ICS-900 Ion Chromatography System Operator s Manual

Transcription

1 ICS-900 Ion Chromatography System Operator s Manual Document No Revision 01 March 2008

2 2008 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 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 AMMS,Chromeleon, and CMMS are registered trademarks of Dionex Corporation. MMS, MicroMembrane, and OnGuard are trademarks of Dionex Corporation. Teflon and Tefzel are registered trademarks of E.I. du Pont de Nemours and Company. Microsoft, Windows 2000, and Windows XP are registered trademarks of Microsoft Corporation. PRINTING HISTORY Revision 01, March 2008

3 Contents 1 Introduction 1.1 Overview of the ICS The ICS-900 Operator s Manual Overview Safety Messages and Notes Safety and Regulatory Information Safety Labels Description 2.1 Operating Features Front Door and Top Cover Component Mounting Panel Rear Panel Fluid Schematic System Component Details Pump Pressure Transducer Injection Valve with Sample Loop MMS 300 MicroMembrane Suppressor Displacement Chemical Regeneration (DCR) Conductivity Cell and DS5 Detection Stabilizer Doc /08 i

4 ICS-900 Operator s Manual 2.4 Chromeleon and Chromeleon Xpress Software The Panel Tabset Software Control Modes System Wellness and Predictive Performance Operation and Maintenance 3.1 Operation Overview Turning On the ICS-900 Power Connecting to Chromeleon or Chromeleon Xpress Preparing the Eluent Preparing the Regenerant Priming the Pump Equilibrating the System Verifying Operational Status Configuring Standby Mode Preparing Samples Collecting and Storing Pretreating Diluting Processing Samples Overview Manually Processing Samples Automatically Processing Samples (Batch Processing) Loading and Injecting Samples with an Autosampler ii Doc /08

5 Contents Loading and Injecting Samples with a Syringe Example Chromeleon Commands for Loading and Injecting Samples Maintenance Troubleshooting 4.1 Alarms and Error Conditions Liquid Leaks Pump Difficult to Prime or Loses Prime Pump Does Not Start No Flow Erratic Flow/Pressure Reading Excessive System Backpressure Peak Ghosting Nonreproducible Peak Height or Retention Time Abnormal Retention Time or Selectivity No Detector Response High Detector Output Baseline Noise or Drift Service 5.1 Diagnostics and Calibrations Opening the Wellness Panel Wellness Panel Features Doc /08 iii

6 ICS-900 Operator s Manual Calibrating the Pressure Transducer Calibrating the Cell Calibrating the Flow Rate Replacing Tubing and Fittings Isolating a Restriction in the Liquid Plumbing Cleaning Eluent Bottles Changing the Sample Loop Cleaning and Replacing Pump Check Valves Replacing a Pump Piston Seal and Backup Seal Replacing a Pump Piston Replacing the Waste Valve Seal Rebuilding the Injection Valve Replacing the Conductivity Cell Replacing the Suppressor Changing the Main Power Fuses A Specifications A.1 Electrical A.2 Physical A.3 Environmental A.4 Front Panel A.5 Rear Panel A.6 Pump A.7 Detector iv Doc /08

7 Contents A.8 Conductivity Cell A.9 Injection Valve A.10 Delay Volume B Reordering Information C TTL and Relay Control C.1 Connecting a TTL or Relay C.2 Selecting TTL Input Control Modes and Functions C.3 Configuring Relay Output 1 or 2 to Respond to the Pump Flow C.4 Controlling TTL and Relay Outputs C.5 Controlling an AS40 Automated Sampler with a Relay D FAQ D.1 How do I hook up an AS40 Automated Sampler? D.2 How often should I perform calibrations? D.3 Why are the retention times moving? D.4 How do I adjust retention times? D.5 When should I remake standards? D.6 When should I remake eluents? D.7 How do I start Chromeleon or Chromeleon Xpress? D.8 How do I back up data? D.9 How do I delete data? D.10 How do I shut off the system? Doc /08 v

8 ICS-900 Operator s Manual D.11 How do I store columns? D.12 How do I know when a column is dirty? D.13 How do I clean a column? D.14 Why is the conductivity high? E Introduction to Ion Chromatography (IC) F Glossary vi Doc /08

9 1 Introduction 1.1 Overview of the ICS-900 The Dionex ICS-900 Ion Chromatography System (ICS-900) performs isocratic ion analyses using suppressed conductivity detection. The ICS-900 is an integrated ion chromatography system consisting of a pump, an injection valve, and a conductivity cell. Other system components (guard column, separator column, and suppressor) are ordered separately. The ICS-900 is controlled with a PC running Windows XP or Windows 2000 and the Chromeleon Chromatography Management System (version 6.8 SP4 or later) or Chromeleon Xpress. The Chromeleon Chromatography Management System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of Dionex chromatography instruments, but does not include data management capabilities. For communication between the ICS-900 and the PC on which Chromeleon or Chromeleon Xpress is installed, the ICS-900 must be connected to a USB (Universal Serial Bus) port on the PC or a USB hub. For details, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document No ). The manual is provided on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). NOTE For an introduction to basic ion chromatography concepts, see Appendix E. Doc /08 1

10 ICS-900 Operator s Manual 1.2 The ICS-900 Operator s Manual Overview The electronic version (i.e., PDF file) of the ICS-900 operator s manual contains numerous hypertext links that can take you to other locations within the file. These links include: Table of contents entries Index entries Cross-references (underlined in blue) to sections, figures, tables, etc. If you are not familiar with how to navigate PDF files, refer to the Help system for Adobe Acrobat or Adobe Reader for assistance. Chapter 1 Introduction Chapter 2 Description Chapter 3 Operation and Maintenance Chapter 4 Troubleshooting Chapter 5 Service Appendix A Specifications Appendix B Reordering Information Introduces the ICS-900; explains the conventions used in this manual, including safety-related information. Describes ICS-900 operating features, the chromatographic flow path, and the software required for ICS-900 control. Provides operating instructions for the ICS-900 and describes routine preventive maintenance procedures. Lists problems and presents step-by-step procedures for how to isolate and eliminate the cause of each problem. Provides step-by-step instructions for routine service and parts replacement procedures that the user can perform. Provides specifications and installation site requirements for the ICS-900. Lists spare parts for the ICS Doc /08

11 1 Introduction Appendix C TTL and Relay Control Appendix D FAQ Appendix E Introduction to Ion Chromatography Appendix F Glossary Describes the ICS-900 TTL and relay control features. Provides answers to frequently asked questions about ICS-900 operation. Describes basic ion chromatography concepts. Provides definitions of terms commonly used in ion chromatography Safety Messages and Notes This manual contains warnings and precautionary statements that can prevent personal injury and/or damage to the ICS-900 when properly followed. Safety messages appear in bold type and are accompanied by icons, as shown below. Indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury. Indicates a potentially hazardous situation which, if not avoided, could result in death or serious injury. 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. Doc /08 3

12 ICS-900 Operator s Manual Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures graves à mortelles. Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures mineures à modérées. Également utilisé pour signaler une situation ou une pratique qui pourrait gravement endommager l'instrument mais qui n'entraînera pas de blessures. Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen. Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen. Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn eine Situation zu schweren Schäden am Gerät führen kann, jedoch keine Verletzungsgefahr besteht. 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. 4 Doc /08

13 1 Introduction 1.3 Safety and Regulatory Information The ICS-900 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of an ICS-900 in a manner not specified by Dionex may result in personal injury. If you have a question regarding appropriate usage, contact Dionex before proceeding. In the U.S., call and select the Technical Support option. Outside the U.S., call the nearest Dionex office Safety Labels The TUV GS, C, US Mark safety, and CE Mark label on the ICS-900 indicates that it is in compliance with the following standards: EMC Susceptibility and Immunity EN including A1:1998 and A2:2001 Safety EN :2001 UL :2004 CAN/CSA-C :2004 These symbols appear on the ICS-900 or on labels affixed to the ICS-900: Alternating current Protective conductor terminal Power supply is on Power supply is off Indicates a potential hazard. Refer to this operator s manual for an explanation of the hazard and how to proceed. Doc /08 5

14 ICS-900 Operator s Manual 6 Doc /08

15 2 Description 2.1 Operating Features Front Door and Top Cover Figure 2-1 illustrates the front door and top cover of the ICS-900 Ion Chromatography System (ICS-900). Eluent Bottle Regenerant Bottle Status LEDs Injection Port Figure 2-1. ICS-900 Ion Chromatography System Doc /08 7

16 ICS-900 Operator s Manual LEDs Three status LEDs (described below) are on the ICS-900 front door. LED Label If On (Green) If Flashing Power ICS-900 power is on Does not flash Ready System check passed, but sequence not yet started (LED stays on until run starts or sequence is aborted) System check failed (occurs if system check executes for 10 minutes without success) Run Running/acquiring data Error/alarm/fault (including injection valve position) Other status information and alarm messages are displayed in the Audit Trail in Chromeleon or Chromeleon Xpress. For a description of these messages, see Section 4.1 Injection Port The injection port can be connected to the injection valve inside the ICS-900. The sample to be analyzed is injected into the injection port using a syringe. For automated sample injections, the ICS-900 injection valve can be connected to an autosampler, instead of to the injection port. For more information about sample injection, see Section Eluent and Regenerant Bottles The ICS-900 top cover is molded to hold one eluent bottle assembly (P/N ) and one regenerant bottle assembly (anion, P/N ; cation, P/N ). Eluent carries the sample through the ICS-900 and facilitates the ion separation process. The type of eluent used depends on the analyses 8 Doc /08

17 2 Description performed. For example, an ICS-900 configured for anion analyses uses carbonate eluent, while an ICS-900 configured for cation analyses uses methanesulfonic acid (MSA) eluent. Regenerant renews the suppressor s ability to suppress eluent conductivity. An ICS-900 configured for anion analyses uses dilute sulfuric acid regenerant. An ICS-900 configured for cation analyses uses tetrabutylammonium hydroxide (TBAOH) regenerant. For more information about suppressor regeneration, see Section Component Mounting Panel Figure 2-2 shows the components installed on the component panel behind the ICS-900 front door Conductivity Cell (Housed in DS5 Detection Stabilizer MMS 300 Suppressor Separator Column 4 Pump Heads Pressure Transducer Injection Valve 7 Tubing Chase Guard Column 9 Backpressure Tubing Figure 2-2. ICS-900 Component Mounting Panel Doc /08 9

18 ICS-900 Operator s Manual Conductivity Cell The flow-through heated conductivity cell measures the electrical conductance of analyte ions as they pass through the cell. A heat exchanger inside the cell regulates the temperature to 40 C (104 F). The cell is housed inside a DS5 Detection Stabilizer (P/N ). For details about the conductivity cell and DS5 Detection Stabilizer, see Section MMS 300 MicroMembrane Suppressor The MMS 300 suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. For details about the MMS 300 suppressor, see Section Separator and Guard Columns Both the separator and guard columns are packed with resin and perform the separation of the sample ions. The main function of the guard column is to trap contaminants and remove particulates that might damage the separator column. Pressure Transducer The pressure transducer measures the system backpressure. See Section for details about the pressure transducer. Pump Heads The ICS-900 includes a dual-piston serial pump. The flow rate can be set from 0.01 ml/min to 5.00 ml/min. However, for optimum performance, set the flow rate to between 0.20 and 3.00 ml/min. Setting the flow rate to 0.00 ml/min turns off the pump. For details about the pump, see Section Injection Valve The injection valve is a six-port, electrically-activated valve. For details about the injection valve, see Section Doc /08

19 2 Description Tubing Chase The tubing chase routes tubing from the component panel, through the ICS-900 interior, to the rear panel Rear Panel Figure 2-3 illustrates the ICS-900 rear panel. 1 USB Connector Link LED TTL and Relay Connector Fuse Holder, Power Switch, and Power Receptacle Plumbing and Waste Lines 5 Figure 2-3. ICS-900 Rear Panel USB Connector The USB connector connects the ICS-900 to the PC on which Chromeleon or Chromeleon Xpress is installed. For the standard system configuration of one ICS-900 connected to a PC, connect a USB cable between the USB connector on the ICS-900 and a USB port on the PC. For detailed connection instructions, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document Doc /08 11

20 ICS-900 Operator s Manual No ), provided on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). Link LED The Link LED indicates the communication status between the ICS-900 and the PC on which Chromeleon or Chromeleon Xpress is installed. Link LED Status On Flashing Off Description The ICS-900 and the PC are linked, but no data is currently being transmitted or received The ICS-900 and the PC are linked and data is being transmitted The ICS-900 and the PC are not currently linked TTL and Relay Connector The TTL and Relay connector strip provides two TTL outputs, two relay outputs, and four TTL inputs. The outputs can be used to control functions in other TTL- or relay-controllable devices. The inputs can be used to switch the injection valve position, turn the pump on and off, and perform an autozero command. For connection instructions, see Appendix C. Fuse Holder, Power Switch, and Power Receptacle The fuse holder contains two fast-blow IEC 127 fuses rated 3.15 A (P/N ). For instructions on how to change the fuses, see Section The power switch provides on/off control of power to the ICS-900. The power cord plugs into the IEC 320 three-prong receptacle. The power supply cord is used as the main disconnect device. Make sure the socket-outlet is located near the ICS-900 and is easily accessible. Le cordon d'alimentation principal est utilisé comme dispositif principal de débranchement. Veillez à ce que la prise de base soit située/installée près du module et facilement accessible. 12 Doc /08

21 2 Description Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen Sie sicher, daß sich die Steckdose nahe am Gerät befindet und leicht zugänglich ist. Plumbing and Waste Lines The following lines exit the ICS-900 through the tubing chase on the lower left corner of the rear panel. Eluent Regenerant Cell outlet Waste (sample, regenerant, and pump priming) Doc /08 13

22 ICS-900 Operator s Manual 2.2 Fluid Schematic Figure 2-4 shows the flow path through the ICS-900. To pump inlet From cell outlet Backpressure Coil (1 or 2, depending on flow rate) 8 Conductivity Cell (in DS5 Detection Stabilizer) Eluent 1 Regenerant 9 6 Regen Out Eluent Out MMS 300 Eluent In Secondary Pump Heads 7 Primary Regen In Pulse Damper 4 2 Pressure Transducer 3 C P To cell inlet To MMS Regen In 5 L L S Injection Valve W Eluent in from pulse damper Sample in To Waste To Waste Figure 2-4. ICS-900 Flow Schematic 14 Doc /08

23 2 Description Liquid flows through the ICS-900 along the following flow path. Refer to Figure 2-4 for the flow path number locations. Eluent from the eluent bottle 1 is drawn into the pump 2. The pump pushes the eluent through the pressure transducer 3, which measures the system pressure, and through a pulse damper 4, which smooths minor pressure variations from the pump to minimize baseline noise. The eluent then flows into the injection valve 5. After sample is loaded into the sample loop and the injection valve is toggled to the Inject position, eluent passes through the sample loop pushing the sample into the eluent stream. The eluent/sample mixture is pumped through the guard and separator columns 6, where the ions are separated by the ion exchange process. The eluent/sample mixture then flows through the suppressor 7, which suppresses the conductivity of the eluent and enhances the conductivity of the analyte. Regenerant flows continuously through the suppressor, restoring the ion exchange sites to their original state. The eluent/sample mixture then flows through the conductivity cell 8, where the analytes are detected. A signal is produced and sent to Chromeleon or Chromeleon Xpress software. Finally, the eluent flows out of the cell and into the regenerant bottle 9, where it pressurizes the regenerant and forces it into the suppressor. Doc /08 15

24 ICS-900 Operator s Manual 2.3 System Component Details Pump The ICS-900 pump is a microprocessor-based isocratic eluent delivery system. Its variable speed, dual-piston series design ensures pulse-free pumping for the most demanding applications. Primary Pump Head The primary pump head pumps eluent into the secondary head (see Figure 2-5). The check valves, which prevent reverse flow through the pump, are located on the bottom (inlet) and top (outlet) of the primary pump head. Secondary Pump Head Outlet Check Valve Primary Pump Head Waste Valve Inlet Check Valve Figure 2-5. ICS-900 Pump Components Secondary Pump Head The secondary pump head delivers eluent to the pressure transducer. The waste valve is located on the front of the secondary pump head (see Figure 2-5). To open the waste valve, turn the knob one-half turn counterclockwise. When the waste valve is in the open position, all output is directed to waste. 16 Doc /08

25 2 Description Pressure Transducer The pressure transducer measures the system pressure at the point that the eluent flows from the pump head outlet check valve. Pressure readings indicate that the pumping system is delivering smooth, accurate flow. Pressure readings can be monitored from Chromeleon or Chromeleon Xpress. The system pressure should remain consistent (no more than a 3% difference from one pressure reading to the next). High and low pressure limits can be used to stop the pump flow if a limit is exceeded. The pressure limits can be set from Chromeleon (in the Server Configuration Properties dialog box or in the Chromeleon or Chromeleon Xpress program). For troubleshooting information if a pressure limit is exceeded, see Section 4.7. Pulse Damper Flow output from the pressure transducer continues to the pulse damper, which smooths minor pressure variations. From there, flow is directed to the injection valve and then to the remainder of the chromatography system. Doc /08 17

26 ICS-900 Operator s Manual Injection Valve with Sample Loop The injection valve is a six-port, electrically-activated Rheodyne valve. A 10 μl sample loop (P/N ) is installed on the valve at the factory. The valve has two operating positions: Load and Inject. Eluent flows through either the Load or Inject path, depending on the valve position. Figure 2-6 shows flow schematics for the valve. LOAD POSITION INJECT POSITION From Pump From Pump Sample Loop L P L W C S To Column Sample In To Waste To Column Sample In To Waste = Sample = Eluent Figure 2-6. Injection Valve Flow Schematics In the Load position, sample is loaded into the sample loop, where it is held until injection. Eluent flows from the pump, through the valve, and to the column, bypassing the sample loop. Sample flows from the syringe or autosampler line (if installed), through the valve, and into the sample loop. Excess sample flows out to waste. In the Inject position, sample is swept to the column for analysis. Eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it. Section describes how to inject samples manually; Section describes how to inject samples with an autosampler. 18 Doc /08

27 2 Description MMS 300 MicroMembrane Suppressor The MMS 300 suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. As illustrated in Figure 2-7, a constant flow of regenerant over the membrane continually restores the suppression ability of the MMS 300. A process called Displacement Chemical Regeneration (DCR) pushes regenerant from the regenerant bottle through the suppressor. See Section for details. For more information about the MMS 300, refer to the suppressor manual. Suppressor manuals are included on the Dionex Reference Library CD- ROM (P/N ). ELUENT IN 4-mm REGEN OUT REGEN IN Regenerant Screen Ion Exchange Membrane Eluent Screen Ion Exchange Membrane Regenerant Screen ELUENT OUT Figure 2-7. MMS 300 Suppressor Flow Doc /08 19

28 ICS-900 Operator s Manual Displacement Chemical Regeneration (DCR) Displacement Chemical Regeneration (DCR) is the process that restores the ability of the MMS 300 suppressor to suppress eluent. In DCR, the eluent that exits the cell is pumped into the regenerant bottle. The eluent pressurizes the bottle and pushes the regenerant into the suppressor. However, because the eluent is a different density than the regenerant, it remains separate. In the anion DCR process (see Figure 2-8), the eluent is less dense than the regenerant and it remains on the top of the bottle, forcing the regenerant into the regenerant line at the bottom of the bottle and out into the suppressor. In the cation DCR process (see Figure 2-9), the eluent is denser than the regenerant and it flows to the bottom of the bottle. This displaces the regenerant, pushing regenerant out of the regenerant line at the top of the bottle and out into the suppressor. Regen In Used eluent out to regenerant reservoir Regen Bottle Out Used Eluent Conductivity Cell (in DS5 Detection Stabilizer) Regen Out Eluent Out AMMS 300 Eluent In Regen In Eluent out to cell Regenerant in from reservoir Anion Regenerant Eluent in from column Regenerant out to waste Figure 2-8. Anion ICS-900 Displacement Chemical Regeneration (DCR) 20 Doc /08

29 2 Description Regen In Used eluent out to regenerant reservoir Regen Bottle Out Cation Regenerant Conductivity Cell (in DS5 Detection Stabilizer) Regen Out Eluent Out CMMS 300 Eluent In Regen In Eluent out to cell Regenerant in from reservoir Used Eluent Eluent in from column Regenerant out to waste Figure 2-9. Cation ICS-900 Displacement Chemical Regeneration (DCR) Connections to the regenerant bottle differ depending on whether the system will run an anion or a cation application. Regenerant bottles for each type of application are available (anion regenerant bottle assembly, P/N ; cation regenerant bottle assembly, P/N ). For detailed installation instructions, refer to the DCR Kit Installation Instructions (Document No ), provided on the Dionex Reference Library CD- ROM (P/N ) Conductivity Cell and DS5 Detection Stabilizer The flow-through heated conductivity cell contains two 316 stainless steel electrodes that are permanently sealed into the PEEK cell body. The cell measures the electrical conductance of analyte ions as they pass through the cell. Temperature directly affects the conductivity of a solution. For example, laboratory heating and air conditioning systems can cause a regular slow cycling in the baseline. This, in turn, can affect the reproducibility of an analysis. The higher the conductivity, the more pronounced the effect. Doc /08 21

30 ICS-900 Operator s Manual In ion analysis, the effect of temperature variation is minimized by suppressing eluent conductivity. Built-in preset temperature compensation also ensures that there is no major change in the baseline or in peak heights. Temperature compensation further improves baseline stability. Direct conductive heating is used in the ICS-900 conductivity cell to provide temperature control and compensation. A heat exchanger inside the ICS-900 cell regulates the temperature. All data is collected at 40 C (104 F). The cell is housed inside a DS5 Detection Stabilizer (P/N ) (see Figure 2-10), which helps to insulate the cell from fluctuations in ambient temperature. DS5 Detection Stabilizer Cell Inlet Cell Outlet Conductivity Cell From suppressor ELUENT OUT port To regenerant reservoir Connector to component mounting panel Figure Conductivity Cell and DS5 Detection Stabilizer The conductivity cell has two detection limit ranges: 0 to 500 μs or 0 to 10,000 μs. Select the range depending on the expected detector readings for the application. The default range of 0 to 500 μs is appropriate for most applications. The detection limit range is set in the Properties dialog box of the Chromeleon Server Configuration program. For details, refer to the ICS-900 Ion Chromatography System Installation Instructions (Document No ), provided on the Dionex Reference Library CD- ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). 22 Doc /08

31 2 Description 2.4 Chromeleon and Chromeleon Xpress Software The ICS-900 is controlled by a PC configured with Chromeleon Chromatography Management System or Chromeleon Xpress. Chromeleon Chromatography Management System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of Dionex chromatography instruments, but does not include data management capabilities The Panel Tabset The Chromeleon and Chromeleon Xpress panel tabset provides a centralized location for controlling system functions. A panel tabset for an ICS-900 system typically includes the following Control panels: An ICS-900 Control panel (see Figure 2-11) provides access to ICS-900 functions. The label on the tab for this panel is the name of the timebase in which the ICS-900 is configured. Figure ICS-900 Control Panel on the Panel Tabset Doc /08 23

32 ICS-900 Operator s Manual A Sequence Control panel lets you define and run sequences (groups of sample injections to be analyzed in the order in which they are listed). A Status panel shows the overall system status. An Autosampler panel (included only if the ICS-900 is connected to an AS Autosampler) provides access to AS functions. To open the panel tabset, use one of the methods below: If Chromeleon is installed, start Chromeleon and click the Default Panel Tabset toolbar button, or select View>Default Panel Tabset. If Chromeleon Xpress is installed, start the application; this automatically displays the ICS-900 panel tabset Software Control Modes Two modes of software control are available: direct control and programmed control. With direct control, you select operating parameters and commands from the Control panels. Direct control commands are executed as soon as they are entered. See Section for details about direct control. With programmed control, you create a list of control commands to be executed in chronological order. Programs can be created automatically (with the help of a software wizard). See Section for details about programmed control. 24 Doc /08

33 2 Description System Wellness and Predictive Performance System Wellness monitors the overall health of a chromatographic system. It provides built-in diagnostic and calibration features that help prevent unscheduled system shutdowns and assure reliable operation of system devices. For details about System Wellness, see Section 5.1. Predictive Performance provides functions for monitoring the usage of replaceable parts and for planning service procedures. Predictive Performance lets you monitor the following functions: The number of hours the ICS-900 has been in use The number of times the injection valve has cycled The number strokes performed by the pump pistons The estimate of the amount of wear to the piston seal The volume of eluent pumped through the suppressor and column You can set limits for injection valve cycles, piston strokes, piston seal wear, suppressor usage, and column usage. Two limits can be set for each parameter. When the first limit is reached, a warning message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail. When the second limit is reached, an error message is displayed in the Audit Trail. After replacing a part, reset the limit counters to zero. Different applications cause different rates of wear on the consumable parts in your instrument. Experience will help you determine the appropriate limits to set to predict when the next maintenance will be required. Predictive Performance commands and parameters are available in the Commands dialog box in Chromeleon or Chromeleon Xpress. To open the Commands dialog box, press F8. Expand the list of commands under Pump_ECD and scroll to the Predictive Performance commands Doc /08 25

34 ICS-900 Operator s Manual (InjectValveCycles, PumpPistonStrokes, SealWear, SuppressorVolume, ColumnVolume) (see Figure 2-12). Figure Predictive Performance Commands: InjectValveCycles If you do not wish to receive these warning or error messages, you can disable them by setting the Warning and Limit parameter for each Predictive Performance function to Off. 26 Doc /08

35 3 Operation and Maintenance This chapter describes routine operating and maintenance procedures for the ICS- 900 Ion Chromatography System (ICS-900). 3.1 Operation Overview Figure 3-1 illustrates the basic steps for routine operation of the ICS-900. Turn on the ICS-900 power Connect to Chromeleon Prepare the eluent and regenerant Prime the pump Equilibrate the system Prepare samples Process samples Figure 3-1. ICS-900 Operation Flow Chart Doc /08 27

36 ICS-900 Operator s Manual 3.2 Turning On the ICS-900 Power Press the power switch on the ICS-900 rear panel (see Figure 2-3) to turn on the system power. These are the conditions at power-up: The pump is off. The injection valve is in the Load position. The conductivity detector begins reading the current conductivity. 3.3 Connecting to Chromeleon or Chromeleon Xpress 1. Turn on the PC. 2. Start the Chromeleon Server, if it is not already running. a. Check the Chromeleon Server Monitor icon on the Windows taskbar. When the server is running, the icon is gray. When the Server is not running, the icon is crossed out in red. To start the server, right-click the icon and select Start Server. b. If the Server Monitor icon is not on the Windows taskbar, click Start and select All Programs (or Programs) > Chromeleon > Server Monitor. The Server Monitor opens. Click Start to start the server. 3. To start the Chromeleon client, click Start and select All Programs (or Programs) > Chromeleon > Chromeleon. 4. If Chromeleon is installed, display the panel tabset by selecting View > Default Panel Tabset or by clicking the Default Panel Tabset toolbar button. If Chromeleon Xpress is installed, starting the application automatically displays the panel tabset. 5. To display the ICS-900 Control panel, select the tab labeled with the ICS-900 timebase name (see Figure 3-2). 28 Doc /08

37 3 Operation and Maintenance Figure 3-2. ICS-900 Control Panel on Panel Tabset 3.4 Preparing the Eluent 1. Prepare the eluent. For instructions refer to the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N ). 2. Fill the eluent bottle with the prepared eluent, insert the stopper assembly tubing into the bottle, and hand tighten the cap. Set the Eluent Level After filling the bottle, move the Eluent Remaining slider on the ICS-900 Control panel (see Figure 3-3) to indicate the volume of liquid in the bottle. The ICS-900 determines the eluent usage by monitoring the flow rate and the length of time the pump is on. As the eluent is used up, the ICS-900 updates the Eluent Remaining slider and gauge. A warning appears in the Audit Trail when the level falls below 200 ml, and then again when the level falls bellow 100 ml. Doc /08 29

38 ICS-900 Operator s Manual For the eluent level to be accurate, you must enter the level each time the bottle is filled. After filling the eluent bottle, move the slider to indicate the volume of liquid in the bottle Note: The Eluent Remaining slider and gauge are updated as the liquid is used up. Figure 3-3. Setting the Eluent Level 3.5 Preparing the Regenerant The type of regenerant used with the ICS-900 depends on the type of analysis to be run. A dilute sulfuric acid regenerant is used for anion analyses; a tetrabutylammonium hydroxide (TBAOH) regenerant is used for cation analyses. Follow the instructions below to prepare either anion or cation regenerant. Use ASTM Type I (18 megohm-cm) filtered and deionized water to prepare the regenerant. 1. Verify that you have the correct regenerant bottle assembly (P/N for anion analyses; P/N for cation analyses): For anions, verify that the cap is labeled ANION and the REGEN BOTTLE OUT line extends to the bottom of the bottle. For cations, verify that the cap is labeled CATION and the REGEN BOTTLE OUT line extends only about 1 cm (0.4 in) into the bottle. 2. Rinse the regenerant bottle with deionized water. 3. Fill the bottle about halfway with deionized water. 30 Doc /08

39 3 Operation and Maintenance 4. Determine the regenerant concentration required for the application. To estimate the regenerant concentration required for an eluent strength, use the following formulas: Anion Regenerant Concentration = (mm eluent) x 2 Cation Regenerant Concentration = (mm eluent) x 5 For example, if you are using 20 mm methanesulfonic acid (MSA) as the eluent for cation analysis, use a regenerant concentration of 100 mm tetrabutylammonium hydroxide (TBAOH). For additional details, refer to the Displacement Chemical Regeneration (DCR) kit installation instructions and the suppressor manual. 5. Empty the required amount of concentrate (sulfuric acid for anions; TBAOH for cations) into the bottle. For acid concentrates (such as the anion regenerant), always pour the concentrate into deionized water, not into the empty bottle. Pour les concentrés acides (comme le régénérant anionique), versez toujours le concentré dans de l'eau désionisée et non dans le réservoir vide. Gießen Sie säurehaltige Konzentrate (beispielsweise den Anionregenerenten) das Konzentrat immer in entionisiertes Wasser und nicht in den leeren Behälter. 6. Fill the bottle almost to the top with deionized water and then place the bottle in the tray on the top of the ICS-900. NOTE To avoid staining the ICS-900, be careful not to spill TBAOH on the instrument. 7. Using the concentrate bottle, pour additional deionized water into the bottle until it is completely filled to the top. If a few drops spill over, then it is full enough. The regenerant bottle must be filled all the way to the top at all times. 8. Insert the stopper assembly tubing into the bottle and hand-tighten the cap. 9. Invert the bottle three or four times to disperse the concentrate. Doc /08 31

40 ICS-900 Operator s Manual After the analysis begins, do not mix the contents of the regenerant bottle. 10.Verify that the liquid lines from the ELUENT and REGEN bottles are connected to the corresponding lines from the ICS-900 (see Figure 3-4). ELUENT Bottle Out REGEN Bottle In REGEN Bottle Out Figure 3-4. Eluent and Regenerant Bottle Liquid Line Connections 3.6 Priming the Pump Prime the pump if the eluent has been changed, the eluent line contains air, or the pump heads are dry (for example, after servicing). NOTE If the eluent line is empty or the pump heads are completely dry, you can use a 10 cc syringe (P/N ) to prime the pump (see page 34). 1. Verify that the ELUENT and REGEN bottles are filled, the bottle caps are installed and hand-tightened, and the liquid lines are connected to the bottles. 2. Verify that the waste lines are directed to a waste container. 32 Doc /08

41 3 Operation and Maintenance 3. Open the waste valve on the secondary (left) pump head by turning the knob one-half turn counterclockwise (see Figure 3-5). Opening the valve directs the eluent flow path to waste and eliminates backpressure. Secondary Pump Head Waste Valve (Open) Figure 3-5. Priming the Pump 4. Click Prime on the ICS-900 Control panel (see Figure 3-2), or open the Commands dialog box (press F8), select the Pump command, and select the Prime option. The pump will begin pumping at approximately 3 ml/min. 5. Continue priming the ICS-900 until no air bubbles are exiting the pump waste line. 6. Click Pump Off. 7. Close the waste valve. Do not overtighten. The pump is now ready for operation. NOTE A convenient way to verify that the waste valve is closed is to select the pump flow rate required for your application, turn on the pump, and then close the valve. The pressure should rise to the value expected for the application and quickly stabilize. Doc /08 33

42 ICS-900 Operator s Manual Priming the Eluent Line with a Syringe (Optional) A syringe can be used to facilitate priming when the eluent line is empty or the pump heads are completely dry. 1. Verify that the pump is turned off. 2. Disconnect the waste line from the luer fitting on the secondary (left) pump head and connect a 10 ml syringe (P/N ) to the luer fitting (see Figure 3-6). Secondary Pump Head Waste Valve (Open) Luer Fitting 10 ml Syringe (P/N ) Figure 3-6. Priming the Eluent Lines 3. Open the waste valve by turning it one-half turn counterclockwise. 4. Draw the syringe back to begin removing air from the flow path. NOTE When the line already contains liquid, the syringe will be difficult to draw back. In this case, prime with the prime command only (see Section 3.6). 5. When a small amount of liquid enters the syringe, remove the syringe from the luer fitting, and reconnect the waste line to the luer fitting. 6. Follow the instructions in Section 3.6 to finish priming. 34 Doc /08

43 3 Operation and Maintenance 3.7 Equilibrating the System 1. Turn on the pump and run at the flow rate recommended for the column. 2. Allow the system to equilibrate. The ICS-900 Control panel displays the background conductivity (the conductivity of the eluent without the offset performed by the autozero command). 3. Offset the background and zero the conductivity reading by clicking the Autozero button on the ICS-900 Control panel. 4. Monitor the system pressure to make sure it is at the expected pressure for the installed column (refer to the column manual for details) and is stable. Column manuals typically provide pressure specifications for systems that do not include a guard column. Expect the ICS-900 system pressure (with a guard column) to be 15% to 20% higher than the specification in the column manual. If the pressure is less than expected, air may be trapped in the system. Release the air by temporarily removing the pump fitting (P) on the injection valve. Allow the air to escape, and then reconnect the fitting. If the pressure is too high, there may be a restriction in the system plumbing. Refer to the Section 4.7 for troubleshooting information. 5. Check for leaks in the regenerant bottle. 6. Check that liquid is flowing out of the suppressor REGEN OUT waste line. 7. Monitor the baseline conductivity. In general, it should be <30 μs for a system set up for anion analyses, and <2 μs for a system set up for cation analyses. Equilibration time varies and it can take some time to reach these expected values. If the conductivity is too high, see Section 4.12 for troubleshooting information. If the baseline is drifting or has excessive noise (large fluctuations in readings), see Section Verifying Operational Status After the system has equilibrated, verify the actual pump pressure and stability by monitoring the pump pressure. Record the short-term pressure fluctuations; they should be less than 0.13 MPa (20 psi). If the pressure fluctuates by more than this amount, prime the pump (see Section 3.6). Doc /08 35

44 ICS-900 Operator s Manual 3.9 Configuring Standby Mode You can configure the ICS-900 to enter standby mode after a period of inactivity (a period of time in which no data collection and no input from Chromeleon or Chromeleon Xpress has occurred). In standby mode, the pump flow rate is reduced. To configure standby mode: 1. Start the Chromeleon Server Configuration program (click Start on the Windows taskbar and select All Programs (or Programs) > Chromeleon > Server Configuration). 2. Right-click the ICS-900 device in the timebase and select Properties. 3. Click Options (see Figure 3-7). Figure 3-7. ICS-900 Properties Dialog Box: Options Tab Page 4. Enter the desired Standby Flow Rate and select the Inactivity Time Out Period. If you select (0, Off), the ICS-900 does not enter standby mode when it is idle. To cancel standby mode and return the pump to the normal flow rate, either turn on the pump from the ICS-900 Control panel or start a new sequence. 36 Doc /08

45 3 Operation and Maintenance 3.10 Preparing Samples NOTE Sample preparation can be performed while the system is equilibrating Collecting and Storing Collect samples in high density polyethylene containers that have been thoroughly cleaned with ASTM Type I (18 megohm-cm) filtered and deionized water. Do not clean containers with strong acids or detergents because these will leave traces of ions on the container walls. The ions may interfere with the analysis. If samples will not be analyzed on the day they are collected, filter them through clean 0.45 μm filters immediately after collection; otherwise, bacteria in the samples may cause the ionic concentrations to change over time. Refrigerating the samples at 4 C (39 F) will reduce, but not 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 Pretreating Analyze rainwater, drinking water, and air particulate leach solutions directly with no sample preparation (other than filtering and possibly diluting). Filter groundwater and wastewater samples through 0.45 μm filters before injection, unless samples were filtered after collection. A Dionex High Pressure Inline Filter (P/N ) is available for removing particulates down to 0.45 micron from samples. Connect the inline filter between the autosampler outlet and the sample inlet port on the injection valve. For details, see the printed installation instructions provided with the inline filter. Before injection, pretreat samples that may contain high concentrations of interfering substances by putting them through Dionex OnGuard Doc /08 37

46 ICS-900 Operator s Manual cartridges. For instructions, refer to Installation and Troubleshooting Guide for OnGuard Cartridges (Document No ). The manual is included on the Dionex Reference Library CD-ROM (P/N ) Diluting Because the concentrations of ionic species in different samples can vary widely from sample to sample, no single dilution factor can be recommended for all samples of one type. In some cases (for example, many water samples), concentrations are so low that dilution is not necessary. Use eluent or ASTM Type I (18 megohm-cm) filtered and deionized water to dilute the sample. When using carbonate eluents, diluting with eluent minimizes the effect of the water dip at the beginning of the chromatogram. If you dilute the sample with eluent, also use eluent from the same lot to prepare the calibration standards. This is most important for fluoride and chloride, which elute near the water dip. To improve the accuracy of early eluting peak determinations, such as fluoride, at concentrations below 50 ppb, dilute standards in eluent or spike the samples with concentrated eluent to minimize the water dip. For example, spike a 100 ml sample with 1.0 ml of a 100 X eluent concentrate. 38 Doc /08

47 3 Operation and Maintenance 3.11 Processing Samples Overview Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-8 shows the typical steps for manual and batch sample processing. Manual Sample Processing Load the sample Batch Sample Processing Create a program* Autozero Create a sequence Start data acquisition Load the sequence Inject the sample Start the batch Monitor chromatogram Stop data acquisition *Includes commands for sample loading, autozero, injection, and data acquisition. Figure 3-8. Sample Processing Overview Doc /08 39

48 ICS-900 Operator s Manual Manually Processing Samples To manually process a sample, select operating parameters and commands from the Chromeleon or Chromeleon Xpress panel tabset. Commands are executed as soon as they are entered. Summary of Manual Sample Processing 1. Complete the instructions in Section 3.2 through Section 3.10 to prepare the ICS-900 for operation and to prepare the sample for processing. 2. Load the sample into the injection valve sample loop with an autosampler (see Section ) or a syringe (see Section ). 3. On the ICS-900 Control panel, click the Autozero button. 4. On the Sequence Control panel, click the Acq On button (or click the Acquisition On/Off button on the Chromeleon toolbar). 5. Switch the injection valve to the Inject position. The method used to switch the injection valve depends on whether you are using an autosampler (see Section ) or a syringe (see Section ). 6. The signal plot is displayed on the ICS-900 Control panel (see Figure 3-9). Monitor the chromatogram and when sample data has been collected, click the Acq Off button on the Sequence Control 40 Doc /08

49 3 Operation and Maintenance panel (or click the Acquisition On/Off button on the Chromeleon toolbar). Figure 3-9. Manual Data Acquisition Saving Manual Data NOTE Chromeleon Xpress does not allow data to be saved. If you are using Chromeleon, data from manual processing is saved in the manual sequence under the timebase folder in the local datasource. To save the data from a manual run: 1. Select the manual folder and select File>Save As. 2. Enter a new name for the sequence. 3. Select the Save raw data check box. Doc /08 41

50 ICS-900 Operator s Manual 4. Click Save Automatically Processing Samples (Batch Processing) You can use Chromeleon or Chromeleon Xpress to create a list of samples (a sequence) to be processed automatically. For each sample, the sequence includes the following: A program with commands and parameters for controlling the ICS-900 and autosampler (if installed), and for acquiring sample data. A quantification method for peak identification and area determination. The quantification method is not included with Chromeleon Xpress. Additional sample processing parameters (sample name, sample type, injection volume, etc.). After creating the sequence, you can start batch processing. Summary of Automatic Sample Processing 1. Complete the instructions in Section 3.2 through Section 3.10 to prepare the ICS-900 for operation and to prepare the samples for processing. 2. If an autosampler is installed, prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions. Autosampler manuals are provided on the Dionex Reference Library CD-ROM (P/N ). 3. If an autosampler is not installed, load the sample into the injection valve sample loop through the sample port on the ICS-900 front door (see Section ). 4. Use the Application Wizard to specify a program and quantitation method, and create a sequence: a. On the Sequence Control panel, click Application Wizard. 42 Doc /08

51 3 Operation and Maintenance b. Select an application template from the list (see Figure 3-10). Figure Application Wizard c. Click Next> and select the in a new sequence via Sequence Wizard option. d. Click Next> to go to the Sequence Wizard. e. Complete the steps in the Sequence Wizard, adding the desired number of samples and standards to the list. For help, click the Help button on the Sequence Wizard page. After you click Finish, a sequence is created and a program appropriate for the selected application is copied to the sequence. If you are using Chromeleon, a quantification method is also copied to the sequence. 5. Load the sequence and start batch processing: a. On the Sequence Control panel, click Load Sequence. b. Select the sequence created in Step 4 and click Open. c. Click Start Batch. Doc /08 43

52 ICS-900 Operator s Manual Loading and Injecting Samples with an Autosampler 1. Verify that the autosampler output line is connected to port S (5) on the injection valve. Direct the injection valve waste line as required for the installed autosampler model. For details about connecting an autosampler, refer to the ICS-900 Installation Instructions (Document No ). The manual is included on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). 2. Prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions. Autosampler manuals are provided on the Dionex Reference Library CD-ROM (P/N ). 3. Use one of the following methods to load sample into the injection valve sample loop and inject it onto the column: Automatically: Include the Load and Inject commands in a Chromeleon or Chromeleon Xpress program. See the examples in Section See Section for details about automatically processing samples. Manually with an AS40: Start the AS40 load cycle (either manually or with a relay). When the AS40 load cycle is complete, click the Inject button on the ICS-900 Control panel (see Figure 3-11). See Section for details about manually processing samples. Figure ICS-900 Control Panel Load and Inject Buttons Manually with an AS: Click the Inject icon on the Chromeleon tool bar or select Control>Inject. On the Inject dialog box, enter the Position and Volume and click OK. 44 Doc /08

53 3 Operation and Maintenance Autosampler Setup Notes Follow the steps below to verify that the ICS-900 injection valve is controlled by the correct device. 1. Open the Chromeleon Server Configuration program. 2. Open the ICS-900 Properties dialog box and click Inject Valve. 3. Under Controlled by, check the device selected for Pump_InjectValve: For an AS, verify that the AS is shown (see Figure 3-12). Figure ICS-900 Properties: Inject valve controlled by AS For an AS40, verify that the ICS-900 is shown (see Figure 3-13). Figure ICS-900 Properties: Inject Valve Controlled by ICS To change the controlling device, select the Pump_InjectValve name and press the F2 key. On the Device Configuration dialog box, select the correct device from the Controlled By list. Click OK. For an AS40, also verify that there is a relay connection from the AS40 Load relay to the ICS-900 RELAY OUT 1. Refer to the connection instructions in Section C.5 for details. Doc /08 45

54 ICS-900 Operator s Manual Loading and Injecting Samples with a Syringe This section describes two methods for loading sample into the injection valve sample loop with a syringe: Loading sample with a syringe through the sample loading port on the front of the ICS-900 (push method) Loading sample with a vacuum syringe through the sample loading port on the front of the ICS-900 (pull method) NOTE For instructions on how to load and inject samples with an autosampler, see Section Loading Samples with a Syringe (Push Method) 1. Verify that the sample loading port on the front of the ICS-900 is connected to sample port S (5) on the injection valve (see Figure 3-14). 2. Fill a syringe with a calibration standard or sample. 3. Insert the syringe into the sample loading port on the front of the ICS Verify that the injection valve is in the Load position. If it is not, click the Load button on the ICS-900 Control panel (see Figure 3-11). 5. Overfill the sample loop with five sample loop volumes. Remember that the line from the syringe to the valve must be filled first before the sample loop can be filled. Excess sample will exit through the injection valve waste line. 6. Leave the syringe in the port. This prevents the sample from siphoning out of the loop before injection. 7. Use one of the following methods to inject the sample onto the column: Manually: Click the Inject button on the ICS-900 Control panel. See Section for details about manually processing samples. Automatically: Include the Inject command in a Chromeleon or Chromeleon Xpress program. See the examples in Section See Section for details about automatically processing samples. 46 Doc /08

55 3 Operation and Maintenance Loading Samples with a Vacuum Syringe (Pull Method) 1. Verify that the sample loading port on the front of the ICS-900 is connected to sample port S (5) on the injection valve (see Figure 3-14). 2. Disconnect the waste line from port W (6) on the injection valve and attach a shorter line: 25 to 30 cm (10 to 12 in) of PEEK or Teflon tubing (see Figure 3-14). 3. Place the free end of this line into the sample. 4. Verify that the injection valve is in the Load position. If it is not, click the Load button on the ICS-900 Control panel (see Figure 3-11). 5. Insert a syringe into the sample loading port on the front door and pull out the plunger to draw the sample into the injection valve. Draw at least five times the sample loop volume. Remember that the line from the sample to port W (6) on the injection valve must be filled first before the sample loop can be filled. Syringe Sample Loading Port (on front door) (5) S L (4) Sample W (6) (1) L P C (3) (2) Injection Valve Figure Loading Sample with a Vacuum Syringe (Pull Method) Doc /08 47

56 ICS-900 Operator s Manual 6. Use one of the following methods to inject the sample onto the column: Manually: click the Inject button on the ICS-900 Control panel. See Section for details about manually processing samples. Automatically: Include the Inject command in a Chromeleon or Chromeleon Xpress program. See the examples in Section See Section for details about automatically processing samples Example Chromeleon Commands for Loading and Injecting Samples The following examples show commands for loading and injecting samples using an AS or AS40 autosampler. Example AS Program Commands 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 ECD_1.AcqOff ;Stop data acquisition. Example AS40 Program Commands Pump_ECD_Relay_1.Closed Duration= ;Note Pump_ECD.Autozero ;Note 2 ECD_1.AcqOn ;Note 3 Pump_InjectValve.InjectPosition Duration=30.00 ;Note ECD_1.AcqOff ;Note 5 48 Doc /08

57 3 Operation and Maintenance 3.12 Maintenance AS40 Program Command Notes: 1. Close the ICS-900 RELAY OUT 1, which is connected to the AS40 LOAD relay. This signals the AS40 to load the sample. 2. Zero the baseline. 3. Start data acquisition. 4. Switch the valve to Inject for 30 seconds. 5. Stop data acquisition. This section describes routine maintenance procedures for the ICS-900 that users may perform. All other maintenance procedures must be performed by Dionex personnel. As Needed Make fresh eluent. Regularly check the eluent bottle and refill it when needed. Every time you refill the eluent bottle, also empty the regenerant bottle, rinse it, and refill it with fresh regenerant. Reset the Eluent Remaining slider on the ICS-900 Control panel (see page 29). Daily Check the ICS-900 component mounting panel (see Figure 2-2) for leaks or spills. Wipe up spills. Isolate and repair leaks (see Section 4.2). Rinse off any dried eluent or regenerant with deionized water. Check the waste container and empty when needed. Weekly Check fluid lines for crimping or discoloration. Relocate any pinched lines. Replace damaged lines. Check the back of the pump head and underneath the head for evidence of liquid leaks. Normal friction and wear may gradually result in small liquid leaks around the piston seal. If unchecked, these leaks can gradually contaminate the piston housing, causing the pump to operate poorly. If leaks occur, replace the piston seals (see Section 5.7). Doc /08 49

58 ICS-900 Operator s Manual Annually Change the pump seals (see Section 5.7). Rebuild the injection valve (see Section 5.10). If an AS Autosampler is installed, perform the AS preventive maintenance procedure. An AS Preventive Maintenance Kit (P/N ) is available for this purpose. If an AS40 Automated Sampler is installed, replace the sample tip and tubing. The ASM/AS40 Sample Tip Replacement Kit (P/N ) contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve. For instructions on how to replace the sampling tip, see the AS40 Automated Sampler Operator s Manual (Document No ). The manual is included on the Dionex Reference Library CD-ROM (P/N ). 50 Doc /08

59 4 Troubleshooting This chapter is a guide to troubleshooting problems that may occur while operating the ICS-900 Ion Chromatography System (ICS-900). Section 4.1 describes the error messages displayed in the Chromeleon or Chromeleon Xpress Audit Trail. Section 4.2 through Section 4.13 describe other operating problems and how to resolve them. If you are unable to eliminate a problem, contact Dionex for help. In the U.S., call Dionex Technical Support at Outside the U.S., call the nearest Dionex office. 4.1 Alarms and Error Conditions If any of the following alarm conditions occurs, an error message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail. Each error message is preceded by an icon that identifies the seriousness of the underlying problem (see the table below). Icon Severity Level Description Warning A message is displayed in the Audit Trail, but the current run is not interrupted. Error Abort A message is displayed in the Audit Trail and the system attempts to correct the problem (sometimes by using an alternative parameter). An Error never interrupts the current analysis; however, if it occurs during the Ready Check, the analysis will not be started. A message is displayed in the Audit Trail and the running batch is aborted. Doc /08 51

60 ICS-900 Operator s Manual The table below lists the ICS-900 error messages. For troubleshooting assistance, refer to the page indicated in the table. Alarms and Error Conditions See Conductivity exceeds limit. page 52 Flow rate calibration error. page 53 Load/inject valve error. page 53 Module data buffer overflow. Data may have been lost. page 54 Pump motor lost control. page 54 Pump pressure hardware error. page 54 Pump pressure slope calibration error. page 55 Remaining eluent below 200 ml. page 55 The system pressure is below the low pressure limit. page 56 The system pressure has exceeded the high pressure limit. page 56 Conductivity exceeds limit. This message may appear at when the ICS-900 power is turned on. If the message appears at other times, it indicates a problem. To troubleshoot: 1. Perform the suppressor inline quick start procedure: a. Disconnect the separator column outlet line from the suppressor ELUENT IN port and disconnect the cell inlet line from the suppressor ELUENT OUT port. Use a union to connect these two lines. b. Turn on the pump flow and allow the suppressor to regenerate for 10 minutes. c. Turn off the pump and allow the suppressor to hydrate for 20 minutes. d. Reconnect the separator column outlet line and cell inlet line to the suppressor ports. 2. If the high background persists: Prepare fresh eluent (see Section 3.4). Prepare fresh regenerant (see Section 3.5). 52 Doc /08

61 4 Troubleshooting Verify the cell calibration by pumping deionized water through the cell (bypassing the column(s) and suppressor). The total background should be less than 1.0 μs. Perform the suppressor off-line regeneration procedure. a. Disconnect the liquid lines from the suppressor and remove the suppressor from the ICS-900. b. Use a syringe to push the following types and amounts of fluid into the suppressor ports: AMMS 300: Push about 3 ml of 100 mm H 2 SO 4 through the ELUENT OUT port and about 5 ml of 100 mm H 2 SO 4 through the REGEN IN port. CMMS 300: Push about 3 ml of 200 mm NaOH through the ELUENT OUT port and about 5 ml of 200 mm NaOH through the REGEN IN port. c. Allow the suppressor to sit for at least 20 minutes to fully hydrate it. If the problem persists, replace the suppressor (see Section 5.12). Flow rate calibration error. This error occurs if you try to calibrate the flow rate when the pump is off, or it is on, but the flow rate is not 1 ml/min. To troubleshoot: Before calibrating the flow rate, be sure to press the Start Calibration button on the Wellness panel. This will automatically start the pump and set the flow rate to 1 ml/min. For flow rate calibration instructions, see Section Load/inject valve error. If the injection valve fails to switch positions within 1 second of being toggled, the ICS-900 Moduleware reports an error to Chromeleon or Chromeleon Xpress and this error message is displayed. Doc /08 53

62 ICS-900 Operator s Manual To troubleshoot: 1. If a sequence is being executed, terminate the sequence by selecting Stop on the Batch menu. 2. Turn off the ICS-900 power briefly and then restart. 3. Try to toggle the valve from Load to Inject by clicking the Inject button on the ICS-900 Control panel. 4. If the problem persists, contact Dionex for assistance. Module data buffer overflow. Data may have been lost. Various electronics-related problems can cause this error message to be displayed. If this warning appears, contact Dionex for assistance. The ICS-900 electronics components cannot be serviced by the user. Pump motor lost control. This error indicates a problem in the pump controller electronics. To troubleshoot: Contact Dionex for assistance. The ICS-900 electronics components cannot be serviced by the user. Pump pressure hardware error. This error indicates a problem in the pump controller electronics. To troubleshoot: Contact Dionex for assistance. The ICS-900 electronics components cannot be serviced by the user. 54 Doc /08

63 4 Troubleshooting Pump pressure slope calibration error. This error occurs if you try to calibrate the pressure slope when the pressure is less than 3 MPa (500 psi). To troubleshoot: Verify that the pump is on and the flow rate is at the rate required for the application. Verify that the pressure gauge is working correctly. Verify that the correct number and type of backpressure coils are installed. Refer to the tables on page 63. Check for liquid leaks (see Section 4.2). Remaining eluent below 200 ml. -or- Remaining eluent below 100 ml. These errors occur when the ICS-900 determines that the eluent bottle contains less than the volume specified in the message. To troubleshoot: The ICS-900 determines the eluent usage by monitoring the flow rate and the length of time the pump is on. For the eluent level to be accurate, you must enter the level on the ICS-900 Control panel each time the bottle is filled. After filling the bottle, move the Eluent Remaining slider on the ICS-900 Control panel (see Figure 3-3) to indicate the volume of liquid in the bottle. Doc /08 55

64 ICS-900 Operator s Manual The system pressure is below the low pressure limit. If the system pressure falls below the minimum pressure limit for 0.5 second, Chromeleon or Chromeleon Xpress stops the pump and displays this error message. The minimum pressure limit can be set to between 0 and 33.7 MPa (0 and 4900 psi) in the Chromeleon Server Configuration Properties dialog box or the Chromeleon or Chromeleon Xpress program. To troubleshoot: 1. Make sure the eluent bottle is full. 2. Check for liquid leaks (see Section 4.2). 3. Prime the pump (see Section 3.6). 4. Restart the pump from the ICS-900 Control panel (see Section 3.6). For additional troubleshooting information about pump priming, see Section 4.3. The system pressure has exceeded the high pressure limit. If the system pressure exceeds the maximum pressure limit for 0.5 second, Chromeleon or Chromeleon Xpress stops the pump and display this error message. The maximum pressure limit can be set to between 0.7 and 34.4 MPa (100 and 5000 psi) in the Chromeleon or Chromeleon Xpress Server Configuration or control program. To troubleshoot: 1. Check for blockages in the liquid lines by working your way backward from the cell to the pump (see Figure 2-4 for the flow schematic). 2. Restart the pump from the ICS-900 Control panel. For additional troubleshooting information about system pressure, see Section Doc /08

65 4 Troubleshooting 4.2 Liquid Leaks Leaking fitting Locate the source of the leak. Tighten or, if necessary, replace the liquid line connection (see Section 5.2). For tightening requirements, refer to the Installation of Dionex Liquid Line Fittings (Document No ), provided on the Dionex Reference Library CD-ROM (P/N ). Broken liquid line Replace the line and fittings (see Section 5.2). Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked. Also, if the blocked line is a waste line, make sure it is not elevated at any point after it exits the ICS-900. If a line is blocked, replace it (see Section 5.2). Loose pump check valve housing Make sure the check valves are firmly seated in the pump head. If they are not, tighten them carefully with an open-end wrench just until the leak stops. Damaged pump piston seal 1. Replace the piston seal (see Section 5.7). 2. If the problem persists, replace the piston (see Section 5.8). Pump head not tight Carefully tighten the pump head mounting screws just until the leak stops. DO NOT OVERTIGHTEN! Leaking pressure transducer Make sure the liquid line connections into the pressure transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No ), included on the Dionex Reference Library CD-ROM (P/N ), for tightening requirements. Replace any damaged fittings. Doc /08 57

66 ICS-900 Operator s Manual Leaking pump head waste valve Make sure the waste valve is closed. To close the valve, turn the knob clockwise, just until tight. DO NOT OVERTIGHTEN! Overtightening may damage the valve and the pump head. Inspect the pump head. If the waste valve is the source of the leak, replace the waste valve seal (see Section 5.9). Leaking MMS 300 Refer to the suppressor manual for troubleshooting procedures. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N ). Leaking injection valve Make sure the liquid line connections to the valve are tight. Replace any damaged fittings. Refer to Installation of Dionex Liquid Line Fittings (Document No ) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N ). Liquid leaks from behind the valve stator may indicate a scratched rotor seal. Rebuild the injection valve (see Section 5.10). Leaking conductivity cell Check the waste lines for blockage; trapped particles can plug the lines and cause a restriction and/or leak. If necessary, clear the waste lines by reversing the direction of flow. Make sure the plumbing downstream from the cell is clear; a blockage may overpressurize the cell, causing it to leak. If the problem continues, contact Dionex for assistance. 4.3 Pump Difficult to Prime or Loses Prime Empty eluent bottle and/or no eluent connected Fill the bottle. Make sure all connections are secure. Dirty check valve Clean or replace the pump check valve (see Section 5.6). 58 Doc /08

67 4 Troubleshooting Liquid leaks at junction between pump head and pump housing Replace the piston seal (see Section 5.7). 4.4 Pump Does Not Start No power (front door Power LED indicator fails to light) Check that the power cord is plugged in. Check the main power fuses and replace if needed (see Section 5.13). No communication between ICS-900 and Chromeleon or Chromeleon Xpress (Link LED on rear panel fails to light) The USB cable is not connected correctly. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No ), provided on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). 4.5 No Flow Pump not primed Prime the pump (see Section 3.6). Broken pump piston Replace the piston (see Section 5.8). 4.6 Erratic Flow/Pressure Reading Pump needs priming Prime the pump (see Section 3.6). Damaged piston seal Replace the piston seal (see Section 5.7). Dirty pump check valve Clean or replace the check valve (see Section 5.6). Doc /08 59

68 ICS-900 Operator s Manual 4.7 Excessive System Backpressure Restriction in system plumbing Check all liquid lines for crimping or blockage. Make sure the ferrule fittings are not overtightened onto tubing. Refer to Installation of Dionex Liquid Line Fittings (Document No ) for details. The manual is included on the Dionex Reference Library CD-ROM (P/N ). Plugged or damaged fitting Isolate the faulty fitting by loosening fittings, one by one, until the pressure returns to normal. Repair or replace the fitting (see Section 5.2). Flow rate through columns too high Check the pump flow rate. Clogged column bed supports Refer to the instructions in the column manual for troubleshooting guidance. Column manuals are included on the Dionex Reference Library CD-ROM (P/N ). Contaminated columns Clean the columns as instructed in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N ). Plugged Injection valve passages Rebuild the injection valve (see Section 5.10). 4.8 Peak Ghosting Ghosting is the appearance of extraneous peaks in a chromatogram. These may be late-eluting peaks from a previous injection or they may result from a contaminated, malfunctioning, or incorrectly installed injection valve. These peaks may co-elute with peaks of interest, resulting in nonreproducible peak heights/areas. Insufficient time between sample injections Wait until the previous sample has been completely eluted before making another injection. 60 Doc /08

69 4 Troubleshooting Insufficient flush between samples Flush the sample loop with at least 10 loop volumes of deionized water or sample between sample injections. Incorrect or contaminated standards Remake standards. Incorrect or contaminated eluent Remake the eluent (see Section 3.4). Malfunctioning injection valve Contact Dionex for assistance. 4.9 Nonreproducible Peak Height or Retention Time Column overloading Dilute the sample (see Section ). 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 ) and replace if damaged. Pump not primed properly Prime the pump (see Section 3.6) Abnormal Retention Time or Selectivity Contaminated or incorrect eluent Remake the eluent, using concentrated eluent and ASTM Type I (18- megohm) filtered and deionized water (see Section 3.4). Contaminated or degraded sample Take appropriate precautions when preparing and storing samples to prevent contamination and degradation (see Section 3.10). Doc /08 61

70 ICS-900 Operator s Manual 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 ). 2. If cleaning is unsuccessful, replace the column No Detector Response Cell not properly installed Check that the cell is plugged into the component mounting panel and the cell housing is screwed down until the bottom of the housing is flush against the sheet metal panel (see Figure 2-2 and Figure 2-10). No flow from pump Several conditions may cause this condition; see Section 4.4 and Section 4.5 for details. Cell electronics malfunctioning Use the Wellness panel to test the electronics with a dummy cell (see Section 5.1 and the Chromeleon Help for instructions). If the conductivity reading with the dummy cell is outside the tolerance range, the electronics are malfunctioning. Contact Dionex for assistance High Detector Output Background not suppressed by suppressor If Conductivity exceeds limit is displayed in the Chromeleon or Chromeleon Xpress Audit Trail, follow the instructions in Section 4.1. For additional troubleshooting guidance, refer to the suppressor manual. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N ). Sample concentration too high Dilute the sample (see Section ). Wrong eluent or regenerant Check that you are using the correct eluent and regenerant for your system (see Section 3.4). 62 Doc /08

71 4 Troubleshooting Cell out of calibration Recalibrate the cell from the Wellness panel (see Section 5.1) 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 ) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N ). Trapped gases Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them. Also loosen and retighten the fittings to and from the MMS eluent ports. Pump not properly primed Prime the pump (see Section 3.6). Contaminated or incorrect eluent and/or regenerant Remake the eluent and regenerant (see Section 3.4). Rapid changes in ambient temperature If the ambient temperature does not meet the specification of 10 to 35 C (50 to 95 F), verify that air conditioning and heating vents are directed away from the ICS-900 and the ICS-900 front door is closed. Insufficient conductivity cell backpressure Verify that the correct backpressure coils are installed: Standard bore systems: Use one or two black backpressure coils (P/N ) supplied in the ICS-900 Ship Kit (P/N ). Flow Rate Number of Coils 1.5 to 3.0 ml/min 1 (black) 0.5 to 1.5 ml/min 2 (black) Doc /08 63

72 ICS-900 Operator s Manual Microbore systems: Use one or two red backpressure coils (P/N ) supplied in the microbore tubing kit (P/N ). Flow Rate Number of Coils 0.3 to 0.5 ml/min 1 (red) Less than 0.3 ml/min 2 (red) Install the tubing between the cell outlet and the regenerant bottle inlet. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No ), provided on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). Insufficient system equilibration following changes to operating parameters; especially apparent when operating at high sensitivities Allow a longer system equilibration time (up to 3 hours) before starting to inject samples. Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N ). Cell above or below temperature Contact Dionex for assistance. Damaged piston seal Replace the piston seal (see Section 5.7). DCR backpressure tubing not installed or incorrectly installed Install the tubing on the end of the suppressor waste line. For connection instructions, see the ICS-900 Ion Chromatography System Installation Instructions (Document No ), provided on the Dionex Reference Library CD-ROM (P/N ) and in the ICS-900 Ship Kit (P/N ). 64 Doc /08

73 5 Service This chapter describes ICS-900 Ion Chromatography System (ICS-900) service and repair procedures that users may perform. Procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call Outside the U.S., call the nearest Dionex office. Before replacing any part, refer to the troubleshooting information in Chapter 4 to correctly identify the cause of the problem. Substituting non-dionex parts may impair system performance, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information. 5.1 Diagnostics and Calibrations The Wellness panel (see Figure 5-2) provides controls for performing diagnostic and calibration functions. This section provides an overview of Wellness panel features. For calibration procedures, see the following sections: Calibrating the Pressure Transducer (Section 5.1.3) Calibrating the Cell (Section 5.1.4) Calibrating the Flow Rate (see Section 5.1.5) Opening the Wellness Panel 1. In the Chromeleon Browser, expand the Dionex Templates\Panels\Wellness folder. Doc /08 65

74 ICS-900 Operator s Manual 2. Double-click Dionex_ICS-900_wellness.pan (see Figure 5-2). Figure 5-1. Opening the Wellness Panel The Wellness panel opens (see Figure 5-2). Figure 5-2. ICS-900 Wellness Panel 66 Doc /08

75 5 Service 3. If the controls on the Wellness panel are disabled, select Connect to timebase on the Control menu and select the ICS-900 timebase Wellness Panel Features The Wellness panel provides the following features: System Status The check box indicates whether the ICS-900 is connected to Chromeleon or Chromeleon Xpress. When there is no connection, the check box is clear and the remaining controls on the Wellness panel are disabled. Click the Pump button to turn the pump on and off. Click the Log Serial # button to record the ICS-900 serial number in the Audit Trail. The Calibration or Diagnostic box is green while a calibration or diagnostic procedure is running. The current total system Pressure, pump Flow rate, and electrochemical detector (ECD) conductivity are displayed. Audit Trail The Audit Trail displays an account of every event that occurs during ICS-900 operation. This includes errors, status messages, operational events, etc. Reset Calibration Parameters Click the View/Reset Cal Values button to open a window that shows the current calibration values, the previous values, and the factory-set values. You can reset the current calibration values to the previous or factory-set values from the window. Doc /08 67

76 ICS-900 Operator s Manual Calibration Pressure Transducer Use the Calibrate Offset and Calibrate Slope buttons when performing the pressure transducer calibration procedure (see Section 5.1.3). The Offset and Slope values and the date of the last calibration are displayed. Conductivity Cell Use the Calibrate Offset and Calibrate Slope buttons when performing the cell calibration procedure (see Section 5.1.4). The Offset and Slope values and the date of the last calibration are displayed. Pump Flow Rate Calibration Click Calibration Procedure to perform the calibration (see Section 5.1.5). Click Log to record the calibration value in the Audit Trail. Diagnostic The Pump and Conductivity Cell Variance values are a measure of the noise of the respective channels. The values of these measurements will vary with differing eluents, pump seal age and wear, background conductivity, and so on. When values (obtained under the same conditions) are compared they can be used as a relative measure of the performance of the system. The Variance, Minimum, and Maximum readings for the last time the Pump and Conductivity Cell diagnostic tests were run are displayed. Dummy Cell Test The Dummy Cell Test connects a fixed resistance in place of the conductivity cell. A measured value outside the typical range of the test indicates a failure in the detector electronics. Click Log to perform the test and record the value in the Audit Trail. Clicking Log enables the dummy cell, logs the value, and then disables the dummy cell. The Dummy Cell On check box enables and disables the dummy cell. 68 Doc /08

77 5 Service Calibrating the Pressure Transducer 1. Toggle the injection valve position a few times by clicking the Load and Inject buttons on the ICS-900 Control panel. This removes any air or contaminant buildup in the injection valve loop. 2. Wait about 10 minutes and then continue to Step Open the ICS-900 Wellness panel (see Section 5.1). 4. Under Pressure Transducer, click the Calibrate Offset button (see Figure 5-2). A panel with instructions and command buttons will open. 5. Follow the instructions on the panel to complete the transducer offset calibration procedure. The new offset is determined and stored as the current value. NOTE To open the waste valve on the front of the secondary pump head (see Figure 5-3), turn the knob one-half turn counterclockwise. Pressure Transducer Waste Valve Figure 5-3. ICS-900 Interior Components Doc /08 69

78 ICS-900 Operator s Manual 6. Close the waste valve. 7. Under Pressure Transducer, click the Calibrate Slope button. A panel with instructions and command buttons will open. 8. Follow the instructions on the panel to complete the transducer slope calibration procedure. The new slope is determined and stored as the current value. 9. Turn off the pump. 10. Disconnect the pressure gauge and backpressure coil. 11. Reconnect the pressure transducer to the pump Calibrating the Cell Calibrate the cell every 6 months or after installing a new conductivity cell. Items Needed Description 1.00 mm KCl solution Prepare by dissolving g of reagentgrade KCl in one liter of ASTM Type I (18 megohm-cm) filtered and deionized (DI) water (use a volumetric flask). Backpressure tubing to provide at least 7 MPa (1000 psi) Use mm (0.003-in) ID yellow PEEK tubing (P/N ). 1. Use an Allen wrench to remove the two screws securing the conductivity cell housing to the ICS-900 component mounting panel (see Figure 5-4). Save the screws. Remove Screws Figure 5-4. ICS-900 Interior Components: Removing the Conductivity Cell Housing 70 Doc /08

79 5 Service 2. Pull the cell housing straight out from the component mounting panel to unplug the cell from its electronics. Let the cell housing hang by the tubing. 3. Open the ICS-900 Wellness panel (see Section 5.1). 4. Under Conductivity Cell, click the Calibrate Offset button (see Figure 5-2). A panel with instructions and command buttons will open. 5. Follow the instructions on the panel to complete the conductivity cell offset calibration procedure. The new offset is determined and stored as the current value. NOTE To reinstall the cell, on the mounting panel, align the 9-pin connectors on the cell housing with the component mounting panel and plug the cell back into the electronics. Replace the mounting screws (removed in Step 1) and tighten. 6. Under Conductivity Cell, click the Calibrate Slope button. A panel with instructions and command buttons will open. 7. Follow the instructions on the panel to complete the conductivity cell slope calibration procedure. The new slope is determined and stored as the current value. NOTE After calibration, the conductivity reading should be ± 2 μs/cm. If this is not the case, call Dionex for assistance. 8. Flush the KCl solution from the system by pumping DI water through the cell. When the conductivity drops to near zero, stop the pump flow. 9. Reconnect the pump to the injection valve and reconnect the line from the suppressor to the cell inlet. Doc /08 71

80 ICS-900 Operator s Manual Calibrating the Flow Rate Calibrate the flow rate if the Operational Qualification or Performance Qualification flow rate accuracy and precision test fails. Items needed: mm (0.003-in) ID yellow PEEK tubing (P/N ) to create 14 ± 2 MPa (2000 ± 300 psi) of backpressure (if needed) High purity ASTM Type I (18 megohm-cm) filtered and deionized water Balance capable of weighing more than 10 g with g readability Tared beaker To calibrate: 1. Open the ICS-900 Wellness panel (see Section 5.1). 2. Under Pump Flow Rate Calibration, click Calibration Procedure. A panel with instructions and command buttons will open. 3. Follow the instructions on the panel to complete the conductivity cell slope calibration procedure. The new slope is determined and stored as the current value. NOTE Enter the weight of the collected water (in grams, to the nearest milligram). 4. Click Log to record the new calibration value in the Audit Trail. This value is stored as the current value. 72 Doc /08

81 5 Service 5.2 Replacing Tubing and Fittings The ICS-900 is plumbed with the tubing and tubing assemblies listed below. Tubing Size and Type mm (0.005-in) ID PEEK, red (P/N ) 0.25-mm (0.010-in) ID PEEK, black (P/N ) 0.50-mm (0.020-in) ID Tefzel, light blue (P/N ) 0.75-mm (0.030-in) ID PEEK, green (P/N ) 1.6-mm (0.062-in) ID Teflon, natural (P/N ) Microbore tubing kit (P/N ) Used For Connection from pump pulse damper to pressure transducer Connections between all other system components Connection from injection port on door to injection valve Connections from injection valve to waste, injection valve to pump pulse damper, and cell to regenerant bottle Connections from suppressor Regen In port to regenerant bottle, Regen Out to waste, pump to eluent bottle, and pump to waste Tubing for exchanging black 0.25-mm (0.010-in) ID PEEK lines with red mm (0.005-in) ID lines (to reduce delay volumes) fittings (P/N ) and ferrules (P/N ) are used for most tubing connections. For tightening requirements, refer to Installation of Dionex Liquid Line Fittings (Document No ). The manual is included on the Dionex Reference Library CD-ROM (P/N ). 1/8-in fittings (P/N ) and ferrules (P/N ) are used for connections to the MMS 300 regen ports and the eluent and regenerant bottles. 1/16-in fittings (P/N ) and ferrules (P/N ) are used for connections from the front door injection port to the injection valve. Doc /08 73

82 ICS-900 Operator s Manual 5.3 Isolating a Restriction in the Liquid Plumbing A restriction in the liquid plumbing will cause excessive system backpressure. 1. Begin pumping eluent through the system (including the columns). 2. Follow the ICS-900 flow schematic (see Figure 2-4) and work backward through the system, beginning at the cell exit. One at a time, loosen each fitting and observe the pressure. The connection at which the pressure drops abnormally indicates the point of restriction. If the restriction has caused such high pressure that the system cannot be operated, you must work forward through the flow schematic, adding parts one at a time until an abnormal pressure increase (and hence, the restriction) is found. 3. If the restriction is in the tubing or fitting, remove the restriction by back flushing or by replacing the tubing or fitting. 74 Doc /08

83 5 Service From cell outlet To pump inlet Backpressure Coil (1 or 2, depending on flow rate) Eluent Regenerant Conductivity Cell (in DS5 Detection Stabilizer) Regen Out Eluent Out MMS 300 Eluent In Regen In Pulse Damper To cell inlet To MMS Regen In Pressure Transducer P L Eluent in from pulse damper Secondary Primary C W Pump Heads L S Injection Valve Sample in To Waste To Waste Figure 5-5. ICS-900 Flow Schematic Doc /08 75

84 ICS-900 Operator s Manual 5.4 Cleaning Eluent Bottles Before preparing new eluent, all eluent bottles should be rinsed thoroughly (inside and out) with ASTM Type I (18 megohm-cm) filtered and deionized water. If a bottle still appears dirty, or has a slimy film on the inside, clean it as instructed below. 1. Dispose of any remaining chemicals according to municipal regulations. 2. Rinse the bottle (inside and out) with ASTM Type I (18 megohm-cm) filtered and deionized water. 3. Rinse the inside of the bottle with isopropyl alcohol or methanol. 4. If algae or bacteria have left a slimy film on the bottle, use an algicide or disinfectant (dilute hydrogen peroxide, etc.). 5. Rinse cleaning chemicals out of the bottle with ASTM Type I (18 megohmcm) filtered and deionized water. 6. Dry the bottle with clean, particulate-free air. 5.5 Changing the Sample Loop A 10 μl PEEK sample loop (P/N ) is installed on the injection valve at the factory. Unless you are using a 2 mm column, replace the sample loop with another 10 μl PEEK sample loop. If you are using a 2 mm column, refer to the column manual for the size of loop required. Column manuals are included on the Dionex Reference Library CD-ROM (P/N ) 1. Turn off the pump from the ICS-900 Control panel. 2. Open the ICS-900 front door. Sample Loop 3. Disconnect the sample loop from ports L and L on the injection valve (see Figure 5-6). Figure 5-6. ICS-900 Injection Valve 76 Doc /08

85 5 Service 4. Install the new sample loop between the two ports. 5. Make sure the loop is tightly coiled, so that the door can close securely. 6. Turn on the pump from the ICS-900 Control panel. 7. Check for leaking fittings and tighten if required. 8. Close the door. 5.6 Cleaning and Replacing Pump Check Valves A dirty check valve causes erratic flow rates and pressures. In addition, it may cause the pump to lose prime and/or be difficult to reprime. If possible, replace dirty check valves. If new check valves are not available, follow the instructions for cleaning. To replace the check valves: 1. Turn off the ICS-900 power switch and disconnect the power cord. 2. To prevent contamination of pump parts, put on a pair of powder-free gloves before disassembling the pump head. 3. Disconnect the tube fittings from the inlet and outlet check valve assemblies on the primary pump head (see Figure 5-7). 4. Use a 1/2-inch wrench to loosen both check valve assemblies. Remove the check valve assemblies from the pump head. Doc /08 77

86 ICS-900 Operator s Manual Outlet Check Valve Secondary Pump Head Primary Pump Head Inlet Check Valve NOTE Figure 5-7. Pump Heads The inlet check valve assembly housing has a 1/4-28 port. The outlet check valve assembly housing has a port. 5. Inspect the new inlet check valve assembly (P/N ) to verify that the double-hole end of the cartridge is visible (see Figure 5-8). If the double-hole end is not visible, remove the cartridge from the housing and install it correctly. 6. Inspect the new outlet check valve assembly (P/N ) to verify that the single-hole end of the cartridge is visible. If the single-hole end is not visible, remove the cartridge from the housing and install it correctly. Inlet Check Valve Outlet Check Valve 1/4-28 Port Port Flow Double-hole Flow Single-hole Figure 5-8. Check Valve Assemblies 78 Doc /08

87 5 Service NOTE The pump will not operate properly unless the cartridge is installed in the housing in the correct orientation. Liquid flows through the check valve in the large single hole and out the small double holes. 7. Install the inlet check valve assembly on the bottom of the primary pump head. Install the outlet check valve assembly on the top of the head. Tighten the check valves fingertight, and then use a wrench to tighten an additional one-quarter to one-half turn. Overtightening may damage the pump head and check valve housing and crush the check valve seats. 8. Reconnect the liquid lines and the power cord. Turn on the ICS-900 main power. 9. Prime the pump (see Section 3.6). 10. When the ICS-900 is at operating pressure, check for leaks from the check valves. Tighten a check valve a little more only if it leaks. To clean the check valves: 1. Follow Step 1 through Step 4 in the check valve replacement procedure to remove the check valve cartridges from the valve housings. 2. Place the check valve housings and cartridges in a beaker with methanol. Sonicate or agitate the parts for several minutes. 3. Rinse each check valve housing and cartridge thoroughly with filtered deionized water. 4. Follow Step 5 through Step 10 in the check valve replacement procedure to reinstall the check valves. Doc /08 79

88 ICS-900 Operator s Manual 5.7 Replacing a Pump Piston Seal and Backup Seal A damaged seal allows leakage past the piston, as well as leakage from the piston seal wash housing. The pump may be difficult to prime, flow rates may be unstable, and there may be baseline noise. Preparation: 1. Rinse the pump flow path with deionized water. Direct the flow to waste by opening the waste valve on the secondary pump head (see Figure 5-7). To open the valve, turn the knob one-half turn counterclockwise. 2. After rinsing, close the waste valve. 3. To prevent contamination of pump parts, put on a pair of rubber gloves before disassembling the pump head. To remove the head and piston: 1. Turn off the power switch and disconnect the power cord. 2. Disconnect all tubing connections to the pump head. 3. Using a 7/64-in hex key (P/N ), loosen the two screws on the pump head with the defective seal. Remove the screws, and then carefully remove the head and place it on a clean surface. 4. Slowly pull the head and allow it to separate from the housing. Carefully disengage the head from the piston by pulling the head straight off and away from its mounting studs. Lateral motion while disengaging the pump head from the piston may break the piston. Un mouvement latéral pendant la séparation de la tête et du piston peut casser le piston. Vermeiden Sie Seitwärtsbewegungen, wenn Sie den Pumpenkopg vom Kolben lösen. Andernfalls kann der Kolben brechen. 5. Place the head (front end down) on a clean work surface 6. The piston does not come off as part of the pump head assembly because it is captured by a magnetic retention system. After removing the pump head, hold 80 Doc /08

89 5 Service the shaft of the piston (near the base), tilt the piston slightly, and pull the piston away from the pump. Refer to Figure 5-9 or Figure 5-10 when disassembling and reassembling the pump head. Outlet Check Valve Assembly (P/N ) Piston Seal (P/N ) O-Ring (P/N ) Spacer with Drain (P/N ) Backup Piston Seal (P/N ) Piston (P/N ) Seal Holder (P/N ) Primary Pump Head (P/N ) Inlet Check Valve Assembly (P/N ) Figure 5-9. Primary Pump Head Piston Seal (P/N ) Seal (P/N ) O-Ring (P/N ) Spacer with Drain (P/N ) Backup Piston Seal (P/N ) Prime Valve (P/N ) Secondary Pump Head (P/N ) Piston (P/N ) Seal Holder (P/N ) Figure Secondary Pump Head Doc /08 81

90 ICS-900 Operator s Manual To install the new backup piston seal: 1. Lift the spacer off the pump head. 2. To remove the seal holder from the spacer, use one of the following methods: With the seal holder facing up, cup the spacer in your hand and blow clean laboratory air at the spacer to dislodge the seal holder. Insert a thin object or pointed tool into the small notch on the spacer and carefully pry out the seal holder. Be careful not to scratch the spacer. 3. To remove the backup piston seal from the spacer, insert a thin object (for example, the straightened end of a paper clip) and carefully pry out the backup piston seal. Be careful not to scratch the spacer. 4. To install the new backup piston seal: a. Hold the new backup piston seal (P/N ) with the grooved side facing down, and insert the shaft of the piston through the seal. b. Insert the piston into the center hole in the spacer. Spacer of backup Grooved side piston seal Notch Seal Holder c. Push the piston into the spacer until the top of the piston is flush with the spacer. A clicking sound indicates that the seal is correctly seated. 82 Doc /08

91 5 Service The piston backup piston seal is made of soft plastic. Do not press on the seal with anything hard or sharp, including your fingernail. If the seal is nicked or gouged, it will not seal properly and may result in leaks. d. Pull out the piston. The top of the seal should be flush with the surface of the spacer. e. Press the seal holder onto the spacer. To remove the old piston seal from the head: 1. Fill the head cavity with deionized water by injecting the liquid through the piston opening. 2. Reinsert the piston approximately 3 mm (0.125 inch) into the seal. 3. If this is the primary pump head, install a fitting plug (P/N ) on the outlet check valve. Tighten the plug. 4. If this is the secondary pump head, install a fitting plug (P/N ) in both the inlet and outlet ports. Tighten the plugs. 5. Push the piston into the head. (This should hydraulically unseat the seal from the head.) Remove the piston and pull off the seal. NOTE If the piston seal is not removed, make sure the fitting plug(s) are tight and add more water. Make sure the head contains no air bubbles, and then repeat Steps 2 and Remove the fitting plug(s). Doc /08 83

92 ICS-900 Operator s Manual To install the new piston seal: 1. If this is the secondary pump head, open the waste valve knob by turning the knob one-half turn counterclockwise. 2. Lubricate the seal and the pump head opening with a small amount of isopropyl Piston Seal alcohol to facilitate insertion. 3. Push the piston through the spacer and then through the new piston seal. Piston Spacer 4. Insert the piston and seal into the pump head. 5. To seat the seal, push down on the spacer until it is flush with the head. A clicking sound indicates that the seal is correctly seated. 84 Doc /08

93 5 Service 6. Remove the spacer and piston and verify that the seal is flush with the surface of the pump head. 7. Verify that the O-ring is installed in the spacer. To reinstall the head and piston: Dionex recommends reinstalling the head and piston as a single assembly, so that the piston centers itself onto the magnetic follower. 1. Hold the assembled spacer and guide with the drain tube aligned vertically and press the spacer into the head until it is flush with the indented surface of the head. 2. Insert the piston so that about 1/4 inch of the shaft is exposed. This ensures that the magnet in the follower picks up the piston. (The follower is the cylinder that holds the piston in place as it moves in and out of the pump head assembly.) 3. Reinstall the head and piston assembly; tighten the screws evenly. Doc /08 85

94 ICS-900 Operator s Manual To complete the procedure: 1. Reconnect all liquid lines to the pump head. 2. Close the waste valve knob. 3. Turn on the ICS-900 power switch. 4. Prime the pump (see Section 3.6). 5. Reset the seal wear counter in Chromeleon or Chromeleon Xpress: a. Press F8 to open the Commands dialog box. b. Expand the list of commands under Pump_ECD and scroll to the ResetSealWear command (see Figure 5-11). c. Select the command and click Execute. Figure Resetting the Seal Wear Counter 5.8 Replacing a Pump Piston Continued leaking of the piston seal after installation of a new seal (assuming the pump head is tight) indicates a dirty, scratched, or broken piston. Follow the instructions in Section 5.7 to install a new piston (P/N ) and piston seal (P/N ). Always replace the piston seal when replacing a piston. After replacing the piston and seal, reset the seal wear and pump piston stroke counters. 86 Doc /08

95 5 Service 5.9 Replacing the Waste Valve Seal A damaged seal causes leakage around the base of the waste valve knob. 1. Turn off the ICS-900 power switch. 2. To remove the waste valve from the pump head (see Figure 5-12), turn the knob counterclockwise until it is loose, and then pull the knob straight out of the cavity in the pump head. Waste Valve Figure Waste and Priming Valves 3. If the seal is removed with the valve knob in Step 2, pull the seal off the end of the Valve Knob knob (see Figure 5-13). If the seal is not removed with the valve knob, insert a thin object (for example, the straightened end of a paper clip) into the cavity in the Seal pump head and carefully pull out the seal. Do not scratch the cavity. Figure Waste Valve Seal Replacement Scratches in the cavity will cause leaks around the base of the knob while the pump is being primed. Doc /08 87

96 ICS-900 Operator s Manual 4. Orient the new seal (P/N ) with the grooved side away from the valve and slide it over the end of the valve. 5. Insert the valve with the new seal into the pump head opening and turn the knob clockwise. Tighten fingertight. 6. Turn on the ICS-900 power switch. 7. Prime the pump (see Section 3.6) Rebuilding the Injection Valve Dionex recommends rebuilding the injection valve annually. The Injection Valve Rebuild Kit (P/N ) contains all required replacement parts. NOTE Substitution of non-dionex parts may impair valve performance and void the product warranty. 1. Turn off the pump. 2. Open the front door of the ICS Disconnect each liquid line connected to the injection valve. 4. Follow the instructions provided in the Injection Valve Maintenance Kit to replace the rotor seal, isolation seal, and stator face. 5. Reconnect all liquid lines to the injection valve. 6. Close the ICS-900 front door. 7. Turn on the pump from the ICS-900 Control panel. 88 Doc /08

97 5 Service 8. Reset the injection valve cycle counter in Chromeleon or Chromeleon Xpress: a. Press F8 to open the Commands dialog box. b. Expand the list of commands under Pump_ECD and scroll to the ResetInjValveCounter command (see Figure 5-14). c. Select the command and click Execute. Figure Resetting the Injection Valve Counter Doc /08 89

98 ICS-900 Operator s Manual 5.11 Replacing the Conductivity Cell 1. Turn off the ICS-900 power switch. 1. Disconnect the power cord. 2. Open the ICS-900 front door. 3. Disconnect the black ELUENT OUT line from the ELUENT OUT port on the suppressor (see Figure 5-15). DS5 Detection Stabilizer ELUENT OUT to suppressor CELL OUT (orange) to CELL OUT (black) Connector to component mounting panel Figure Conductivity Cell Assembly 4. Disconnect the orange CELL OUT line from the union that connects it to the black CELL OUT line. 5. Use an Allen wrench to remove the two screws on the top of the cell housing. 6. Remove the cell by unplugging it from the component mounting panel. 7. Plug the new conductivity cell (P/N ) into its mounting location. 8. Replace the screws on the top of the cell housing and tighten. 9. Attach the orange CELL OUT line from the cell to the union attached to the black CELL OUT line. Attach the ELUENT OUT line to the ELUENT OUT port on the suppressor. 10. Close the front door. 90 Doc /08

99 5 Service 11. Reconnect the power cord and turn on the ICS-900 power. 12. Calibrate the cell (see Section 5.1.4) Replacing the Suppressor Refer to the suppressor manual for guidance about when to replace a suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N ). 1. Turn off the pump. 2. Open the front door of the ICS Disconnect the four eluent and regenerant lines from the suppressor. 4. Slide the suppressor to the left to detach it from the component mounting panel. 5. Slide the new suppressor to the right until it locks into place on the mounting panel. 6. Connect the four eluent and regenerant lines to the new suppressor. 7. Close the ICS-900 front door. 8. Prime the pump (see Section 3.6). Doc /08 91

100 ICS-900 Operator s Manual 5.13 Changing the Main Power Fuses 1. Turn off the ICS-900 power switch. 1. Disconnect the power cord. HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the ICS-900. HAUTE TENSION Débranchez le cordon d'alimentation principal de sa source et du panneau arrière du ICS-900. HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des ICS The fuse drawer is located above the power switch (see Figure 5-16). A small tab locks the fuse drawer in place. Using a small screwdriver, press the tab in and then up to release the fuse drawer. 3. Pull the fuse drawer out of the rear panel and remove the old fuses. 4. Replace the two fuses with new fast-blow IEC 127 fuses rated 3.15 A (P/N ). Dionex recommends always replacing both fuses. Fuse Drawer Tab Figure Fuse Drawer 5. Insert the fuse drawer into the rear panel and press until the drawer snaps into place. 6. Reconnect the main power cord and turn on the power. 92 Doc /08

101 A Specifications A.1 Electrical Main Power 90 to 265 VAC, 47 to 63 Hz (Auto-sensing power supply; no manual voltage or frequency adjustment required) Maximum input power: 90 W Maximum line draw: 1.5 A Fuses Two fast-blow IEC 127 fuses rated 3.15 A (P/N ) A.2 Physical Dimensions Weight Decibel Level Height without bottles: cm (12.85 in) Height with bottles and cap tubing: cm (23.85 in) Width: cm (9.29 in) Depth: cm (15.89 in) 14 kg (30 lb) < 53 dba Doc /08 93

102 ICS-900 Operator s Manual A.3 Environmental Operating Temperature Humidity 10 to 35 C (50 to 95 F) 5% to 95% relative humidity, noncondensing A.4 Front Panel Operational LED Indicators LEDs display the ICS-900 operational status: Power Off: No power On: Power present Ready Off: Not connected to Chromeleon or Chromeleon Xpress On: System check passed and the ICS-900 is connected to Chromeleon or Chromeleon Xpress Flashing: System check failed (occurs if system check executes for 10 minutes without success) Run Off: Not running On: Running/acquiring data Flashing: Error/alarm/fault (including injection valve position fault) 94 Doc /08

103 A Specifications A.5 Rear Panel Link LED The Link LED displays the communication status between the ICS-900 and Chromeleon or Chromeleon Xpress: Off: There is no communication link between the ICS-900 and Chromeleon or Chromeleon Xpress. On: The communication link between the ICS-900 and Chromeleon or Chromeleon Xpress is activated, but data is not being transmitted or received. Flashing: The communication link between the ICS-900 and Chromeleon or Chromeleon Xpress is activated and data is being transmitted or received. A.6 Pump Type Flow Rate Maximum Operating Pressure Dual-piston (in series), variable speed, 100 μl per revolution Programmable range: 0.01 to 5.00 ml/min, in 0.01 increments Optimal operational range: 0.20 to 3.00 ml/min 35 MPa (5000 psi) Doc /08 95

104 ICS-900 Operator s Manual A.7 Detector Range Temperature Compensation Cell Drive Auto Offset Control and Data Evaluation Digital signal range of 0 to 500 μs or 0 to 10,000 μs (userselectable) Preset for accurate reading at 40 ºC 8 khz square wave -999 to 999 μs Provided by Chromeleon or Chromeleon Xpress software; communication with the ICS-900 is via USB (Universal Serial Bus) Linearity 1% A.8 Conductivity Cell Cell Body Electrodes Active Volume Maximum Pressure PEEK Passivated 316 stainless steel 1 μl 2.0 MPa (300 psi) Temperature Regulated at 40 ºC A.9 Injection Valve Injection Valve Two-position, six-port, electrically-activated Rheodyne valve with PEEK wetted components A.10 Delay Volume System Total <5 ml 96 Doc /08

105 B Reordering Information Part Number Item Pump Primary pump head assembly Secondary pump head assembly Outlet check valve assembly, Inlet check valve assembly, 1/ Piston seal O-ring Backup piston seal Seal holder Piston Sample Loop and Injection Valve μl sample loop assembly Injection valve rebuild kit Luer adapter fitting, 1/4-28 (for manual injections) Reagent Bottle Assemblies Eluent bottle assembly (includes stopper and cap) Anion regenerant bottle assembly (includes stopper and cap) Cation regenerant bottle assembly (includes stopper and cap) O-ring for eluent or regenerant bottle stopper Doc /08 97

106 ICS-900 Operator s Manual Part Number Item Reagents Anion regenerant concentrate (75 ml of 2.0 N sulfuric acid) pack of anion regenerant concentrate Cation regenerant concentrate (100 ml of 2.06 M TBAOH) pack of cation regenerant concentrate Suppressors and Cell AMMS 300 suppressor, 4 mm AMMS 300 suppressor, 2 mm CMMS 300 suppressor, 4 mm CMMS 300 suppressor, 2 mm T Conductivity cell with DS5 Detection Stabilizer P/N Microbore tubing kit 98 Doc /08

107 C TTL and Relay Control A 12-pin connector strip for TTL/relay control is located on the ICS-900 rear panel. The connector provides two relay outputs, two TTL outputs, and four TTL inputs (see Figure C-1). Pin Function Description RELAY OUT 1 2 Solid State Relay Contacts Output Solid State Relay Contacts Output TTL OUT (+) TTL IN (+) TTL GND (-) TTL Output 1 (1 k Ω pull up to +5, 100 ma sink) TTL Output 2 (1 k Ω pull up to +5, 100 ma sink) TTL Input 1 Autozero TTL Input 2 Inject/Load TTL Input 3 Pump On/Off TTL Input 4 Autozero Ground Ground Note: These are the default TTL input function assignments. Functions can be reassigned to any input. Figure C-1. TTL and Relay Connector on Rear Panel Relay loads in excess of 200 ma or with included power supplies over 60 V may damage the relay drivers on the instrument s CPU board. TTL and relay outputs can be used to control functions in external devices, such as an autosampler or another Dionex module. Relay outputs 1 and 2 can be programmed to switch any low-voltage control. Switched current must be less than 200 ma and 60 V peak. Relay outputs 1 and 2 can be configured to close when the pump flow is on and open when the pump flow is off, thus ensuring that a connected device is turned off when the pump flow is off. See Section C.3 for details. Doc /08 99

108 ICS-900 Operator s Manual When connected to a controlling device, the inputs can be programmed to perform the following ICS-900 functions: Switch the injection valve position (load/inject) Set the conductivity to zero (autozero) Turn the pump on and off C.1 Connecting a TTL or Relay 1. Locate the 12-position connector plug (P/N ) (see Figure C-2) in the ICS-900 Ship Kit (P/N ). 2. Obtain a twisted pair of wires (P/N ) from the Ship Kit of the Dionex instrument that will be connected to the ICS Follow these basic steps to connect the TTL or relays. Locking Screws Figure C Position Connector Plug a. For each TTL or relay to be used, connect an active wire (red) and a ground wire (black) to the 12-position connector plug at the appropriate pin locations. Refer to Figure C-1 or the label on the ICS-900 rear panel for the connector pin assignments. To attach a wire to the plug, strip the end of the wire (if necessary), insert it into the plug, and use a screwdriver to tighten the locking screw. Multiple ground wires can be attached to a single TTL input/output ground pin. When attaching wires to the connector plug, be careful not to allow stray strands of wire to short to the adjoining position on the connector. b. Plug the connector into the 12-pin connector on the ICS-900 rear panel. c. Connect the wires from the ICS-900 connector plug to the TTL or relay connector pins on the other module(s). Additional connector plugs are provided with other Dionex modules. 100 Doc /08

109 C TTL and Relay Control NOTE Check the polarity of each connection. Connect signal wires to signal (+) pins and ground wires to ground (-) pins. 4. If you connected a TTL input, verify that the correct input control mode and function is assigned to the input. Select different settings if necessary (see Section C.2). 5. If you connected a TTL output that you want to be turned off when the pump flow is off, enable the Flow Zero option in the Chromeleon Server Configuration program (see Section C.3). C.2 Selecting TTL Input Control Modes and Functions To select a control mode and function for a TTL input: 1. Start the Chromeleon Server Configuration program (click Start on the Windows taskbar and select All Programs (or Programs) > Chromeleon > Server Configuration). 2. Right-click the ICS-900 device in the timebase and select Properties. 3. Click the TTL Inputs tab (see Figure C-3). Figure C-3. ICS-900 Server Configuration Properties: TTL Inputs Tab Page Doc /08 101

110 ICS-900 Operator s Manual 4. Double-click the TTL input name or select the name and press the F2 key to open the Device Configuration dialog box (see Figure C-4). Figure C-4. ICS-900 Server Configuration Properties: TTL Input Configuration 5. Select the desired Mode and Control Function. TTL Input Control Modes The ICS-900 TTL inputs respond to four types of signals to accommodate different controlling devices. The default control mode, Normal Edge, is compatible with the output signals provided by Dionex modules. If the device connected to the ICS-900 does not send a normal edge signal, select the appropriate control mode. Refer to the documentation provided with the controlling device and the information below to select the correct type. 102 Doc /08

111 C TTL and Relay Control Normal Edge: In normal edge operation, the negative (falling) edge of a signal turns on the function. For example, for the Load/Inject function, the negative edge switches the injection valve position to Load. For the Pump On/Off function, the negative edge turns on the pump. For the Autozero function, the negative edge performs an autozero command. The action of the positive (rising) edge depends on the function. For example, for the Load/Inject function, the positive edge switches the injection valve to the Inject position. For the Pump On/Off function, the positive edge turns off the pump. For the Autozero function, the positive edge has no effect. Inverted Edge: The inverted edge mode Action On works identically to the normal edge mode except that the positive and TTL +5 V INVERTED negative edges are reversed in function. EDGE Normal Pulse: In normal pulse operation, the negative edge of the TTL signal is the active edge and the positive edge is ignored. TTL +5 V NORMAL EDGE +0 V Action Off or No Effect Action On Action Off or No Effect A pulse width of 50 ms or more is guaranteed to be detected. A pulse width of 4 ms or less is guaranteed to be ignored. The action for pulse widths that are greater than 4 ms and less than 50 ms is undefined. Inverted Pulse: The inverted pulse mode operates identically to the normal Action On Action Off pulse mode except that the positive and TTL +5 V negative edges are reversed in function. INVERTED +0 V +5 V TTL NORMAL PULSE +0 V Action On PULSE +0 V Action Off Doc /08 103

112 ICS-900 Operator s Manual C.3 Configuring Relay Output 1 or 2 to Respond to the Pump Flow Relay Output 1 or 2 can be configured to open and close with the pump flow. This allows a connected accessory device to be turned on when the pump flow starts and turned off when the flow stops. 1. Start the Chromeleon Server Configuration program (click Start on the Windows taskbar and select All Programs (or Programs) > Chromeleon > Server Configuration). 2. Right-click the ICS-900 device in the timebase and select Properties. 3. Click the State Devices tab (see Figure C-5). Figure C-5. ICS-900 Server Configuration Properties: State Devices Tab Page 104 Doc /08

113 C TTL and Relay Control 4. Select the Relay output name (Pump_ECD_Relay_1 or Pump_ECD_Relay_2) and press the F2 key to open the Device Configuration dialog box (see Figure C-6). NOTE Select Pump_ECD_Relay_2 if an AS40 is already connected to Pump_ECD_Relay_1. Figure C-6. ICS-900 Server Configuration Properties: Flow Zero Configuration 5. Select the Flow Zero check box and click OK. The ICS-900 will now open this relay output when the pump flow stops and close the relay when the flow starts. The relay can then be used turn a connected accessory device off and on with the pump flow. To use this relay output for another function, clear the check box. Chromeleon or Chromeleon Xpress will then control the relay output (see Section C-4). Doc /08 105

114 ICS-900 Operator s Manual C.4 Controlling TTL and Relay Outputs The ICS-900 provides two TTL outputs and two relay contacts for control of functions in external devices, such as an autosampler. The relay outputs can be used to switch any low-voltage control. Switched current must be less than 200 ma and 60 V peak blocking. The relay-contact closures are normally open. When the relay is closed, current flows to the connected device. Relay loads in excess of 200 ma or with included power supplies over 60 V may damage the relay drivers on the CPU. The TTL outputs are normally at 5 volts. Setting a TTL output to 0 volts turns on the action in the connected device. You can control the TTL and relay output states, either by issuing direct control commands from the Chromeleon or Chromeleon Xpress Commands dialog box or by including the commands in a program. To directly control TTL and relay outputs: 1. Press the F8 key to open the Commands dialog box. 2. Expand the list of command under Pump_ECD and select the TTL or relay output name. Then, execute the desired command (see the example in Figure C-7). Figure C-7. Chromeleon Commands Dialog Box: Example TTL Output Control Command 106 Doc /08

115 C TTL and Relay Control To program control of TTL and relay outputs: Add commands for controlling the TTL and relay outputs to the Chromeleon or Chromeleon Xpress program. You can enter the commands on the Relay and State Devices page in the Program Editor or Program Wizard (see Figure C-8). Figure C-8. Chromeleon or Chromeleon Xpress Program Editor: Example Relay Output Control Command Doc /08 107

116 ICS-900 Operator s Manual C.5 Controlling an AS40 Automated Sampler with a Relay ICS-900 Rear Panel TTL/Relay Connector AS40 Rear Panel RELAY CONTROL RELAY OUT 1 2 READY OUT GND F2 GND LOAD GND CBL PRESENT GND +5VDC<50Ma GND TTL OUT (+) 1 2 red green TTL IN (+) red green Load Relay Control Cable TTL GND (-) 1 2 Figure C-9. Example AS40 Automated Sampler Connection Figure C-10 shows example commands for controlling Relay Out 1 on the ICS-900. This relay is connected to the Load relay on an AS40. The command Pump_ECD_Relay_1.Closed closes Relay Out 1, which starts the AS40 sample 108 Doc /08

117 C TTL and Relay Control Load cycle. After 138 seconds (Duration=138.00), the AS40 Load cycle is complete and the relay is opened. Relay Out 1 closed. The AS40 Load cycle starts. When the AS40 Load cycle ends, Relay Out 1 opened. Figure C-10. Example Program for AS40 Control Doc /08 109