates in the tray, an error message is reported in Chromeleon and the Alarm LED flashes.

Pump Heads

The ICS-1000 includes a serial isocratic dual-head pump. The flow rate can be set to 0.00 and to between 0.05 and 5.0 mL/min. However, for optimum performance, set the flow rate to between 0.4 and 2.0 mL/min. Setting the flow rate to 0.00 turns off the pump. See Section 2.4.3 details about the pump.

Pressure Transducer

The pressure transducer measures the system backpressure.

for

Injection Valve

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

Section 2.4.4

Separator and Guard Columns

for details about valve operation.

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

Column Heater (Optional—Not Pictured)

The column heater controls the temperature of the separator and guard columns. The temperature can be set to between 30 °C and 60 °C and it must be set at least 5 °C above the ambient temperature. See Section 2.4.5 for details about the column heater.

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ICS-1000 Ion Chromatography System

Suppressor

The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an AES® Atlas Electrolytic Suppressor, SRS® Self-Regenerating Suppressor, or MMS™ MicroMembrane™ Suppressor can be used with the ICS-1000. See Section 2.4.6

DS6 Heated Conductivity Cell

The flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. A heat exchanger inside the cell regulates the temperature, which can be set to between 30 °C and 55 °C. For optimum performance, set the temperature to at least 7 °C above the ambient temperature. See Section 2.4.7 cell.

Tubing Chases

The upper tubing chase routes tubing from the top cover to the component panel. The lower tubing chase routes tubing from the component panel through the ICS-1000 interior to the rear panel.

for details.

for details about the

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2.1.4 Rear Panel

Figure 2-5 illustrates the ICS-1000 rear panel.

Tubing Clips

Power

Switch

2 • Features

Analog Output Connector

USB Connections

Main Power

Receptacle

Analog Output Connector

The analog output connector outputs conductivity data (scaled to 1 volt) to an integrator or recording device. See Section B.19 setup information.

USB Connections

A USB receptacle is provided to allow connection to the Chromeleon computer. Two USB ports are provided for connecting to other USB devices. See Section B.5

TTL and Relay Connector Strip

Waste Lines

Figure 2-5. ICS-1000 Rear Panel

for connection and

for connection instructions.

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ICS-1000 Ion Chromatography System

TTL and Relay Connector

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

Section C.1

Tubing Clips

The tubing clips hold tubing in place when routing it from the top cover.

Power Switch

The power switch provides on/off control of power to the ICS-1000.

Main Power Receptacle

The power supply cord plugs into the AC power receptacle.

The power supply cord is used as the main disconnect device. Make sure the socket-outlet is located near the ICS-1000 and is easily accessible.

for connection instructions.

Le cordon d'alimentation principal est utilisé comme dispositif principal de débranchement. Veillez à ce que la prise de base soit située/installée près du module et facilement accessible.

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

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2.2 Flow Schematic

Figure 2-6 illustrates the liquid flow path through an ICS-1000 when using

suppression in autorecycle mode.

2 • Features

PUMP

DEGAS

(Optional)

ELUENT

OUT

COND

OUT

CELL

PULSE

DAMPER

SAMPLE

WASTE

VALV E

OUT

PUMP PUMP

HEAD

OUT

PRESS.

XDUCER

HEAD

WASTE

OUT

SUPPRESSOR

HEAT EXCHANGER

SEPARATOR COLUMN

COLUMN HEATER (optional)

GUARD

WASTE

IN OUT

ELUENT

VALV E

Figure 2-6. ICS-1000 Flow Schematic

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ICS-1000 Ion Chromatography System

• Eluent from the eluent reservoirn flows first through the pump degas

assembly (if it is installed) and then through the eluent valve pump

p. It is then pushed through the pressure transducerq, which measures

the system pressure.

• From there, it is pushed through a pulse damperr, which smooths minor

pressure variations from the pump to minimize baseline noise. The eluent then flows into the injection valve.

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

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

• If the optional column heater is installed, the eluent/sample mixture is

pumped through the heat exchanger heater temperature.

• The mixture then goes to the guard and separator columnsv and through the

suppressor.

o to the

u, which heats the mixture to the column

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

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

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

suppressor, where it is used as the water source for the regenerant chamber. Flow is then routed to waste.

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2.3 The Chromeleon Interface

NOTE This section provides a brief overview of the

Chromeleon interface. For details, refer to the Chromeleon Help or user’s manual.

Chromeleon software is used for remote control of ICS-1000 operation. Two modes of software control are available: direct control and automated control.

• With direct control, you select operating parameters and commands from the

Chromeleon menu bar, toolbars, and Control Panels. Direct control commands are executed as soon as they are entered. Section 2.3.2 the commands available from the ICS-1000 Control Panels.

• With automated control, you create a list of samples (a sequence) to be

processed automatically. The sequence includes programs with commands and parameters for controlling the ICS-1000, acquiring sample data, and producing reports. Section 3.11.2

describes automatic sample processing.

2 • Features

describes

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ICS-1000 Ion Chromatography System

2.3.1 The Chromeleon Main Window and Browser

When you start Chromeleon, the main window and the Chromeleon Browser appear (see Figure 2-7

Figure 2-7. Chromeleon Main Window and Browser

NOTE The Chromeleon Browser looks and functions like

Windows Explorer, but do not confuse the two. If you copy files from the Chromeleon Browser into Explorer, the files will be corrupted.

The Browser displays the directories in which chromatographic data is located, and allows you to open, move, and delete data.

• The left pane of the Browser shows the directory tree structure. By

clicking the ‘+’ signs next to the folders and expanding the directory tree, you can access sequences, System Control Panels, Wellness Panels, and reports.

• The right pane displays information about the item selected in the left

pane.

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2.3.2 The ICS-1000 Control Panels

Chromeleon provides two types of Control Panels for the ICS-1000.

• System Control Panels are used for controlling and monitoring ICS-

1000 operation. System Control Panels are described below.

• The Wellness Panel is used for performing calibration and diagnostic

functions. The Wellness Panel is described in Section 5.1

System Control Panels

System Control Panels for the ICS-1000 are located in the Dionex Templates/Panels/Dionex_IC\ICS-1000 folder. Chromeleon provides

panels for each ICS-1000 system configuration. There are two styles of panels:

• Traditional system panels (see Figure 2-8) provide controls on a

single window with minimal graphics.

• System panels (see Figure 2-9) provide a more graphical interface

than the traditional style. On these panels, clicking a control often brings up another window in which you enter a value.

2 • Features

When you open a System Control Panel, select a panel that matches your system configuration and choose the style that you prefer.

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ICS-1000 Ion Chromatography System

Figure 2-8. ICS-1000 System Control Panel (Traditional)

Figure 2-9. ICS-1000 System Control Panel (Graphical)

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2 • Features

System Controls Overview

This section provides brief descriptions of the various controls available on the ICS-1000 System Control Panels.

NOTE The examples are from the traditional style of panel.

Sample

Datasource

Displays the database in which the chromatographic data for the sample is saved.

Sequence

Displays the sequence in which this sample is included.

Sample

Displays the name of the sample that is running.

Program

Displays the name of the program that is running.

Elapsed Time

Displays the time that has elapsed since the sample analysis began.

Run Time

Displays the total run time.

System

Startup

Starts the pump and suppressor. The flow rate and suppressor current settings that were in effect at system shutdown (see below) are restored.

Shutdown

Stops the pump and suppressor. The flow rate and suppressor current settings currently in effect are remembered and will be restored at system startup (see above).

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ICS-1000 Ion Chromatography System

Audit Trail

The Audit Trail displays an account of every event that occurs during ICS-1000 operation. This includes errors, status messages, operational events, etc.

Pump

Eluent Bottle

The entry field and gauge indicate the level of liquid (in liters) in the eluent bottle. This is a user controlled feature. The level must be entered by the user when the reservoir is filled. See Section 3.4.4

for details.

Connected

Connects the ICS-1000 to the Chromeleon Control Panel, enabling communication between the PC and the module. Clearing the check box disconnects the ICS-1000 from the PC.

Hold Mode

Indicates when an automatic (batch) run is on hold; pump flow is not stopped.

Stop Mode

Indicates when an automatic (batch) run is stopped; pump flow is also stopped.

Flow Rate

Sets the pump flow rate in mL/min.

Pressure

The sliders select the upper and lower pressure limits. The Pressure field displays the current pressure.

On, Off, Prime

Turn the pump on and off or start the pump priming function.

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Column Heater (Optional)

Detector

2 • Features

Inject Valve

Displays the current position of the inject valve. The position.

Eluent Flow Valve

Displays the current position of the eluent flow valve. The select the position.

Set Temp

Sets the temperature of the column heater.

Inject and Load buttons select the

Closed and Open buttons

Connected

Connects the ICS-1000 to the Chromeleon Control Panel, enabling communication between the PC and the module. Clearing the Connected check box disconnects the ICS-1000 from the PC.

Autozero

Sets the conductivity to zero.

Ready

Indicates if the detector is ready to begin data acquisition.

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ICS-1000 Ion Chromatography System

Signal

Displays the offset conductivity.

Data Rate

Sets the rate at which data points are recorded.

Supp. Type

Selects the type of suppressor installed.

SRS Current

Sets the current supplied to the suppressor.

Cell Temp

Sets the temperature of the cell.

SRS Mode

Selects whether the suppressor is on or off.

Show Plot

Displays the ICS-1000 detector signal plot in a separate window.

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2.4 System Component Details

This section provides details about ICS-1000 system components, including the vacuum degas assembly (optional), eluent valve, pump, injection valve, column heater (optional), suppressor, and conductivity cell.

2.4.1 Vacuum Degas Assembly (Optional)

The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user. The assembly, which must be installed in the ICS-1000 at the factory, consists of:

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

internal capacity of 17 mL

• A dual-stage diaphragm vacuum pump

• A solenoid valve

• An on-board vacuum sensor

• The electronics required to operate the vacuum pump

2 • Features

• Tubing, fittings, and other accessories

By default, the ICS-1000 monitors the degas pressure reading and turns the degas pump on and off as needed. A different degas operating mode can be selected from Chromeleon. To select degas operating options from Chromeleon, open the Server Configuration program, select the ICS-1000

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ICS-1000 Ion Chromatography System

device icon under the timebase, and select Properties from the Edit menu. Select the Options tab (see Figure 2-10

Figure 2-10. Server Configuration Properties: Degas Mode Options

Degas Mode Options

• Always Off: The degas pump is always off.

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

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

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

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

Cycle On and Off fields. Cycle On specifies for how

Cycle Off specifies the time

• Monitor: (default mode) The ICS-1000 monitors the degas pressure

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

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2.4.2 Eluent Valve

Figure 2-11. Eluent Valve

2.4.3 Pump

2 • Features

The eluent valve controls the flow from the eluent reservoir. It opens automatically when the pump is running and closes when the pump is off. The valve can also be opened and closed manually from the Chromeleon Control Panel (see Section 2.3.2 perform service procedures on pump components without eluent leaks occurring.

). This lets you

The ICS-1000 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 mobile phase into the secondary head (see

Figure 2-12

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

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ICS-1000 Ion Chromatography System

Pressure

Transducer

Secondary

Pump Head

Waste Valve

Outlet Check Valve

Primary Pump Head

Priming Valve

Inlet Check Valve

Figure 2-12. ICS-1000 Pump Components

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

NOTE The priming valve must be open when the pump is

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

Section B.12

Secondary Pump Head

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

Figure 2-12

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

NOTE The waste valve must be open when the pump is

being primed using the Prime button. For detailed priming instructions, see Section B.12

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2 • Features

Pressure Transducer

Flow exiting the secondary pump head is directed to the pressure transducer (see Figure 2-12

Pressure measurements, which can be monitored from the Chromeleon Control Panel, indicate that the pumping system is delivering smooth, accurate flow.

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. See

Section 4.1

for troubleshooting information if a pressure limit is

exceeded.

Pulse Damper

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

), which measures the system pressure.

Piston Seal Wash

The pump includes a piston seal wash assembly that can be set up to continuously rinse the back of the piston seals to remove salt crystals and prolong the life of the seals. To use this feature, an external water source must be connected. See Section B.21

for connection instructions.

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

Section 5.6

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

whenever you replace the main piston seals for the ICS-1000 pump.

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ICS-1000 Ion Chromatography System

2.4.4 Injection Valve

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

Sample In

Sample Loop

To Waste

The valve has two operating positions: Load and Inject (see Figure 2-13

LOAD POSITION

To Column

From Pum

Figure 2-13. Injection Valve Flow Schematics

Sample In

Sample Loop

INJECT POSITION

To Waste

To Colum

From Pum

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

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

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

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

Eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it. Section 3.10 describes how to inject samples.

Figure 2-14

plumbed at the factory with all tubing and fittings for connection to the pump, injection port, column, and waste. A 25-µL PEEK sample loop (P/N 042857) is installed between ports L (1) and L (4). Dionex offers

2-24 Doc. 031879-01 3/03

shows the injection valve connections. The injection valve is

Page 43

2 • Features

sample loops in various sizes. If necessary, the pre-installed 25-µL loop can be replaced with a loop that has a different sample injection volume.

Figure 2-14. Injection Valve Plumbing

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ICS-1000 Ion Chromatography System

2.4.5 Column Heater (Optional)

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

The heater temperature can be set to between 30 °C and 60 °C and it must be set at least 5 °C above the ambient temperature. Temperature is monitored via a thermistor mounted in the heater block. Setting the temperature to 0 °C turns off the column heater.

If the temperature exceeds 65 °C, the column heater is shut off and the error message “Column heater exceeds safe temperature.” is displayed in Chromeleon. See Section 4.1 for troubleshooting information.

The column heater can either be installed at the factory or ordered separately (P/N

058060).

Figure 2-15. Column Heater

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2.4.6 Suppressor

The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an Atlas Electrolytic Suppressor, Self-Regenerating Suppressor, or MicroMembrane Suppressor can be used with the ICS-1000.

For details about any of the suppressors or for information about selecting a suppressor for your application, refer to the suppressor manuals. The manuals are on the Dionex Reference Library CD-ROM (P/N 053891), located in the ICS-1000 Ship Kit (P/N 057905).

2.4.7 DS6 Heated Conductivity Cell

The ICS-1000 flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. Two passivated 316 stainless steel electrodes are permanently sealed into the PEEK cell body. The cell design provides efficient sweep-out, low volume (1 and low dispersion. Temperature control and compensation help ensure good peak reproducibility and baseline stability.

2 • Features

µL),

Temperature Control

Temperature directly affects the conductivity of a solution. For example, laboratory heating and air conditioning systems can cause a regular slow cycling in the baseline. This, in turn, can affect the reproducibility of an analysis. The higher the conductivity, the more pronounced the effect.

In ion analysis, the effect of temperature variation is minimized by suppressing eluent conductivity. To further reduce the effect of temperature variation, the ICS-1000 provides temperature control to the cell. A heater inside the cell regulates the temperature. The cell heater can be set to between 30 °C and 55 °C. The set temperature must be at least 7 °C above the ambient temperature. Setting the cell temperature to 0 °C turns off the cell heater.

Temperature Compensation

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

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ICS-1000 Ion Chromatography System

DS6 Heated Conductivity Cell Components

The cell front cover provides CELL IN and CELL OUT fittings for connecting the cell to the suppressor (see Figure 2-4 components are mounted behind the component panel. To replace, the cell remove the screws on the cell front cover and pull the entire cell assembly out through the component panel. See Section 5.9 instructions.

). The remaining cell

for cell replacement

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3 • Operation and Maintenance

This chapter describes routine operating and maintenance procedures for the ICS1000 Ion Chromatography System.

3.1 Operation Overview

Figure 3-1 illustrates the basic steps for routine operation of the ICS-1000.

Power up the system

Start Chromeleon

Set up the reservoir

Check all

connections

Prime the pump

Set operating

conditions

Equilibrate the

system

Prepare samples

Verify operating

status

Process samples

Figure 3-1. ICS-1000 Operation Flow Chart

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ICS-1000 Ion Chromatography System

Sample Processing Overview

Samples can be run either manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-2 batch sample processing. Samples can be loaded into the sample loop with an autosampler or with a syringe through the injection port on the ICS-1000 front door.

shows the typical steps for manual and

Man ual Sample

Processing

Using Chromeleon

Load the sample

Start data

acquisition

Autozero

Inject the sam ple

Stop data

acquisition

(Optional)

Save the manual

sequence data

Batch Sample

Processing

Using Chromeleon

Create a Sequence (Sequence Wizard)

Add the Sequence

to the Batch

Start the Batch

Figure 3-2. Sample Processing Overview

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3.2 Power Up the System

Power

Switch

3 • Operation and Maintenance

Press the power switch on the ICS1000 rear panel (see Figure 3-3 turn on the system power. Table 3-2 shows the ICS-1000 conditions at power up.

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

) to

Figure 3-3. ICS-1000 Rear Panel

Feature Power-Up Condition

Pump Off

Injection valve Load position

Cell Reading current value

Suppressor Off*

Cell heater Set to the last value used. The default when the

ICS-1000 is turned on for the first time is 35 °C.

Column oven temperature (Optional)

Table 3-2. ICS-1000 Power-Up Conditions

* When you start the suppressor, the value used last is restored.

Doc. 031879-01 3/03 3-3

Set to the last value used. The default when the ICS-1000 is turned on for the first time is 30 °C.

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ICS-1000 Ion Chromatography System

3.3 Start Chromeleon

NOTE See Section B.8 for how to set up Chromeleon, if you are

beginning operation of an ICS-1000 that has not been configured in a timebase.

1. If the Chromeleon Server is not running (the icon on the taskbar is crossed out

in red ), start the Server by right-clicking the icon and selecting Start

Server. When the server starts, the icon changes to gray

2. Start Chromeleon by selecting Start> Programs>Chromeleon> Chromeleon. The Chromeleon main window and the Browser will open.

Your screen display should resemble Figure 3-4

. If the Browser does not

open, select Browser from the File menu to open it.

Figure 3-4. Chromeleon Main Window and Browser

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3 • Operation and Maintenance

3. In the Browser, expand the Dionex Templates\Panels\Dionex_IC\ICS-1000 System Panels folder. Several ICS-1000 System Control Panels (.PAN files)

are provided, corresponding to various system configurations. There are two styles of panels:

• Traditional panels provide controls on a single window with minimal

graphics.

• System panels provide a more graphical interface than the traditional style

and include more controls. You can choose either style of panel, depending on your personal preference.

4. Open a panel for your system configuration by double-clicking its name in the list. For example, if your system includes an ICS-1000 and an AS50 autosampler, double-click either ICS-1000_Traditional_System_AS50.pan or ICS-1000_System_AS50.pan.

5. The Control Panel opens, unconnected (see Figure 3-5

). To connect to the timebase, open the Control menu and click the name of the ICS-1000 timebase from the list at the bottom of the menu.

Figure 3-5. ICS-1000 System Control Panel (Unconnected)

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ICS-1000 Ion Chromatography System

Figure 3-6 shows a connected Control Panel for an ICS-1000 system.

Figure 3-6. ICS-1000 System Control Panel (Connected)

NOTE The ICS-1000 Ion Chromatography System is designed

for use for IC (ion chromatography) and BioLC applications and should not be used for any other purpose. If there is a question regarding appropriate usage, contact Dionex.

3.4 Set Up the Eluent Reservoir

3.4.1 Prepare the Eluent

Prepare the eluent according to the instructions in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891).

3.4.2 Degas the Eluent

Eluent quality significantly affects the performance of the ICS-1000. To ensure optimal pump performance, observe the following precautions:

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3 • Operation and Maintenance

• Dionex strongly recommends vacuum degassing all eluents. This

helps prevent bubbles, caused by outgassing, from forming in the pump heads and the detector flow cell.

• The optional vacuum degas assembly provides programmable, online

degassing. The degas assembly must be installed in the ICS-1000 at the factory. If the ICS-1000 does not contain a degas assembly, manually degas eluents daily (following the instructions below) and store it in pressurized reservoirs.

Manual Degassing of Eluent

1. Prepare the eluent required for the application and pour it into a vacuum flask

1. Pour the deionized water into a vacuum flask

2. Attach the flask to a vacuum pump or water aspirator.

3. Vacuum degas the eluent deionized water for 5 to 10 minutes by shaking or sonication.

4. Remove the flask from the vacuum. Do not allow water to flow

from the aspirator back into the flask.

5. Pour the degassed eluent deionized water into a pressurizable reservoir. Do not shake the eluent.

6. Install an end-line filter on the eluent deionized water line (see

Section 3.4.3

7. Pressurize the reservoir (see Section B.20

3.4.3 Filter the Eluent

Filtering removes small particulates in the eluent that may contaminate the pump check valves and cause erratic flow rates or loss of prime. An end-line filter (P/N 045987) is provided in the ICS-1000 Ship Kit (P/N 057905) for this purpose.

Install the end-line filter on the end of the eluent line, inside the reservoir. Verify that the end of the filter extends to the bottom of the reservoir and that the filter is submerged in eluent. This prevents air from being drawn through the lines. Refer to the Pressurizable Reservoir Installation Instructions for details.

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ICS-1000 Ion Chromatography System

3.4.4 Fill the Reservoir

Fill the reservoir with the prepared eluent.

3.4.5 Set the Eluent Level

After filling the reservoir, enter the volume of liquid in the reservoir on the Chromeleon the eluent usage by monitoring the flow rate and the length of time the pump is on, and updates the warning first appears if the level falls below 200 mL. Warnings are repeated at 100 mL and 0 mL.

In order for the eluent level displayed on the Control Panel to be accurate, the level must be entered by the user when the reservoir is filled. The ICS-1000 does not automatically detect when the reservoir is filled, nor when it is empty.

Control Panel (see Figure 3-6). The ICS-1000 determines

Eluent Level field as the eluent is used up. A

Enter the volume of

liquid in the reservoir

Figure 3-7. Setting the Eluent Level

3.4.6 Connect the Reservoir

If it is not already connected, connect the ELUENT BOTTLE OUT line from the reservoir cap to the and cable chase on the top of the ICS-1000.

ELUENT IN line, which extends from the plumbing

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

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3.5 Check All Connections

(

)

1. Make sure the reservoir is filled and the tubing connecting the reservoir to the ICS-1000 tubing is securely connected.

2. Make sure the USB cable from the computer is connected to the USB receptacle on the ICS-1000 rear panel.

3.6 Prime the Pump

If you changed eluent or if the eluent lines are dry, prime the lines first with a syringe before priming the pump. See Section B.14.1 for instructions.

1. Verify that the priming valve on the primary pump head (see Figure 3-8) is closed (turned all the way clockwise).

2. Open the waste valve on the secondary pump head by turning the knob onequarter to one-half turn counterclockwise. Opening the valve directs the eluent flow path to waste and eliminates backpressure.

3 • Operation and Maintenance

Secondary

Pump Head

Waste Valve

(open)

Primary

Priming Valve

Pump Hea

Figure 3-8. Priming the Pump

3. Press

Prime on the Chromeleon Control Panel. A confirmation message is

displayed, asking if you opened the waste valve. Select

Yes. The pump will

begin pumping at approximately 3.0 mL/min.

4. Continue priming the ICS-1000 until all air and previous eluent are purged and no air bubbles are exiting the waste line.

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ICS-1000 Ion Chromatography System

5. Press Pump Off.

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

3.7 Set System Operating Conditions

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

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

Set or verify system operating parameters from the Chromeleon Control Panel. Operating parameters can also be set automatically by loading a Chromeleon sequence.

NOTE Clicking the System Startup button on the Chromeleon

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

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

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

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

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

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3 • Operation and Maintenance

3.8 Equilibrate the System and Verify Operational Status

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

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

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

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

Autozero button

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

system. Release the gas by removing the pump fitting on the injection valve port, labeled fitting.

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

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

pump. See Section 4.3

for additional troubleshooting information.

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

plumbing. See Section 4.7

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

Section 4.12

See Section 4.13 fluctuations in readings).

6. Verify that the cell heater is at the set point and is stable. The temperature is at equilibrium when the Set Temperature and Current Temperature readings on the Control Panel are the same.

for troubleshooting information if the conductivity is too high.

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

for troubleshooting information.

µS for a system set up

µS for a system set up for cation analyses. See

7. Verify that the column heater temperature (if installed) is at the set point and stable. The temperature is at equilibrium when the Set Temperature and Current Temperature readings on the Control Panel are the same.

The system is now ready for sample processing.

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ICS-1000 Ion Chromatography System

3.9 Prepare Samples

NOTE Sample preparation can be performed while the system

is equilibrating.

3.9.1 Collecting and Storing Samples

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

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

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.

° C (39° F) will reduce, but not

3.9.2 Pretreating Samples

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

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

Before injection, pretreat samples that may contain high concentrations of interfering substances by putting them through Dionex OnGuard cartridges. Refer to the Installation and Troubleshooting Guide for OnGuard Cartridges (Document No. 032943) for instructions.

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3.9.3 Diluting Samples

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

Use eluent or ASTM filtered, Type I (18-megohm) deionized water or eluent 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.

3 • Operation and Maintenance

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ICS-1000 Ion Chromatography System

3.10 Loading and Injecting Samples

Samples can be loaded into the sample loop through the injection port on the front door using a syringe or vacuum syringe, or they can be loaded using an autosampler.

For autosampler injections, the injection port tubing is disconnected from the ICS1000 injection valve and replaced by the autosampler outlet tubing. Other setup requirements depend upon the model of autosampler.

Setup for an AS40 Autosampler

A relay or TTL connection is required for Chromeleon to control sample loading. See Section B.18

Setup for an AS50 Autosampler

To use an AS50 autosampler with the ICS-1000, the AS50 must meet the following requirements:

• An injection valve cannot be installed in the AS50

• The AS50 must have Moduleware version 1.11 or later installed

for AS40 autosampler installation instructions.

• Control of the ICS-1000 injection valve must be enabled in the AS50

The following AS50 models are configured at the factory to meet the above requirements:

• AS50 without injection valve (P/N 061309)

• AS50 without injection valve; with sample preparation (P/N 061310)

• AS50 without injection valve; with sample preparation and sample tray

cooling (P/N 061311)

• AS50 without injection valve; with sample tray cooling (P/N 061312)

See Section B.17

After the AS50 is configured for use with the ICS-1000, all AS50 modes of injection (full-loop, partial-loop, and partial-loop limited-sample) are supported. In addition, all AS50 injection valve commands (whether issued from the AS50 front panel or from Chromeleon) will control the ICS-1000 injection valve. For Chromeleon control, the AS50 must be added to the ICS-1000 timebase (see

Section B.8

for AS50 autosampler installation instructions.

). For front panel control, the AS50 and ICS-1000 can be set up for

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3 • Operation and Maintenance

stand-alone operation. This requires a TTL cable connection between the AS50 and the ICS-1000. See Section C.3

for stand-alone setup instructions.

3.10.1 Loading Samples with a Syringe

1. Make sure the injection port on the ICS-1000 front door (see

Figure 2-1

(see Figure 3-9

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

Figure 3-9. Injection Valve Connections

2. Fill the 1 cc syringe (P/N 016388) provided in the ICS-1000 Ship Kit (P/N 057905) with a calibration standard or sample.

3. Insert the syringe into the injection port on the ICS-1000 front door.

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

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

6. Leave the syringe in the port.

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

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ICS-1000 Ion Chromatography System

3.10.2 Loading Samples with a Vacuum Syringe

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

Figure 3-9

PEEK or Teflon® tubing.

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

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

4. Insert the 1 cc syringe (P/N 016388) provided in the ICS-1000 Ship Kit (P/N 057905) into the injection port on the ICS-1000 front door (see Figure 2-1 injection valve.

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

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

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

3.10.3 Loading Samples with an Autosampler

1. Verify that the autosampler output line is connected to port S (5) of the ICS-1000 injection valve.

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

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

• Include the commands for controlling sample loading in a

Chromeleon program. See the examples in Section 3.10.5

• Enter the commands for loading the sample from the autosampler

front panel.

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

NOTE If you are running the ICS-1000 without

Chromeleon control, see Section C.3 alone setup and operation instructions using an AS50 autosampler.

for stand-

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3 • Operation and Maintenance

3.10.4 Injecting Samples

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

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

(see Figure 3-6

• Automatically: Include the Inject command in a Chromeleon

program. See the examples in Section 3.10.5

3.10.5 Example Chromeleon Commands for Loading and Injecting Samples

The following examples show commands for loading and injecting samples using an AS50 or AS40 autosampler.

Example AS50 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 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

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ICS-1000 Ion Chromatography System

AS40 Program Command Notes:

1. Close the ICS-1000 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.

5. Stop data acquisition.

3.11 Process Samples

Samples can be run either manually (one at a time) or automatically (in groups or “batches”).

3.11.1 Manual Sample Processing

To process samples manually, select operating parameters and commands from the Chromeleon menu bar, toolbars, and Control Panel. Commands are executed as soon as they are entered.

1. Complete the steps in Sections 3.2

through 3.8 to prepare for

operation and start up the ICS-1000.

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

3. Select Acquisition On from the Control menu. Chromeleon records the signal supplied by the detector and displays the signal plot on the Control Panel.

4. Click the

5. Inject the sample (see Section 3.10.4

Autozero button on the Control Panel.

6. Monitor the chromatogram on the Control Panel and select Acquisition Off from the Control menu when sample data is collected.

NOTE Data from Chromeleon manual processing is saved

in the MANUAL sequence folder under the local datasource. This data is overwritten each time a

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3 • Operation and Maintenance

new manual sample is processed. To save the data from a manual run, select the MANUAL folder, select Save As from the File menu, and enter a new name for the sequence.

3.11.2 Automatic (Batch) Sample Processing

For batch processing, you use Chromeleon to create a list of samples (a sequence) to be processed automatically. For each sample, the sequence includes a program with commands and parameters for controlling the ICS-1000, controlling the autosampler (if used), and acquiring sample data. The sequence also includes a quantification method for peak identification and area determination. Additional sample processing parameters are included in the sequence (for example, the sample name, sample type, injection volume, etc.).

After defining the sequence, you can start batch processing.

1. Complete the steps in Sections 3.2

through 3.8 to prepare for

operation and to start up the ICS-1000.

2. Create a new sequence or modify an existing one.

To create a new sequence:

a. In the Browser, select File> New. Select Sequence (using

Wizard) and click OK.

b. Complete the steps in the Sequence Wizard, adding the desired

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

NOTE A simple way to get started is to select the “Use

Application Template” option in Step 4 of the Sequence Wizard. This option lets you select a column and suppressor type from a list of applications. The Wizard then copies a program and quantification method, appropriate for the selected application, to the sequence folder and adds them to the sequence definition.

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ICS-1000 Ion Chromatography System

3. To start the sample processing, make sure the System Control Panel is open (see Section 3.3 from the Batch menu. The Batch dialog box opens (see Figure 3-10

Figure 3-10. Batch Dialog Box

) and is the active window. Then, select Edit

4. Click the Add button on the Batch List tab and add the sequence you created in Step 2

Figure 3-11. Batch Dialog Box with an Example Sequence Added to the Batch List

. See Figure 3-11 for an example.

5. To start the batch, click Start.

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3.12 Maintenance

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

As Needed

• Regularly check the eluent reservoir to see if it needs to be refilled.

• Make fresh eluent as needed.

Daily

• Check the ICS-1000 component mounting panel (see Figure 2-4) for leaks or

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

• Check the waste container daily and empty when needed.

Weekly

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

pinched lines. Replace damaged lines.

3 • Operation and Maintenance

). Rinse off any

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

evidence of liquid leaks. If piston seal wash tubing is not connected, check the drain tubes at the rear of the pump heads for evidence of moisture. 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 5.6

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

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

NOTE It is especially important to regularly replace end-line

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

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Every Six Months

• Calibrate the cell (see Section 5.1.2).

• Calibrate the vacuum degas assembly (see Section 5.1.4).

• Replace the pump piston rinse seals and piston seals (see Section 5.6).

Yearly

• Rebuild the injection valve (see Section 5.4).

• Replace the AS40 Automated Sampler tip and tubing. The AS40/ASM

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

• Perform the AS50 preventive maintenance procedure. The AS50 Maintenance

Kit (P/N 060581) contains all of the required components and instructions for performing the procedure.

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4 • Troubleshooting

This chapter is a guide to troubleshooting problems that may occur while operating the ICS-1000 Ion Chromatography System.

• Section 4.1 describes error messages and how to troubleshoot them. Table 4-3

lists the messages and the page numbers where they are described.

• The remaining sections in this chapter describe other operating problems and

how to resolve them. Table 4- 4 numbers where they are described

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

Alarms and Error Conditions See

COLUMN HEATER EXCEEDS SAFE TEMPERATURE

COLUMN HEATER OPEN CIRCUIT

COLUMN HEATER SHORT CIRCUIT

DEGAS CALIBRATION FAILED

HARDWARE NOT PRESENT

LEAK SENSOR WET

LOAD/INJECT VALVE ERROR

OPTION NOT INSTALLED

PRESSURE SLOPE CALIBRATION ERROR

PUMP MOTOR LOST CONTROL

PUMP PRESSURE HARDWARE ERROR

PUMP OVER PRESSURE

PUMP UNDER PRESSURE

SUPPRESSOR OVER CURRENT

SUPPRESSOR OVER VOLTAGE

SUPPRESSOR OVER POWER

SUPPRESSOR NOT CONNECTED

lists the operating problems and the page

page 4-3

page 4-4

page 4-5

page 4-6

page 4-7

page 4-8

Table 4-3. ICS-1000 Alarms and Error Messages Summary

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ICS-1000 Ion Chromatography System

Alarms and Error Conditions See

SUPPRESSOR STOPPED FOR FLOW RATE

Table 4-3. ICS-1000 Alarms and Error Messages Summary (Continued)

4.1 Alarms and Error Conditions

If any of the following alarm conditions occurs, a message is displayed in the Chromeleon Audit Trail.

COLUMN HEATER EXCEEDS SAFE TEMPERATURE

This error occurs when the column heater temperature is higher than the maximum allowed. This error may occur if the ICS-1000 is operating in an extreme environment (greater than 40 °C).

To troubleshoot:

• Refer to Section A.3 for environmental specifications.

COLUMN HEATER OPEN CIRCUIT

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

4 • Troubleshooting

To troubleshoot:

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

2. If the error persists, the column heater may be faulty. Replace the column heater (see Section 5.11

COLUMN HEATER SHORT CIRCUIT

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

To troubleshoot:

• Replace the column heater (see Section 5.11).

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DEGAS CALIBRATION FAILED

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

To troubleshoot:

1. Retry the calibration.

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

HARDWARE NOT PRESENT

This error indicates an error in the ICS-1000 electronics.

To troubleshoot:

• Contact Dionex for assistance. The ICS-1000 electronics components

cannot be serviced by the user.

LEAK SENSOR WET

The leak sensor is installed in the drip tray at the bottom of the component

panel (see Figure 2-4 problem and the “Leak sensor wet” error message appears.

To troubleshoot:

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

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

Section 4.2

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

4-4 Doc. 031879-01 3/03

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

for detailed troubleshooting of various types of leaks.

Page 73

4 • Troubleshooting

LOAD/INJECT VALVE ERROR

If the injection valve fails to switch position within 1 second of being toggled, the ICS-1000 Moduleware reports an error to Chromeleon and the “Load/Inject valve error” message appears.

To troubleshoot:

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

2. Turn off the ICS-1000 power briefly and then restart.

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

Inject

buttons on the ICS-1000 Control Panel in Chromeleon.

Load and

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

OPTION NOT INSTALLED

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

To troubleshoot:

• Check the Chromeleon Server Configuration program to verify that the

option is enabled.

PRESSURE SLOPE CALIBRATION ERROR

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

To troubleshoot:

• This is a service level error message. Contact Dionex for assistance.

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ICS-1000 Ion Chromatography System

PUMP MOTOR LOST CONTROL

This error indicates an error in the pump controller electronics.

To troubleshoot:

• Contact Dionex for assistance. The ICS-1000 electronics components

cannot be serviced by the user.

PUMP PRESSURE HARDWARE ERROR

This error indicates an error in the pump controller electronics.

To troubleshoot:

• Contact Dionex for assistance. The ICS-1000 electronics components

cannot be serviced by the user.

PUMP OVER PRESSURE

The ICS-1000 has a maximum system pressure limit of 34.5 MPa (5000 psi). The pressure limit can be lowered from Chromeleon (in the Server Configuration or in the control program). If the system pressure exceeds the set limit for at least 0.5 seconds, the pump stops and the “Pump over pressure” error message appears.

To troubleshoot:

1. Check for blockages in the liquid lines by working your way backward from the cell to the pump. See Figure 2-6 schematic).

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

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

4. Restart the pump.

for the flow

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4 • Troubleshooting

PUMP UNDER PRESSURE

The ICS-1000 has a minimum pressure limit of 0. The low pressure limit can be raised from Chromeleon (in the Server Configuration or in the control program). If the system pressure falls below the low pressure limit, the pump stops and the “Pump under pressure” error message appears.

To troubleshoot:

1. Make sure the eluent reservoir is full.

2. Check for liquid leaks (see Section 4.2

3. Check that the waste valve is closed.

4. Prime the pump (see Section B.12

5. Restart the pump.

SUPPRESSOR OVER CURRENT

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

To troubleshoot:

1. Follow the instructions in the suppressor manual to regenerate the suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891), located in the ICS-1000 Ship Kit (P/N 057905).

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

3. If a malfunction in the suppressor controller is suspected, contact Dionex for assistance. The ICS-1000 electronics components cannot be serviced by the user.

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ICS-1000 Ion Chromatography System

SUPPRESSOR OVER VOLTAGE

This error appears if you turn on the suppressor and the ICS-1000 cannot establish a connection with the suppressor.

To troubleshoot:

1. Check the suppressor cable connection (see Section 5.10

2. If the error persists, replace the suppressor (see Section 5.10

SUPPRESSOR OVER POWER

This error appears when, in order to maintain the selected current, the ICS1000 is required to apply a higher voltage than the suppressor can support.

To troubleshoot:

• Reduce the flow rate.

• Rehydrate the suppressor. Refer to the suppressor manual for instructions.

Suppressor manuals are included on the Dionex Reference Library CDROM (P/N 053891), located in the ICS-1000 Ship Kit (P/N 057905).

• If the error persists, replace the suppressor (see Section 5.10).

SUPPRESSOR NOT CONNECTED

This error appears if you turn on the suppressor and the ICS-1000 cannot establish a connection with the suppressor.

To troubleshoot:

1. Check the suppressor cable connection (see Section 5.10

2. If the error persists, contact Dionex for assistance. There may be a problem in the suppressor controller electronics. The ICS-1000 electronics components cannot be serviced by the user.

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SUPPRESSOR STOPPED FOR ZERO FLOW RATE

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

To troubleshoot:

• If the pump stopped unexpectedly, see Section 4.5 for pump

troubleshooting information.

4.2 Liquid Leaks

• Leaking fitting

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

4 • Troubleshooting

). Refer to Installation of Dionex Liquid Line

• Broken liquid line

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

• Blocked or improperly installed line

Make sure the lines are not crimped or otherwise blocked. Also, if the blocked line is a waste line, make sure it is not elevated at any point after it exits the ICS-1000. If a line is blocked, replace it (see Section 5.3

• Loose pump check valve

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.

If the leak persists, replace the check valve (see Section 5.5

• Leaking seal wash port

Leaking from the seal wash port indicates a leaking piston seal. Replace the seal (see Section 5.6

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ICS-1000 Ion Chromatography System

• Damaged pump piston seal

1. Replace the piston seal (see Section 5.6

2. If the leak persists, replace the piston (see Section 5.7

• Pump head not tight against casting

Carefully tighten the pump head mounting nuts 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) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings. The pressure transducer cannot be serviced by the user. Contact Dionex for assistance.

• Leaking pump head waste valve

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

Overtightening may damage the valve and the pump head.

If the leak persists, replace the waste valve O-ring (see Section 5.8

• Leaking suppressor

Refer to the suppressor manual for troubleshooting procedures. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891), located in the ICS-1000 Ship Kit (P/N 057905).

• Leaking injection valve

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

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

• Leaking 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.

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4 • Troubleshooting

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

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

• Empty eluent reservoir and/or no eluent connected

Fill the reservoir. Make sure all connections are secure.

• Eluent improperly or insufficiently degassed

If the ICS-1000 does not contain a vacuum degas assembly, degas the eluent manually (see Section 3.4.2

If the ICS-1000 contains a vacuum degas assembly, check the degas settings:

1. Open the Chromeleon Server Configuration program, select the ICS1000 device icon under the timebase and select Properties from the Edit menu (or double-click the ICS-1000 device icon).

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

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ICS-1000 Ion Chromatography System

Figure 4-1. ICS-1000 Server Configuration Properties: Options

3. Verify that the Degas check box is enabled under Installed Options.

4. Check the Degas Mode settings. Select either the Monitor option or the Cycle option. If you select Cycle, set the time on to 30 seconds and the time off to 10 minutes. If Cycle is already selected, try increasing the time on or decreasing the time off.

• End-line filter is dirty or clogged

When new, end-line filters (P/N 045987) are pure white. If the system is in continuous operation, change the end-line filter weekly, or whenever it becomes discolored. Replace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent. See the Pressurizable Reservoir Installation Instructions for more information about end-line filters.

NOTE It is especially important to regularly replace end-line

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

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4 • Troubleshooting

• Blockages in inlet tubing

Kinked or clogged tubing causes the pump to be “starved” for eluent. Replace the tubing and fittings (see Section 5.3

• Dirty check valve

Clean or replace the pump check valve (see Section 5.5

• Liquid leaks at junction between pump head and pump casting

Use the open-end wrench (P/N 014605) provided in the ICS-1000 Ship Kit (P/N 057905) to tighten the two acorn nuts that attach the pump head to the pump housing (see Figure 5-4

If the leak persists, replace the piston seal (see Section 5.6

• Liquid leaks from the seal wash port

Replace the piston seal (see Section 5.6

• Scratched pump piston

Check the pump pistons for scratches and replace if necessary (see

Section 5.7

4.4 Pump Does Not Start

• No power (front Power LED indicator is not lit)

Check that the power cord is plugged in.

Check the main power fuses and replace if needed (see Section 5.16

• No communication between ICS-1000 and Chromeleon

). Tighten the nuts evenly (12 in-lb torque).

Verify that the USB cable is connected correctly. See Section B.5 installation instructions.

for

• Pump is turned off

Turn on the pump from the Chromeleon Control Panel.

• Flow rate is set to 0

Set the flow rate from the Chromeleon Control Panel.

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ICS-1000 Ion Chromatography System

4.5 No Flow

• Pump waste or priming valve open (see Figure 4-2).

Close the valves by turning the knobs clockwise until fingertight. DO NOT OVERTIGHTEN! Overtightening may damage the valve and the pump head.

Waste Valve

Priming Valve

Figure 4-2. Waste and Priming Valves

• Flow rate is set to 0

Set the flow rate from either the Chromeleon Control Panel.

• Eluent valve is closed

Open the eluent valve from either the Chromeleon Control Panel.

• Pump not primed

Prime the pump (see Section B.12

• Broken pump piston

Replace the piston (see Section 5.7

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Page 83

4.6 Erratic Flow/Pressure Reading

• Pump needs priming

4 • Troubleshooting

Prime the pump (see Section B.12

• Damaged piston seal

Replace the piston seal (see Section 5.6

• Dirty pump check valve

Clean or replace the check valve (see Section 5.5

• Leaking liquid lines or fittings

Check the liquid lines and fittings for small leaks. Tighten or, if necessary, replace the liquid line connection (see Section 5.3 Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is on the Dionex Reference Library CD-ROM (P/N 053891).

4.7 Excessive System Backpressure

• Restriction in the 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 on the Dionex Reference Library CD-ROM (P/N 053891). If you have trouble isolating the restriction, refer to Section 5.2

). Refer to Installation of

• 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 5.3

• Flow rate through the columns too high

Set the correct rate for your application. If an incorrect flow rate calibration is suspected, calibrate the flow (see Section 5.1.3

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ICS-1000 Ion Chromatography System

• 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), located in the ICS-1000 Ship Kit (P/N 057905).

• Contaminated columns

Clean the columns as instructed in the column manual.

• Plugged injection valve passages

Rebuild the injection valve (see Section 5.4

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 be the result of a contaminated standard or eluent, or a malfunctioning 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.

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

Install or replace the end-line filter on the end of the deionized water line (see

Section 3.4.3

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• Malfunctioning injection valve

4 • Troubleshooting

1. Rebuild the injection valve (see Section 5.4

2. If the valve leak persists, contact Dionex for assistance.

4.9 Nonreproducible Peak Height or Retention Time

• Column overloading

Dilute the sample (see Section 3.9

• 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 B.12

4.10 Abnormal Retention Time or Selectivity

• Contaminated or incorrect eluent

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

• Contaminated or degraded sample

Take appropriate precautions when preparing and storing samples to prevent contamination and degradation (see Section 3.9

• 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), located in the ICS-1000 Ship Kit (P/N 057905).

2. If cleaning is unsuccessful, replace the column.

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ICS-1000 Ion Chromatography System

4.11 No Cell Response

• Cell not properly installed

Verify that the cell front cover is flush against the component panel. If necessary, tighten the two mounting screws. When the cell is correctly installed and the screws tightened, an electronics connector on the cell plugs into a receptacle inside the ICS-1000.

• No flow from pump

This condition has several possible causes. See Section 4.4 for details.

• Cell electronics malfunctioning

Use the Chromeleon Wellness Panel diagnostics to test the electronics (see

Section 5.1

reading is outside the tolerance range (less than 1 µS), the electronics are malfunctioning. Contact Dionex for assistance. The ICS-1000 electronics cannot be serviced by the user.

and the Chromeleon online Help for instructions). If the variance

4.12 High Cell Output

• Background not suppressed by suppressor

Verify that the suppressor is turned on and the current is set to the correct value. Refer to the suppressor manual for additional troubleshooting guidance. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891), located in the ICS-1000 Ship Kit (P/N 057905).

• Sample concentration too high

Dilute the sample Section 3.9.3

• Wrong eluent

and Section 4.5

Check that you are using the correct eluent for your application.

• Background conductivity not offset from conductivity reading

Before making an injection, allow the background conductivity to equilibrate, and then press

4-18 Doc. 031879-01 3/03

Autozero on the Chromeleon Control Panel.

Page 87

• Cell out of calibration

4 • Troubleshooting

Recalibrate the cell (see Section 5.1.2

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 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 suppressor eluent ports.

• Pump not properly primed

Prime the pump (see Section B.12

• Contaminated or incorrect eluent

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

• Rapid changes in ambient temperature

Make sure the ambient temperature is between 4 and 40 °C (40 and 104 °F).

Make sure air conditioning and heating vents are directed away from the ICS1000 and the ICS-1000 front door is closed.

• Insufficient system equilibration following changes to operating

parameters; especially apparent when operating at high sensitivities

Allow a longer system equilibration time (up to 2 hours) before starting operation.

• 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), located in the ICS-1000 Ship Kit (P/N 057905).

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ICS-1000 Ion Chromatography System

• Cell above or below temperature

Contact Dionex for assistance.

• Damaged piston seal

Replace the piston seal (see Section 5.6

4.14 Vacuum Degas Assembly Does Not Run

• Degas option not enabled in Chromeleon

a. Open the Chromeleon Server Configuration program. Select the ICS-

1000 device icon under the timebase and select Properties from the Edit menu (or double-click the ICS-1000 device icon).

Select the Options tab (see Figure 4-3

Figure 4-3. ICS-1000 Server Configuration Properties: Options.

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4 • Troubleshooting

b. Under Installed Options, verify that the Degas check box is selected.

c. Under Degas Mode, verify that the Always Off option is not selected. If

it is, select one of the following settings:

• Cycle, and select On: 30 seconds and Off: 10 minutes

• Monitor

d. If the Degas Mode settings are correct, but the degas assembly still does

not run, test the assembly by selecting the Always On option. The pump should turn on immediately. If it does not, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance.

Select the Degas Mode, Always On option only when testing the vacuum degas assembly. Do not select the Always On option for routine use.

e. If the degas pump runs when you select Always On, but does not run

when Monitor mode is selected, recalibrate the degas assembly (see

Section 5.1.4

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ICS-1000 Ion Chromatography System

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5•Service

This chapter describes ICS-1000 service and repair procedures that the user can perform. All 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 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

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

Substituting non-Dionex parts may impair ICS-1000 performance, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information.

5.1 Diagnostic and Calibration Procedures

Diagnostic and calibration procedures are performed from the Chromeleon Wellness Panel (see Figure 5-1

For an overview of the Wellness Panel features, see Section 5.1.1 on performing calibration and diagnostic procedures, see the following sections:

• Calibrating the Conductivity Cell (Section 5.1.2)

• Calibrating the Flow Rate (Section 5.1.3)

• Calibrating the Vacuum Degas Assembly (Section 5.1.4)

. For instructions

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ICS-1000 Ion Chromatography System

5.1.1 Chromeleon Wellness Panel Overview

NOTE Do not open a System Wellness Control Panel if the

name includes "Service.pan." These Wellness panels are reserved for use by Dionex Service Representatives.

To Open the Wellness Panel

1. Open the Chromeleon Browser and expand the Dionex Templates folder.

2. Expand the Panels folder and then the Wellness folder.

3. In the right pane of the Browser window, double-click ICS- 1000_1500_2000_Wellness_user.pan.The Wellness Panel appears.

4. Open the Control menu and click the name of the ICS-1000 timebase at the bottom of the menu. This connects the Wellness Panel to the ICS-1000 and enables the controls on the panel.

Figure 5-1. Chromeleon Wellness Panel

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5•Service

Use the Wellness Panel to perform the following functions:

• Calibrate the pump flow rate

• Calibrate the vacuum degas assembly

• Calibrate the conductivity cell

• Test the conductivity cell electronics, using a dummy cell

• Upload calibration values from the ICS-1000 to the Chromeleon

Wellness database

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ICS-1000 Ion Chromatography System

5.1.2 Calibrating the Conductivity Cell

When to Calibrate

• After every 6 months of use

NOTE Do not use this procedure to calibrate a new cell. If you

are replacing a cell, see the instructions in Section 5.9 install the new cell and calibrate it.

Items Needed Description

1.0 mM KCl solution Prepare by dissolving 0.07456 g of reagent-

grade KCl in 1 liter of 18-megohm DI water.

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

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

1. Open the ICS-1000 Wellness Panel in Chromeleon (see

Section 5.1.1

2. On the Wellness Panel under Electric Conductivity Cell Calibration, click Offset Cal.

3. When the offset calibration is complete, click Slope Cal on the Wellness Panel.

4. Disconnect the pump output line from the injection valve.

5. Disconnect the line from the suppressor

ELUENT OUT port to the cell

inlet and connect the pump output line directly to the cell inlet.

6. Verify that there is a minimum of 7 MPa (1000 psi) of backpressure.

7. On the Wellness Panel under Conductivity Cell Calibration, click

Cell 35 C

. Allow the cell to reach this temperature and then wait an

additional 5 minutes to let it stabilize.

8. Select

1.00 mL/min to begin pumping 1.0 mM KCl through the cell at

1.0 mL/min.

9. Wait until the total conductivity reading stabilizes (in about 15 minutes) and then select Calibrate on the Wellness Panel.

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5•Service

After calibration, the conductivity reading should be 147.00 ± 2 µS and the cell constant should be between 120 and 180. If this is not the case, contact Dionex for help.

10. Click Log to record the new calibration values in the Audit Trail.

11. Flush the KCl solution from the system by pumping deionized water through the cell. When the conductivity drops to less than 1 stop the pump.

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

µS/cm,

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ICS-1000 Ion Chromatography System

5.1.3 Calibrating the Flow Rate

When to Calibrate

If you run the ICS-1000 Operational Qualification or Performance Qualification and it 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)

• Deionized water

• Balance capable of weighing more than 10 grams with 0.001 grams

readability

• Tared beaker

To Calibrate

1. Open the ICS-1000 Wellness Panel in Chromeleon (see

Section 5.1.1

2. Verify that there is 14 ± 1.4 MPa (2000 ± 200 psi) of backpressure.

3. On the Chromeleon Wellness Panel under Pump Flow Rate Calibration, select Reset Cal.

4. Select

1 mL/min to set the flow rate and begin pumping deionized

water.

5. Allow the pump to stabilize for 20 minutes.

6. Click

5.00 min to start the timer. Immediately start collecting water

into the tared beaker.

7. Collect the water for exactly 5.00 minutes.

8. Enter the weight of the water (in grams).

9. Click

Calibrate to download the value to the ICS-1000.

10. To recheck the value, wait at least 15 minutes, and then repeat the calibration.

11. Click

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Log to record the new calibration value in the Audit Trail.

Page 97

5.1.4 Calibrating the Vacuum Degas Assembly

When to Calibrate

• After every 6 months of use

1. Open the ICS-1000 Wellness Panel in Chromeleon (see

Section 5.1.1

2. On the Wellness Panel under Degas Calibration, select Calibrate. The degas pump runs for 90 seconds to allow a vacuum to be created. After 90 seconds, the vacuum degas pressure reading is recorded. When the vacuum degas assembly is running in monitor mode, this calibration value is used to determine when to turn on the degas pump.

5•Service

3. Click

Log to record the new calibration value in the Audit Trail.

5.2 Isolating a Restriction in the Liquid Lines

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

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

2. Follow the ICS-1000 flow schematic in Figure 5-2 through the system, beginning at the suppressor loosen each fitting and observe the pressure. The connection at which the pressure drops abnormally indicates the point of restriction.

NOTE The numbers on the flow schematic indicate the order in

which liquid flows through the system components.

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 (see Section 5.3

and work backward

Regen Out exit. One at a time,

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ICS-1000 Ion Chromatography System

PUMP

DEGAS

(Optional)

ELUENT

OUT

COND

OUT

CELL

PULSE

DAMPER

SAMPLE

WASTE

VALV E

OUT

PUMP PUMP

HEAD

OUT

PRESS.

XDUCER

HEAD

WASTE

OUT

SUPPRESSOR

HEAT EXCHANGER

SEPARATOR COLUMN

COLUMN HEATER (optional)

GUARD

WASTE

IN OUT

ELUENT

VALV E

Figure 5-2. ICS-1000 Flow Schematic

NOTE The numbers on the flow schematic indicate the

order in which liquid flows through the system components.

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5.3 Replacing Tubing and Fittings

The ICS-1000 is plumbed with the tubing and tubing assemblies listed below.

Tubing Size and Type Color Used For

5•Service

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

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

0.50-mm (0.020-in) ID PEEK (P/N 042855)

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

1.58-mm (0.062-in) ID Teflon® (P/N 014157)

25 µL sample loop (P/N 042857)

Red Connection from pump pulse damper

to pressure transducer

Black Connections between other system

components

Orange Connection from injection port to

injection valve

Green Connection from injection valve to

waste

Clear Connection from pump to degas or

eluent reservoir; pump waste

Orange Connection between ports

L (4) on the injection valve

L (1) and

• 10-32 fittings (P/N 043275) 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 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 suppressor

REGEN OUT port and the eluent reservoir.

Doc. 031879-01 3/03 5-9

Page 100

ICS-1000 Ion Chromatography System

5.4 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 from the ICS-1000 Control Panel in Chromeleon.

2. Open the ICS-1000 front door.

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

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

5. Reconnect all liquid lines to the injection valve (see Figure 5-3

6. Close the door.

7. Turn on the pump.

Figure 5-3. Injection Valve Plumbing

5-10 Doc. 031879-01 3/03

Dionex ICS-1000 Operator's Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1 • Introduction

1.1 Introduction to Ion Chromatography (IC)

1.2 Overview of the ICS-1000

1.3 About This Manual

1.3.1 Safety Messages and Notes

Messages d'avertissement en français

Warnhinweise in Deutsch

Notes

1.3.2 Safety Labels

2.1 Operating Features

2.1.1 Front Panel

2•Features

2.1.2 Top Cover

2.1.3 Component Panel

Eluent Valve

Leak Sensor

Pump Heads

Pressure Transducer

Injection Valve

Separator and Guard Columns

Suppressor

DS6 Heated Conductivity Cell

Tubing Chases

2.1.4 Rear Panel

Analog Output Connector

USB Connections

TTL and Relay Connector

Tubing Clips

Power Switch

Main Power Receptacle

2.2 Flow Schematic

2.3 The Chromeleon Interface

2.3.1 The Chromeleon Main Window and Browser

2.3.2 The ICS-1000 Control Panels

System Control Panels

System Controls Overview

Sample

System

Audit Trail

Pump

Column Heater (Optional)

Detector

2.4 System Component Details

2.4.1 Vacuum Degas Assembly (Optional)

Degas Mode Options

2.4.2 Eluent Valve

2.4.3 Pump

Primary Pump Head

Secondary Pump Head

Pressure Transducer

Pulse Damper

Piston Seal Wash

2.4.4 Injection Valve

2.4.5 Column Heater (Optional)

2.4.6 Suppressor

2.4.7 DS6 Heated Conductivity Cell

Temperature Control

Temperature Compensation

DS6 Heated Conductivity Cell Components

3 • Operation and Maintenance

3.1 Operation Overview

3.2 Power Up the System

3.3 Start Chromeleon

3.4 Set Up the Eluent Reservoir

3.4.1 Prepare the Eluent

3.4.2 Degas the Eluent

Manual Degassing of Eluent

3.4.3 Filter the Eluent

3.4.4 Fill the Reservoir

3.4.5 Set the Eluent Level

3.4.6 Connect the Reservoir

3.5 Check All Connections

3.6 Prime the Pump

3.7 Set System Operating Conditions

3.8 Equilibrate the System and Verify Operational Status