Dionex ICS-1000 Operator's Manual

ICS-1000 ION CHROMATOGRAPHY SYSTEM
OPERATOR’S MANUAL
© 2003 Dionex Corporation
Document No. 031879
Revision 01 March 2003
©2003 by Dionex Corporation All rights reserved worldwide. Printed in the United States of America.
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

Contents

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
Doc. 031879-01 3/03 i
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
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
Doc. 031879-01 3/03 iii
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
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
Doc. 031879-01 3/03 v
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
vi Doc. 031879-01 3/03
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
Doc. 031879-01 3/03 vii
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
viii Doc. 031879-01 3/03

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.
Doc. 031879-01 3/03 1-1
ICS-1000 Ion Chromatography System
n
6
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.
1-2 Doc. 031879-01 3/03
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.
Doc. 031879-01 3/03 1-3
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
1-4 Doc. 031879-01 3/03

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.
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.
1-6 Doc. 031879-01 3/03
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.
Doc. 031879-01 3/03 1-7
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
1-8 Doc. 031879-01 3/03
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
Doc. 031879-01 3/03 2-1
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
2-2 Doc. 031879-01 3/03

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.
Doc. 031879-01 3/03 2-3
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.
11
11
10
8
9
5
7
6
Eluent Valve
1
Leak Sensor
2
Pump Heads
3
Pressure Transducer
4
Injection Valve
5
6
Columns
Connector for
7
optional column heater
4
Suppressor
8
DS6 Conductivity
9
3
Cell
Mounting brackets
10
for a second suppressor
2
Tubing Chase (2)
1
11
Figure 2-4. ICS-1000 Component Panel
2-4 Doc. 031879-01 3/03
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.
Doc. 031879-01 3/03 2-5
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
2-6 Doc. 031879-01 3/03

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.
Doc. 031879-01 3/03 2-7
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.
2-8 Doc. 031879-01 3/03

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)
7
1
ELUENT
OUT
11
IN
COND
OUT
CELL
PULSE
DAMPER
SAMPLE
5
L
S
W
WASTE
C
6
P
L
VALV E
OUT
PUMP PUMP
HEAD
OUT
4
PRESS.
XDUCER
HEAD
WASTE
OUT
12
8
10
SUPPRESSOR
HEAT EXCHANGER
IN
SEPARATOR COLUMN
COLUMN HEATER (optional)
9
GUARD
3
WASTE
IN OUT
ELUENT
VALV E
2
IN
Figure 2-6. ICS-1000 Flow Schematic
Doc. 031879-01 3/03 2-9
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.
s
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.
w
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.
11
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.
12
2-10 Doc. 031879-01 3/03

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
Doc. 031879-01 3/03 2-11
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.
2-12 Doc. 031879-01 3/03
Loading...
+ 180 hidden pages