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Dionex ICS-1100 Operator's Manual

Ion chromatography system
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ICS-1100 Ion Chromatography System
Operator's Manual
Document No. 065289
Revision 01
March 2009

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Summary of Contents for Dionex ICS-1100

  • Page 1 ICS-1100 Ion Chromatography System Operator’s Manual Document No. 065289 Revision 01 March 2009...

  • Page 2: Printing History

    Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94088-3603 U.S.A.

  • Page 3: Table Of Contents

    Overview of the ICS-1100 ........
  • Page 4 ICS-1100 Ion Chromatography System System Component Details ........26 2.4.1...
  • Page 5 Contents Set System Operating Conditions ......46 Equilibrate the System and Verify Operational Status ... . . 46 Prepare Samples .
  • Page 6 ICS-1100 Ion Chromatography System Excessive System Backpressure .......72 Peak “Ghosting” ......... . .73 4.10 Nonreproducible Peak Height or Retention Time .
  • Page 7 Contents 5.11 Replacing the Suppressor ........103 5.12 Replacing the Column Heater .
  • Page 8 ICS-1100 Ion Chromatography System A.13 Suppressors ..........136 A.14 Autosampler .
  • Page 9 Contents D.13 How do I clean a column? ........153 D.14 Why is the conductivity high? .
  • Page 10 ICS-1100 Ion Chromatography System viii Doc. 065289-01 3/09...

  • Page 11: Introduction

    1 • Introduction Introduction to Ion Chromatography (IC) The Dionex ICS-1100 Ion Chromatography System (ICS-1100) performs ion analyses using suppressed or non-suppressed conductivity detection. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system.
  • Page 12 1. Eluent Delivery • Eluent, a liquid that helps to separate the sample ions, carries the sample through the ion chromatography system. The ICS-1100 is an isocratic delivery system. This means that the eluent composition and concentration remain constant throughout the run.
  • Page 13 • As the eluent and sample are pumped through the separator column, the sample ions are separated. In the ICS-1100, the mode of separation is called ion exchange. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites.

  • Page 14: Overview Of The Ics-1100

    The ICS-1100 can optionally be configured with a column heater for temperature control of the column. An optional second high-pressure valve (6-port or 10-port) can be installed for sample preparation applications.

  • Page 15: About This Manual

    ® ® Adob Acrobat or Adobe Reader for assistance Chapter 1 Introduces ion analysis and the ICS-1100; explains the Introduction conventions used in this manual, including safety-related information. Chapter 2 Provides an overview of ICS-1100 operating features and Features system components; introduces the Chromeleon user interface.

  • Page 16: Safety Messages And Notes

    ICS-1100 Ion Chromatography System Appendix E Defines terms commonly used in ion analysis. Glossary 1.3.1 Safety Messages and Notes This manual contains warnings and precautionary statements that, when properly followed, can prevent personal injury and/or damage to the instrument. Safety messages appear in bold type and are accompanied by icons, as shown below.
  • Page 17 1 • Introduction Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen. Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen. Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn eine Situation zu schweren Schäden am Gerät führen kann, jedoch keine Verletzungsgefahr besteht.

  • Page 18: Safety And Regulatory Information

    • EN 61326-1:2006 Safety • CAN/CSA-C22.2 61010-1:2004 • UL 61010-1:2004 • EN 61010-1:2001 The symbols below appear on the ICS-1100 or on labels affixed to the ICS-1100. Alternating current Primary protective conductor terminal Secondary protective conductor terminal Doc. 065289-01 3/09...
  • Page 19 1 • Introduction Power supply is on Power supply is off Hot surface Indicates a potential hazard. Refer to the operator’s manual for an explanation of the hazard and how to proceed. Doc. 065289-01 3/09...
  • Page 20 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 21: Features

    2 • Features This chapter describes key ICS-1100 features and introduces the Chromeleon user interface. Operating Features 2.1.1 Front Panel Figure 2-1 illustrates the front panel of the ICS-1100. Injection Port The sample to be analyzed can be injected manually into the injection port, using a syringe.
  • Page 22 The suppressor is turned off. Column Column heater is at set Column heater is transitioning to a new Heater temperature. temperature. Table 2-1. ICS-1100 Status LED States Doc. 065289-01 3/09...

  • Page 23: Top Cover

    2 • Features 2.1.2 Top Cover Figure 2-3 illustrates the top cover of the ICS-1100. Reservoir Storage The ICS-1100 top cover has room for up to three 2-L plastic Eluent reservoirs (P/N 044129) or one 4- Reservoir L plastic reservoir (P/N 039164).

  • Page 24: Component Panel

    ICS-1100 Ion Chromatography System 2.1.3 Component Panel Figure 2-4 shows the user-accessible components installed on the component panel behind the ICS-1100 front door. Pressure Transducer Leak Sensor Pump Heads Injection Valve Site for Auxiliary Valve (Optional) DS6 Conductivity Cell Suppressor...
  • Page 25 LED flashes. Alarm Pump Heads The ICS-1100 includes a dual-piston serial pump. The flow rate can be set to 0.00 mL/min or to between 0.05 and 5.00 mL/min. However, for optimum performance, set the flow rate to between 0.40 and 2.00 mL/min.
  • Page 26 The upper tubing chase routes tubing from the top cover to the component panel. The lower tubing chase routes tubing from the component panel, through the interior of the ICS-1100, to the rear panel. It also routes tubing from the RFIC-ER compartment, through the interior of the ICS- 1100, to the component panel.

  • Page 27: Right-Side Panel

    If you plan to operate in the RFIC-ER mode, you must order one of these kits: • RFIC-ER Anion Startup Kit, ICS-1100/ICS-1600 (P/N 069570) • RFIC-ER Cation Startup Kit, ICS-1100/ICS-1600 (P/N 069569) Each Startup Kit includes one Installation Kit and one Consumables Kit.

  • Page 28: Rear Panel

    ICS-1100 installation instructions. USB Connectors A USB receptacle is provided to allow connection to the Chromeleon computer. Two USB ports are provided for connecting to other USB devices. For connection instructions, refer to the ICS-1100 installation instructions. Doc. 065289-01 3/09...
  • Page 29 Tubing Chases The upper tubing chase routes tubing from the RFIC-ER compartment to the ICS-1100 rear panel. The lower chase routes tubing from the rear panel to the component panel. Tubing Clips The tubing clips hold tubing routed from the top cover in place.

  • Page 30: Flow Schematics

    ICS-1100 Ion Chromatography System Flow Schematics The following figures illustrate the liquid flow path through an ICS-1100 when using suppression in autorecycle mode. Two configurations are shown: • Figure 2-7 illustrates the liquid flow path through components when performing conventional ion chromatography.
  • Page 31 2 • Features WASTE ELUENT COND CELL PULSE DAMPER PUMP PUMP HEAD HEAD WASTE PRESS. XDUCER Figure 2-7. ICS-1100 Flow Schematic: Standard Configuration Doc. 065289-01 3/09...
  • Page 32 ICS-1100 Ion Chromatography System Flow Description for RFIC-ER Mode • Eluent from the eluent reservoir flows first through the pump degas assembly (if it is installed) and then through the eluent valve to the pump . The eluent is then pushed through the pressure transducer , which measures the system pressure.
  • Page 33 2 • Features ERC 10 ELUENT ER3b ER3a COND CELL PULSE DAMPER PUMP PUMP HEAD HEAD WASTE PRESS. XDUCER Figure 2-8. ICS-1100 Flow Schematic: RFIC-ER Mode Doc. 065289-01 3/09...

  • Page 34: Chromeleon And Chromeleon Xpress

    ICS-1100 Ion Chromatography System Chromeleon and Chromeleon Xpress The ICS-1100 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.

  • Page 35: Software Control Modes

    • A Status panel shows the overall system status. • An Autosampler panel (included if the ICS-1100 is connected to an AS, AS-DV, or AS-HV Autosampler) provides access to autosampler functions. To open the panel tabset, use one of the methods below: •...

  • Page 36: System Component Details

    The electronics required to operate the vacuum pump • Tubing, fittings, and other accessories By default, the ICS-1100 monitors the degas pressure reading and turns the degas pump on and off as needed. Different degas operating modes can be selected from Chromeleon.
  • Page 37 • : The degas pump is always on. This setting is for test Always On purposes by a Dionex Service Representative. Do not use this setting for routine operation. • : The degas pump cycles on and off according to the times...

  • Page 38: Eluent Valve

    Figure 2-11. Eluent Valve 2.4.3 Pump The ICS-1100 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 2-12).
  • Page 39 Inlet Check Valve Pressure Transducer Figure 2-12. ICS-1100 Pump Components Secondary Pump Head The secondary pump head delivers eluent to the remainder of the chromatography system (the injection valve, column, and detector). The waste valve is located on the front of the secondary pump head (see Figure 2-12).

  • Page 40: Injection Valve

    For continued protection of the pump, replace the piston rinse seals (see Section 5.7) and O-rings in the seal wash assembly every 6 months, or whenever you replace the main piston seals for the ICS-1100 pump. 2.4.4 Injection Valve The injection valve (P/N 057968) is a six-port, electrically-activated valve.
  • Page 41 A 25-μL PEEK sample loop (P/N 042857) is installed between ports L (1) and L (4). Dionex offers sample loops in various sizes. If necessary, the pre-installed 25-μL loop can be replaced with a loop that has a different sample injection volume.

  • Page 42: Auxiliary Valve (Optional)

    • ™ AutoNeutralization • Matrix diversion prior to MS (mass spectrometry) detection For more information, refer to Installing the ICS-1100/ICS-1600/ICS- 2100 Auxiliary Valve (Document No. 065288). The manual is provided in the Auxiliary Valve Kit. Doc. 065289-01 3/09...

  • Page 43: Column Heater (Optional)

    2 • Features 2.4.6 Column Heater (Optional) The column heater provides temperature control for the separator and guard column. The heater temperature can be set to between 30 °C and 60 °C. However, the set temperature must be at least 5 °C above the ambient temperature.

  • Page 44: Suppressor

    MicroMembrane Suppressor can be used with the ICS-1100. For details about any of the suppressors or for information about selecting a suppressor for your application, refer to the suppressor manuals. The manuals are on the Dionex Reference Library CD-ROM (P/N 053891). 2.4.8 DS6 Heated Conductivity Cell The flow-through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell.

  • Page 45: Er Controller

    (such as hydrogen and oxygen) in the eluent stream. If the predefined safety limit is exceeded, the ERC 10 shuts down the ICS-1100 pump to prevent the buildup of gases in the eluent bottle.
  • Page 46 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 47: Operation And Maintenance

    This chapter describes routine operating and maintenance procedures for the ICS- 1100. The ICS-1100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of the ICS-1100 in a manner not specified by Dionex may result in personal injury. Operation Overview Figure 3-1 illustrates the basic steps for routine operation of the ICS-1100.
  • Page 48 ICS-1100 Ion Chromatography System Sample Processing Overview Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-2 shows the typical steps for manual and batch sample processing. Manual Sam ple...

  • Page 49: Turning On The System Power

    Reading current value Suppressor Off* Cell heater Set to the last value used. The default when the ICS-1100 is turned on for the first time is 35 °C. Column oven temperature Set to the last value used. The default when the ICS-1100 (Optional) is turned on for the first time is 30 °C.

  • Page 50: Connecting To Chromeleon

    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-1100 Control panel, click the tab labeled with the ICS- 1100 timebase name (see Figure 3-4).

  • Page 51: Set Up The Eluent Reservoir

    3 • Operation and Maintenance Figure 3-4. ICS-1100 Control Panel on the Chromeleon Panel Tabset Set Up the Eluent Reservoir NOTE If you plan to operate the system in the RFIC-ER mode, disregard the instructions here. Follow the instructions provided with your RFIC-ER Installation Kit to set up the RFIC-ER eluent reservoir.

  • Page 52: Degas The Eluent

    • The optional vacuum degas assembly provides programmable, online degassing. The degas assembly must be installed in the ICS-1100 at the factory. If the ICS-1100 does not contain a degas assembly, manually degas eluent daily (following the instructions below) and store it in pressurized reservoirs.

  • Page 53: Filter The Eluent

    Filtering removes small particulates in the eluent that may contaminate the pump check valves and cause erratic flow rates or loss of prime. An end-line filter (P/N 045987) is provided in the ICS-1100 Ship Kit (P/N 057905) for this purpose.

  • Page 54: Connect The Reservoir

    ELUENT IN and cable chase on the top of the ICS-1100. Check All Connections Make sure the eluent reservoir is filled and the tubing connecting the reservoir to the ICS-1100 tubing is securely connected.

  • Page 55: Prime The Pump

    Prime on the Chromeleon Control panel. The pump will begin pumping at approximately 3 mL/min. 4. Continue priming the ICS-1100 until all air and previous eluent are purged and no air bubbles are exiting the waste line. 5. Press Pump Off 6.

  • Page 56: Set System Operating Conditions

    ICS-1100 Ion Chromatography System Set System Operating Conditions NOTE This section is an overview of the steps needed to start up the system and begin running samples. Actual operating parameters (flow rate, cell heater temperature, suppressor current, etc.) depend on the application to be run.

  • Page 57: Prepare Samples

    3 • Operation and Maintenance • If the pressure is less than the expected amount, gas may be trapped in the system. To release the gas, remove the pump fitting on the injection valve port, labeled ). Allow the air to escape and then reconnect the fitting. •...

  • Page 58: Pretreating Samples

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

  • Page 59: Loading And Injecting Samples

    1100 injection valve and replaced by the autosampler outlet tubing. Other setup requirements depend upon the model of autosampler. Setup for an AS Autosampler To use an AS Autosampler with the ICS-1100, the following requirements must be met: • The ICS-1100 injection valve (or the auxiliary valve, if installed) must be specified as the injection valve and must be linked to the AS in the Chromeleon timebase.

  • Page 60: Loading Samples With A Syringe

    3-7). Figure 3-7. Injection Valve Connections 2. Fill the 1 cc syringe (P/N 016388) provided in the ICS-1100 Ship Kit (P/N 057905) with a calibration standard or sample. 3. Insert the syringe into the injection port on the ICS-1100 front door...

  • Page 61: Loading Samples With An Autosampler

    3 • Operation and Maintenance 4. Insert the 1 cc syringe (P/N 016388) provided in the ICS-1100 Ship Kit (P/N 057905) into the injection port on the ICS-1100 front door (see Figure 2-1) and pull out the plunger to draw the sample into the injection valve.

  • Page 62: Injecting Samples

    Summary of Manual Sample Processing 1. Complete the instructions in Section 3.2 through Section 3.8 prepare the ICS-1100 for operation and to prepare the sample for processing. 2. Load the sample, using a syringe, vacuum syringe, or autosampler (see Section 3.10).

  • Page 63: Automatic (Batch) Sample Processing

    Section 3.2 through Section 3.8 prepare the ICS-1100 for operation and to prepare the sample for processing. 2. If an autosampler is installed, prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions.
  • Page 64 ICS-1100 Ion Chromatography System 3. If an autosampler is not installed, load the sample into the injection valve sample loop through the sample port on the ICS-1100 front door (see Section 3.10.1). 4. Use the Application Wizard to specify a program and quantitation method, and create a sequence: a.

  • Page 65: Maintenance

    Open. c. Click Start Batch. 3.12 Maintenance This section describes routine maintenance procedures that users may perform. All other maintenance procedures must be performed by Dionex personnel. As Needed • Regularly check the eluent reservoir and refill when needed.
  • Page 66 Replace the pump piston rinse seals and piston seals (see Section 5.7). Yearly • Dionex recommends performing preventive maintenance annually, as well as before scheduled Performance Qualification tests. An ICS-1100 Preventive Maintenance Kit (P/N 057954) is available for this purpose. • Rebuild the auxiliary valve, if installed (see Section 5.4).

  • Page 67: Troubleshooting

    4 • Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the ICS-1100. Turn to the section of this chapter that best describes the operating problem or symptom that has been observed. Each section lists possible causes of the problem or symptom in order of probability.
  • Page 68 ICS-1100 Ion Chromatography System The table below lists the most frequently observed ICS-1100 error messages. For troubleshooting assistance, refer to the page indicated in the table. Alarms and Error Conditions Column heater exceeds safe temperature page 59 Column heater open circuit...

  • Page 69: Troubleshooting Error Messages

    Troubleshooting Error Messages COLUMN HEATER EXCEEDS SAFE TEMPERATURE This error occurs when the column heater temperature is higher than the maximum allowed. This error may occur if the ICS-1100 is operating in an extreme environment (greater than 40 C (104 F)).

  • Page 70: Degas Calibration Failed

    2. If calibration still fails, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance. HARDWARE NOT PRESENT This error indicates a problem in the ICS-1100 electronics. To troubleshoot: Contact Dionex for assistance. The ICS-1100 electronics components cannot be serviced by the user.

  • Page 71: Load/Inject Valve Error

    4 • Troubleshooting LOAD/INJECT VALVE ERROR If the injection valve fails to switch position within 1 second of being toggled, the ICS-1100 Moduleware reports an error to Chromeleon and this error message appears. To troubleshoot: 1. If a sequence is being executed, terminate the sequence by selecting Batch >...

  • Page 72: Pump Motor Lost Control

    PUMP MOTOR LOST CONTROL This error indicates a problem in the pump controller electronics. To troubleshoot: Contact Dionex for assistance. The ICS-1100 electronics components cannot be serviced by the user. PUMP PRESSURE HARDWARE ERROR This error indicates a problem in the pump controller electronics.

  • Page 73: Pump Stopped Due To Lost Usb Communication Error

    ERROR This error occurs if the ICS-1100 loses communication with Chromeleon. To troubleshoot: Verify that the USB cable is connected correctly from the ICS-1100 rear panel to the Chromeleon PC. PUMP UNDER PRESSURE If the system pressure falls below the low pressure limit, the pump stops and this error message appears.

  • Page 74: Suppressor Not Connected

    Step 5. If the problem persists, contact Dionex for assistance. SUPPRESSOR NOT CONNECTED This error occurs if you turn on the suppressor and the ICS-1100 cannot establish a connection with the suppressor. To troubleshoot: 1. Check the suppressor cable connection (see Section 5.11).

  • Page 75: Suppressor Over Power

    If the error persists, replace the suppressor (see Section 5.11). SUPPRESSOR OVER VOLTAGE This error occurs if you turn on the suppressor but the ICS-1100 cannot establish a connection with the suppressor. To troubleshoot: 1. Check the suppressor cable connection (see Section 5.11).

  • Page 76: Liquid Leaks

    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-1100. If a line is blocked, replace it (see Section 5.2).
  • Page 77 031432) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891). Replace any damaged fittings. 2. If the pressure transducer continues to leak, contact Dionex for assistance. The pressure transducer cannot be serviced by the user. •...

  • Page 78: Pump Difficult To Prime Or Loses Prime

    Empty eluent reservoir and/or no eluent connected Fill the reservoir. Make sure all connections are secure. • Eluent improperly or insufficiently degassed If the ICS-1100 does not contain a vacuum degas assembly, degas the eluent manually (see Section 3.4.2). If the ICS-1100 contains a vacuum degas assembly, check the degas settings: 1.
  • Page 79 • Liquid leaks at junction between pump head and pump casting Use the open-end wrench (P/N 014605) provided in the ICS-1100 Ship Kit (P/N 057905) to tighten the two acorn nuts that attach the pump head to the pump housing (see Figure 5-7).

  • Page 80: Pump Does Not Start

    ICS-1100 installation instructions. • Pump is turned off Turn on the pump from the ICS-1100 Control panel in Chromeleon. • Flow rate is set to 0 Set the flow rate from the ICS-1100 Control panel in Chromeleon.

  • Page 81: Erratic Flow/Pressure Reading

    4 • Troubleshooting • Flow rate is set to 0 Set the flow rate from the ICS-1100 Control panel in Chromeleon. • Eluent valve is closed Open the eluent valve from the ICS-1100 Control panel in Chromeleon. • Pump not primed...

  • Page 82: Excessive System Backpressure

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

  • Page 83: Peak "Ghosting

    Install or replace the end-line filter on the end of the deionized water line (see Section 3.4.3). • Malfunctioning injection valve or auxiliary valve 1. Rebuild the valve (see Section 5.4). 2. If the valve leak persists, contact Dionex for assistance. Doc. 065289-01 3/09...

  • Page 84: Nonreproducible Peak Height Or Retention Time

    (see Section 3.9). • Contaminated column 1. Clean the column as instructed in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 2. If cleaning is unsuccessful, replace the column. Doc. 065289-01 3/09...

  • Page 85: No Cell Response

    Background not suppressed by suppressor Verify that the suppressor is turned on and the current is set to the correct value. Refer to the suppressor manual for additional troubleshooting guidance. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). •...

  • Page 86: Baseline Noise Or Drift

    Flow system leak; erratic baseline Check all fittings and liquid lines for leaks. Tighten or, if necessary, replace all liquid line connections. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is included on the Dionex Reference Library CD-ROM (P/N 053891).

  • Page 87: Vacuum Degas Assembly Does Not Run

    Allow a longer system equilibration time (up to 2 hours) before starting operation. • Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). • Cell above or below temperature Contact Dionex for assistance.
  • Page 88 ICS-1100 Ion Chromatography System Figure 4-3. ICS-1100 Server Configuration Properties: Options 3. Verify that the Degas check box is selected. 4. Under Degas, verify that the Always Off option is not selected. If it is, select one of the following settings instead: •...

  • Page 89: Service

    5 • Service This chapter describes ICS-1100 service and repair procedures that the user can perform. All procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

  • Page 90: Chromeleon Wellness Panel Overview

    NOTE Do not open a System Wellness Control panel if the name includes “Service.pan.” These Wellness panels are reserved for use by Dionex Service Representatives. To Open the Wellness Panel 1. In the Chromeleon Browser, expand the Dionex Templates\Panels\Wellness folder. 2. Double-click ICS-1100_1600_2100_Wellness_user.pan. The Wellness Panel opens (see Figure 5-1).

  • Page 91: Calibrating The Conductivity Cell

    Calibrate the vacuum degas assembly • Calibrate the conductivity cell • Test the conductivity cell electronics, using a dummy cell • Upload calibration values from the ICS-1100 to the Chromeleon Wellness database 5.1.2 Calibrating the Conductivity Cell When to Calibrate •...
  • Page 92 ICS-1100 Ion Chromatography System 6. Disconnect the line from the suppressor port to the cell REGEN IN outlet. Direct the cell outlet line to a waste container. 7. Verify that the backpressure is at least 7 MPa (1000 psi). 8. On the Wellness Panel under Conductivity Cell Calibration, click Cell 35 °C.

  • Page 93: Calibrating The Flow Rate

    5 • Service 5.1.3 Calibrating the Flow Rate When to Calibrate If you run the ICS-1100 Operational Qualification or Performance Qualification and it fails. Items Needed • 0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715) to create 14 ± 2 MPa (2000 ± 300 psi) of backpressure (if needed) •...

  • Page 94: Calibrating The Vacuum Degas Assembly

    Calibrating the Vacuum Degas Assembly When to Calibrate • After every 6 months of use 1. Open the ICS-1100 Wellness Panel in Chromeleon (see Section 5.1.1). 2. On the Wellness Panel under Degas Calibration, select Calibrate. The degas pump runs for 90 seconds to allow a vacuum to be created.
  • Page 95 5 • Service WASTE ELUENT COND CELL PULSE DAMPER PUMP PUMP HEAD HEAD WASTE PRESS. XDUCER Figure 5-2. ICS-1100 Flow Schematic: Standard Configuration Doc. 065289-01 3/09...
  • Page 96 ICS-1100 Ion Chromatography System ERC 10 ELUENT ER3b ER3a COND CELL PULSE DAMPER PUMP PUMP HEAD HEAD WASTE PRESS. XDUCER Figure 5-3. ICS-1100 Flow Schematic: RFIC-ER Mode Doc. 065289-01 3/09...

  • Page 97: Replacing Tubing And Fittings

    5 • Service Replacing Tubing and Fittings The ICS-1100 is plumbed with the tubing and tubing assemblies listed below. Tubing Size and Type Color Used For 0.125-mm (0.005-in) ID PEEK Connection from pump pulse damper (P/N 044221) to pressure transducer 0.25-mm (0.010-in) ID PEEK...

  • Page 98: Rebuilding The Injection Valve Or Auxiliary Valve

    Refer to the warranty statement in the Dionex Terms and Conditions for more information. 1. Turn off the pump from the ICS-1100 Control panel in Chromeleon. 2. Open the ICS-1100 front door. 3. Disconnect each liquid line connected to the valve.
  • Page 99 5 • Service Figure 5-4. Injection Valve Plumbing Doc. 065289-01 3/09...

  • Page 100: Replacing An Auxiliary Valve Pod

    Refer to the warranty statement in the Dionex Terms and Conditions for more information. 1. Turn off the pump flow from the ICS-1100 Control panel in Chromeleon. 2. Open the ICS-1100 front door. 3. Disconnect each liquid line connected to the valve.
  • Page 101 5 • Service 8. Also verify that the two splines on the pod align with the matching splines inside the valve holder (see Figure 5-6). If necessary, twist the end of the pod to adjust the position of the splines. Valve Pod Valve Holder Slot (larger)

  • Page 102: Cleaning And Replacing The Pump Check Valves

    If new check valves are not available, follow the instructions for cleaning. Replacing Check Valves 1. Close the eluent valve from the ICS-1100 Control panel in Chromeleon. 2. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-1100.
  • Page 103 10. Prime the pump (see Section 5.17). 11. When the ICS-1100 is at operating pressure, check for leaks from the check valves. Tighten a check valve a little more only if it leaks. Cleaning Check Valves 1. Carefully remove the check valve cartridges from the valve housings.

  • Page 104: Replacing A Pump Piston Seal And Piston Rinse Seal

    1. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-1100. 2. Disconnect all tubing connections to the pump head. 3. Locate the open-end wrench (P/N 014605) provided in the ICS-1100 Ship Kit (P/N 057905). Use the wrench to remove the two acorn nuts (see Figure 5-7) from the pump head.
  • Page 105 5 • Service 5. Place the head (front end down) on a clean work surface and lift off the spacer to expose the piston seal (see Figure 5-8 Figure 5-9). Priming Valve Knob (P/N 055709) Outlet Check Valve Assembly (P/N 045721) O-Ring (P/N 055752) Piston Seal...
  • Page 106 ICS-1100 Ion Chromatography System 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 the shaft of the piston (near the base), tilt the piston slightly, and pull the piston away from the pump.
  • Page 107 5 • Service Removing the Piston Seal from the Head 1. Fill the head cavity with deionized water by injecting the liquid through either the piston opening or the inlet check valve. 2. Reinsert the piston approximately 3 mm (0.125) inch into the seal. 3.

  • Page 108: Replacing A Pump Piston

    ICS-1100 Ion Chromatography System Reinstalling 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 tubes aligned vertically and press the spacer into the head until it is flush with the indented surface of the head.

  • Page 109: Replacing The Waste Valve Or Priming Valve O-Ring

    A damaged O-ring causes leakage around the base of the waste valve or priming valve knob. 1. Close the eluent valve from the ICS-1100 Control panel in Chromeleon. 2. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-1100.
  • Page 110 ICS-1100 Ion Chromatography System 4. If the O-ring is removed with the valve knob in Step 3, pull the O-ring off the end of the knob (see Figure 5-11). If the O-ring is not removed with the valve knob, insert a thin object (for example, the bent end of a paper clip) into the cavity in the pump head and carefully pull out the O-ring.

  • Page 111: Replacing The Conductivity Cell

    5 • Service 5.10 Replacing the Conductivity Cell 1. Turn off the ICS-1100 power. 2. Open the front door and disconnect the tubing from the CELL IN CELL fittings (see Figure 5-12, View A). Loosen the two screws on the cell front cover.
  • Page 112 In the field next to the Download button, verify that Current is selected and then click Download to download the new value to the ICS-1100. To ensure that the new values are recorded in the ICS-1100 memory, do not turn off the ICS-1100 power for at least 1 minute after downloading.

  • Page 113: Replacing The Suppressor

    Figure 5-14. Removing the Suppressor 8. Connect the cable from the new suppressor to the ICS-1100 cable (align the pins on the two connectors and push them together). 9. Orient the suppressor with the...
  • Page 114 13. Connect the two eluent and two regenerant lines to the new suppressor. 14. Close the ICS-1100 front door. Figure 5-15. Suppressor Guidelines and Mounting Tabs on Component Panel Doc. 065289-01 3/09...

  • Page 115: Replacing The Column Heater

    5 • Service 5.12 Replacing the Column Heater 1. Turn off the ICS-1100 power. 2. Open the front door of the ICS-1100. 3. Remove the existing column heater: a. Unscrew the two thumbscrews on the heater cover (they remain attached to the cover).
  • Page 116 Download to download the new calibration values to the ICS-1100. d. To ensure the new calibration values are recorded in the ICS-1100 memory, do not turn off the ICS-1100 power for at least 1 minute after downloading the values. Doc. 065289-01 3/09...

  • Page 117: Replacing The Column Heater Heat Exchanger

    C on the injection valve. Figure 5-17. ICS-1100 Column Heater Cover Removed 7. Disconnect the heat exchanger outlet line from the guard column inlet. 8. Use an Allen wrench to remove the three screws from the heat exchanger metal plate and remove the plate (with the tubing) from the heater.

  • Page 118: Replacing The Eluent Valve

    ICS-1100 Ion Chromatography System 5.14 Replacing the Eluent Valve 1. Turn off the power to the ICS-1100. 2. Open the ICS-1100 front door. 3. To prevent an eluent leak during the valve replacement procedure, disconnect the eluent line from the reservoir cap or plug the line on the left side of the...
  • Page 119 Step Figure 5-20. Removing the Eluent Valve Mounting Plate 11. Connect the cable from the new valve (P/N 057945) to the ICS-1100 cable. Feed the cables back inside the ICS-1100. Doc. 065289-01 3/09...

  • Page 120: Replacing The Leak Sensor

    12. Align the new valve on the component panel with the liquid ports facing up and attach it with the two screws removed in Step 5. Reconnect the liquid lines. 13. Turn on the power to the ICS-1100. 14. Prime the pump (see Section 5.17). 5.15 Replacing the Leak Sensor 1.

  • Page 121: Priming The Pump

    5 • Service 7. Connect the cable from the new leak sensor (P/N 058053) to the ICS-1100 cable. 8. Feed the cables back inside the ICS-1100. Align the leak sensor with the component panel opening and fingertighten the screw. 9. Make sure the leak sensor does not touch the bottom of the drip tray.
  • Page 122 Figure 5-23. Priming the Eluent Lines 3. Open the priming valve by turning it one-quarter to one-half turn counterclockwise. 4. On the ICS-1100 Control panel in Chromeleon, click the Pump Settings button. The Pump Settings window opens (see Figure 3-5).

  • Page 123: Priming With The Prime Button

    Confirm that the waste valve is open by clicking OK when the reminder message appears. The pump will begin pumping at about 3 mL/min. 4. Continue priming the ICS-1100 until no air bubbles are exiting the pump waste line. 5. In the Pump Settings window, click Pump Off.

  • Page 124: Priming The Pump With Isopropyl Alcohol

    ICS-1100 Ion Chromatography System 5.17 Priming the Pump with Isopropyl Alcohol NOTE Prime the pump heads with isopropyl alcohol only if the standard priming procedures described Section 5.16 are unsuccessful. 1. Connect a 10-mL syringe (P/N 054578) filled with Secondary...

  • Page 125: Changing Main Power Fuses

    2. The fuse holder is part of the main power receptacle (see Figure 5-26) on the ICS-1100 rear panel. To remove the fuse holder, squeeze the tab on the top of the holder to release it and pull the holder straight out of its compartment. Figure 5-26. Main Power Fuse Holder...
  • Page 126 3. Replace the two fuses in the holder with new IEC 127 fast-blow fuses rated 3.15 amps (P/N 954745). Dionex recommends always replacing both fuses. 4. Reinsert the fuse holder into its compartment and push in until the tab clicks in place.

  • Page 127: A • Specifications

    A • Specifications A.1 Electrical Main Power 100 to 240 Vac, 50 to 60 Hz (Auto-sensing power supply; no manual voltage or frequency adjustment required) Fuses Two 3.15 amp fast-blow IEC 127 fuses (P/N 954745) A.2 Physical Dimensions Height: 56.1 cm (22.1 in) (Without Width: 22.4 cm (8.8 in) reservoir)

  • Page 128: Environmental

    ICS-1100 Ion Chromatography System A.3 Environmental Operating 4 to 40 °C (40 to 104 °F); cold room-compatible (4 °C) as long Temperature as system power remains on Operating 5% to 95% relative humidity, noncondensing Humidity Operating Pressure 35 MPa (5000 psi) maximum liquid path (tubing, valve, columns, etc.)
  • Page 129 A • Specifications Pressure Ripple <1% at 13.8 MPa (2000 psi) and 1.0 mL/min Eluent On/Off Standard feature Valve Piston Seal Dual-pump head; wash can be continuous when connected to rinse Wash solution supply • Pressure Alarm Upper limit: 0 to 35 MPa or 0 to 5000 psi in one unit (MPa or Limits psi) increments •...

  • Page 130: Eluent Regeneration

    ICS-1100 Ion Chromatography System A.6 Eluent Regeneration Eluent Optional feature; RFIC-ER Startup Kit required Regeneration • Eluents Carbonate and carbonate/bicarbonate up to 20 mM • MSA up to 34 mM Flow Rates 0.01 to 2.00 mL/min Continuous Up to 28 days or 2000 samples, typically...
  • Page 131 A • Specifications • Digital signal range: 0 to 15,000 μS Full-Scale • Output Ranges Analog signal range: 0 to 15,000 μS ±0.1 nS/cm when background conductivity is 0 to 150 μS/cm Electronic Noise ±2 nS/cm when background conductivity is 151 to 3200 μS/cm Filter Rise times from 0 to 10 s;...

  • Page 132: Conductivity Cell With Heat Exchanger

    ICS-1100 Ion Chromatography System A.8 Conductivity Cell with Heat Exchanger Cell Body Chemically inert polymeric material Cell Electrodes Passivated 316 stainless steel; compatible with MSA <1 μL Cell Volume Maximum Cell 10 MPa (1500 psi) Operating Pressure Heat Exchanger Inert, tortuous path for low axial dispersion Operating 30 to 55 ºC (86 to 130 ºF);...

  • Page 133: Column Heater (Optional)

    A • Specifications A.12 Column Heater (Optional) Operating 30 to 60 °C (86 to 140 °F); minimum 5 °C above ambient Temperature temperature. Settable range is equal to working range. Temperature ±0.5 °C at sensor Stability Temperature ±0.5 °C at sensor, at 40 °C Accuracy Maximum 250 mm analytical column with 50 mm guard column...

  • Page 134: Suppressors

    ICS-1100 Ion Chromatography System A.13 Suppressors Chemical 2 mm and 4 mm anion and cation, membrane suppression bed types Suppression Displacement 2 mm and 4 mm anion and cation, membrane suppression bed types Chemical Regeneration • Electrolytic Self-Regenerating: 2 mm and 4 mm anion and cation; both ™...

  • Page 135: Autosampler

    AMMS ICE 300 (4 mm): <50 μL AMMS ICE 300 (2 mm): <15 μL Anion AES: <35 μL Cation AES: <35 μL A.14 Autosampler Automation Dionex AS, AS-DV, or AS-HV Autosampler (or third-party Using autosampler) Autosampler Sequential/ May be available; depends on autosampler capabilities...
  • Page 136 ICS-1100 Ion Chromatography System System Wellness Standard feature and Predictive Performance Data Trending Numerical device parameters can be plotted Plots • Virtual Column Evaluation mode: Standard feature • Simulator Isocratic and gradient modes: Optional features Application Standard feature Templates Automation...
  • Page 137 A • Specifications Storage of Factory, current, and previous calibration values are stored; the user System can reset current values to factory or previous values Calibration Settings Customized Standard feature; unlimited report workbooks Reporting Automated Detailed, comprehensive qualification reports System Qualification Doc.
  • Page 138 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 139: B • Ttl And Relay Control

    B • TTL and Relay Control B.1 TTL and Relay Connections A 12-pin connector strip for TTL/relay control is located on the ICS-1100 rear panel. The connector provides two relay outputs, two TTL outputs, and four TTL inputs (see Figure B-1).
  • Page 140 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-1100 rear panel. Doc. 065289-01 3/09...

  • Page 141: Selecting Ttl Input Functions And Control Types

    B • TTL and Relay Control c. Connect the wires from the ICS-1100 connector plug to the TTL or relay connector pins on the other module(s). Additional connector plugs are provided with other Dionex modules. NOTE Check the polarity of each connection. Connect signal wires to signal (+) pins and ground wires to ground (-) pins.
  • Page 142 Normal Edge the output signals provided by Dionex modules. If the device connected to the ICS-1100 does not send a normal edge signal, select the appropriate control type. Refer to the documentation provided with the controlling device and the information below to select the correct type.

  • Page 143: Controlling Ttl And Relay Outputs

    B.2 Controlling TTL and Relay Outputs The ICS-1100 provides two TTL outputs and two relay contacts for control of functions in external devices, such as an integrator or 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.
  • Page 144 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 145: C • Reordering Information

    C • Reordering Information Part Number Item Reservoirs 046548 2-L plastic reservoir assembly (includes stopper and cap) 039164 4-L plastic reservoir assembly (includes stopper and cap) Pump 057937 Primary pump head assembly 057938 Secondary pump head assembly 045721 Outlet check valve assembly, 10-32 045722 Inlet check valve assembly, 1/4-28 045994...
  • Page 146 Microbore tubing kit Relay/TTL 923686 12-position connector plug 043598 Twisted pair of wires RFIC-ER Kits 069570 RFIC-ER Anion Startup Kit, ICS-1100/ICS-1600 067791 RFIC-ER Anion Consumables Kit, ICS-1100/ICS-1600 069569 RFIC-ER Cation Startup Kit, ICS-1100/ICS-1600 067792 RFIC-ER Cation Consumables Kit, ICS-1100/ICS-1600 070061...
  • Page 147 C • Reordering Information Part Number Item Preventive Maintenance Kits 057954 ICS-1100 Preventive Maintenance Kit 060581 AS Preventive Maintenance Kit 055647 AS-DV Preventive Maintenance Kit Doc. 065289-01 3/09...
  • Page 148 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 149: D • Faq

    D • FAQ D.1 How do I hook up an autosampler? For instructions on how to connect the ICS-1100 to an autosampler, refer to the ICS-1100 installation instructions. Also refer to the autosampler operator’s manuals, which are included on the Dionex Reference Library CD-ROM (P/N 053891).

  • Page 150: When Should I Remake Eluents

    In Chromeleon, select File > Export/Backup. Back up the data and indicate the backup source. D.10 How do I shut off the system? In Chromeleon, click the System Shutdown button on the ICS-1100 Control panel. On the instrument, turn off the power switch on the rear panel (see Figure 2-6).

  • Page 151: How Do I Clean A Column

    Section 5.1.2 for calibration instructions. • Section 4.13 for additional troubleshooting information. D.15 How do I configure and operate the auxiliary valve? See Installing the ICS-1100/ICS-1600/ICS-2100 Auxiliary Valve (Document No. 065288), provided in the Auxiliary Valve Kit. Doc. 065289-01 3/09...
  • Page 152 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...

  • Page 153: E • Glossary

    E • Glossary Analytical Column Synonymous with Separator Column. Band Spreading The broadening of the sample band as it travels through the column. Band spreading can also occur in the injection valve, detector cell, and interconnecting tubing. Calibration Curve A graph showing detector response in peak height or area versus analyte concentration.
  • Page 154 ICS-1100 Ion Chromatography System Cell Constant (k) A factor determined experimentally by measuring the conductance (G) of a standard solution of known equivalent conductivity (k). κ G ⁄ The value of k depends upon the surface area of, and distance between, the electrode faces in the conductivity detector cell.
  • Page 155 E • Glossary of relatively clean sample. This allows large volumes of sample to be injected, lowering concentration detection limits. Conductivity A measure of the ease with which electrical current flows through a liquid contained between two opposite charged electrodes. Conductivity is a characteristic of ions in solution.
  • Page 156 ICS-1100 Ion Chromatography System Packing The material that fills a chromatographic column; usually a resin or silica-based material. Pellicular Resin A resin with a solid, nonporous core coated with a thin layer of more porous material. The exchange sites of pellicular ion exchange resins are located only on the surface layer of the bead.
  • Page 157 E • Glossary Siemens (S) Unit measure of conductance; the reciprocal of the electrical resistance of a solution. Suppressor A device used to minimize eluent conductivity and convert sample species to a common form, thus increasing detection sensitivity. Temperature Coefficient The percent of change in the conductivity of a solution with a 1 C change in temperature.
  • Page 158 ICS-1100 Ion Chromatography System Doc. 065289-01 3/09...
  • Page 159 Index Does not switch position, 63 Installation instructions, 32 Air particulate samples, 48 Leaking, 67 Alarm conditions, 59 – 65 Maintenance, yearly, 56 See also Error messages Passages blocked, 72 Ambient temperature, 76 Rebuilding, 88 Analog output, 142 Reordering, 147 Connector, 18 Replacing the mechanical part (pod), 88, Anion separations, 47...
  • Page 160 ICS-1100 Ion Chromatography System Cation separations, 47 Conductivity cell, 15, 34 Cell Calibrating, 81 See Conductivity cell Calibration constant, 102 Cell calibration, 81 High cell output, 75 Check valves Leaking, 67 Cleaning procedure, 92 – 93 No response, 75 Replacement procedure, 92 – 93...
  • Page 161 Temperature compensation, 132 Degas calibration failed, 60 Diagnostics, 79 Hardware not present, 60 Dimensions, 129 Leak sensor wet, 60 Dionex Load/inject valve error, 61 Contacting, 79 Option not installed, 61 Direct software control, 25 Pump motor lost control, 62 Drip tray, 15...
  • Page 162 ICS-1100 Ion Chromatography System Leak sensor wet alarm, 60 Replacement, 110 Ghosting, 73 Leaks Guard column, 16 Auxiliary valve, 67 Cell, 67 Fittings, 66 Injection valve, 67 Liquid, 66 Hardware not present error, 60 Pressure transducer, 67 Heater, column, 33...
  • Page 163 Index PGM file See Programs Offsetting background conductivity, 46 Physical specifications Operating features, 11 Decibel level, 129 Operating humidity, 130 Dimensions, 129 Operating ranges Weight, 129 Cell heater, 15 Piston seals Column heater, 16 Replacement procedure, 94 – 95 Flow rate, 15 Pistons Operating temperature, 130 Replacement procedure, 98...
  • Page 164 ICS-1100 Ion Chromatography System Programs (Chromeleon), 25 Controlling an autosampler, 51 Rear panel, 18 Pulse damper, 20, 22, 30 Analog output connector, 18 Pump, 28 Power receptacle, 19 Flow rate, 15 USB connections, 18 Leaks, 66 Rebuilding the auxiliary valve, 88...
  • Page 165 Index Sample processing, 38, 52 – 53 Waste valve O-ring replacement, 99 Batch, 38, 53 Software control, 24 Manual, 38, 52 Modes of, 25 With Chromeleon, 52 – 53 Software specifications Samples Application templates, 137 Collecting and storing, 47 Automated procedure wizards, 137 Diluting, 48 Automation support for third-party Filtering, 47...
  • Page 166 ICS-1100 Ion Chromatography System Replacement procedure, 103 Excessive backpressure, 72 Suppressor alarms Flow rate, 70 Suppressor not connected, 64 High cell output, 75 Suppressor over current, 64 Liquid leaks, 66 Suppressor over power, 65 No cell response, 75 Suppressor stopped for zero flow rate, 65...
  • Page 167 Index See Injection valve See Waste valve Warranty, voiding, 79, 88, 90 Waste lines Blocked, 66 Waste valve, 29 Opening, 29, 94 O-ring replacement procedure, 99 Water samples, 48 Weekly maintenance, 55 Weight, 129 Wellness, 25 Wellness panel, 79 Yearly maintenance, 56 Index-9 Doc.
  • Page 168 ICS-1100 Ion Chromatography System Index-10 Doc. 065289-01 3/09...