ICS-2100 Ion Chromatography System Operator’s Manual Document No.
©2009 by Dionex Corporation All rights reserved worldwide. Printed in the United States of America. This publication is protected by federal copyright law.
Contents 1 • Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 1.1 Introduction to Ion Chromatography (IC) . . . . . . . . . . . . . . . . . . . . . . . . 1 1.2 Overview of the ICS-2100 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 1.3 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.3.1 1.4 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . .
ICS-2100 Ion Chromatography System 2.4.2 Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34 2.4.3 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34 2.4.4 Eluent Generator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37 2.4.5 Auxiliary Power Supply (Optional) . . . . . . . . . . . . . . . . . . . . . .42 2.4.6 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Contents 3.9 Prepare Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60 3.9.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . . . 60 3.9.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 3.9.3 Diluting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 3.10 Loading and Injecting Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62 3.10.
ICS-2100 Ion Chromatography System 4.10 Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . . .94 4.11 Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . . . .94 4.12 No Cell Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .94 4.13 High Cell Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .95 4.14 Baseline Noise or Drift . . . . . . . . . . . . . . . . . . . . . . . . .
Contents 5.12 Replacing the Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131 5.13 Replacing the Column Heater Heat Exchanger . . . . . . . . . . . . . . . . . . 134 5.14 Replacing the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135 5.15 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137 5.16 Priming the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138 5.16.
ICS-2100 Ion Chromatography System 5.23.2 Removing the CR-TC and Reinstalling it in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . .188 5.23.3 Removing the EPM and Reinstalling it in the New EGC Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . .190 5.23.4 Installing the New EGC Holder Without a CR-TC or EPM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .192 5.23.5 Reinstalling the EluGen Cartridge . . . . . . . . . . . . . . .
Contents B • Touch Screen Operation. . . . . . . . . . . . . . . . . . . . . . . . . . . 207 B.1 Using the Touch Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 207 B.2 Using the Touch Screen with Chromeleon . . . . . . . . . . . . . . . . . . . . . 210 B.3 Overview of ICS-2100 Touch Screen Pages . . . . . . . . . . . . . . . . . . . . 211 B.4 Home Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 212 B.4.
ICS-2100 Ion Chromatography System B.9 B.8.4 Monitoring the EluGen Cartridge Life . . . . . . . . . . . . . . . . . .228 B.8.5 Controlling the CR-TC Power . . . . . . . . . . . . . . . . . . . . . . . . .229 Suppressor Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .230 B.10 Detector Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .231 B.10.1 Setting the Data Rise Time . . . . . . . . . . . . . . . . . . . . . . . . .
Contents E.4 How do I adjust retention times? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255 E.5 When should I remake standards? . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255 E.6 When should I replace the eluent generator cartridge? . . . . . . . . . . . 256 E.7 How do I start Chromeleon? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256 E.8 How do I delete data? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256 E.
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1 • Introduction 1.1 Introduction to Ion Chromatography (IC) The Dionex ICS-2100 Ion Chromatography System (ICS-2100) performs ion analyses using suppressed or non-suppressed conductivity detection. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system. Before running a sample, the ion chromatography system is calibrated using a standard solution.
ICS-2100 Ion Chromatography System A typical IC analysis consists of six stages (see Figure 1-1). 6. Data Analysis Conductivity Cell 5. Detection Suppressor 1. Eluent Delivery 4. Suppression Eluent Separator Column 3. Separation Pump Guard Column Injection Valve Sample 2. Sample Injection Sample Loop Figure 1-1. Ion Analysis Process 1. Eluent Delivery • • Eluent, a liquid that helps to separate the sample ions, carries the sample through the ion chromatography system.
1 • Introduction • The pump pushes the eluent and sample through the guard and separator columns (chemically-inert tubes packed with a polymeric resin). The guard column removes contaminants that might poison the separator column. 3. Separation • As the eluent and sample are pumped through the separator column, the sample ions are separated. In the ICS-2100, the mode of separation is called ion exchange.
ICS-2100 Ion Chromatography System 1.2 Overview of the ICS-2100 The ICS-2100 is an integrated ion chromatography system containing an eluent generator, pump, injection valve, column heater, and conductivity detector. Other system components, including a guard column, separator column, and suppressor vary, depending on the analyses to be performed. The ICS-2100 can be configured with a vacuum degas assembly for online eluent degassing.
1 • Introduction 1.3 About This Manual The electronic version (i.e., PDF file) of this 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.
ICS-2100 Ion Chromatography System Appendix E FAQ Provides answers to frequently asked questions about ICS2100 operation. Appendix F Glossary Defines terms commonly used in ion analysis. 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.
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.
ICS-2100 Ion Chromatography System 1.4 Safety and Regulatory Information The ICS-2100 was manufactured by Dionex Corporation at the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The ICS-2100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. If there is a question regarding appropriate usage, contact Dionex at 1-800-346-6390 before proceeding. Outside the United States, call the nearest Dionex office. 1.4.
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.
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2 • Features This chapter describes key ICS-2100 features and introduces the Chromeleon user interface. 2.1 Operating Features 2.1.1 Front Panel Figure 2-1 illustrates the front panel of the ICS-2100. Injection Port Touch Screen Power LED Injection Port The sample to be analyzed can be injected manually into the injection port, using a syringe. For automated sample injection, the ICS-2100 must be connected to an autosampler. For more information about sample injection, see Section 3.10.
ICS-2100 Ion Chromatography System Summary of Touch Screen Operation Status Field Edit Field Command Button (selected) Command Button (unselected) Figure 2-2. ICS-2100 Touch Screen Home Page NOTE To adjust the screen contrast, open the front door and adjust the knurled knob under the screen (see Figure 2-8). • • • Edit fields and command buttons have blue text on a shaded background. Fields that display status information are not shaded.
2 • Features • • Selecting a command button changes the button’s appearance to white text on a dark backgound (for example, ). Touching an edit field (for example, ) opens a page with a number keypad (see Figure 2-3). Use the keypad to enter the desired numerical value for the field and then touch the ENTER button. Touch CANCEL to cancel the entry and return to the previous page. Touch a number to enter the value. Touch ENTER to confirm the entry and return to the previous page. Figure 2-3.
ICS-2100 Ion Chromatography System • Touching the page name (for example, ) in the bottom right corner opens a menu of pages (see Figure 2-4). Touch a page name to display the page. Figure 2-4. ICS-2100 Touch Screen Menu of Pages • 14 Touching a page name on the menu of pages displays the selected page. For example, touching SUPPRESSOR displays the Doc.
2 • Features SUPPRESSOR page (see Figure 2-5). See Appendix B for details about each touch screen page. Touch to select a different option. Touch to return to the Home page. Figure 2-5. Suppressor Page • Touching returns you to the HOME page. • Touching opens a list of options (see Figure 2-6). Touch an option to select it. Figure 2-6. Suppressor Page: Selecting an Option Doc.
ICS-2100 Ion Chromatography System 2.1.2 Top Cover Figure 2-7 illustrates the top cover of the ICS-2100. EluGen Cartridge and Holder Second EluGen Cartridge or Reservoir Area EGC, EPM, CR-TC, and Auxiliary Power Supply Connectors EluGen Cartridge and Reservoir Storage The top cover holds one or two EluGen® cartridges and up to two 2-L plastic reservoirs (P/N 044129) or one 4-L plastic reservoir (P/N 039164).
2 • Features EluGen cartridge holder, is connected to the EGC-2 connector. However, the connections can be reversed, if desired. EGC Service Area The EGC service area holds the cartridge during installation and replacement. For details, refer to the ICS-2100 installation instructions. Doc.
ICS-2100 Ion Chromatography System 2.1.3 Component Panel Figure 2-8 shows the user-accessible components installed on the component panel behind the ICS-2100 front door.
2 • Features Pressure Transducer The pressure transducer measures the system backpressure. Leak Sensor The leak sensor is installed in the drip tray at the bottom of the component panel. If liquid accumulates in the tray, an error message is logged in the Chromeleon Audit Trail and displayed on the LCD touch screen. Pump Heads The ICS-2100 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.
ICS-2100 Ion Chromatography System Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an AES® Atlas Electrolytic Suppressor, SRS® Self-Regenerating Suppressor, or MMS™ MicroMembrane™ Suppressor can be used with the ICS-2100. See Section 2.4.9 for details about the suppressor.
2 • Features 2.1.4 Rear Panel Figure 2-9 illustrates the ICS-2100 rear panel. Tubing Clips Analog Output Connector Power Switch USB Connectors 12 TTL and Relay Connector Strip Main Power Receptacle Waste Lines Figure 2-9. ICS-2100 Rear Panel Analog Output Connector The analog output connector outputs conductivity data (as a 0 to 1 V signal) to an integrator or recording device. For connection and setup information, refer to the ICS-2100 installation instructions.
ICS-2100 Ion Chromatography System TTL and Relay Connector The TTL and Relay connector strip provides two TTL outputs, two relay outputs, and four TTL inputs. The outputs can be used to control functions in other TTL- or relay-controllable devices. The inputs can be used to switch the injection valve position, turn on the pump, perform an autozero command, and send an event mark to the analog output. See Section C.1 for connection instructions.
2 • Features 2.2 Flow Schematics • • • Figure 2-10 illustrates the liquid flow path when the components required for producing KOH, LiOH, MSA, or NaOH eluent are installed. The required components include the corresponding type of EluGen cartridge and a CRTC. Figure 2-11 illustrates the liquid flow path when the components required for producing carbonate/bicarbonate eluent are installed.
ICS-2100 Ion Chromatography System To the pump Degas In EGC Vent 6 EGC II KOH, LiOH, MSA, or NaOH 1 Deionized Water Inlet Outlet Regen In 8 Regen Out Eluent 7 EGC Degas Eluent Out 16 CR-TC 17 From the pulse damper Degas In To the inject valve port P(2) Column Heater Degas Out 13 Suppressor Cell Out 15 Eluent Out Regen In 14 Heat Exchanger Conductivity Cell Cell In 5 Pulse Damper Valve 10 W L Press. 4 Xducer.
2 • Features Flow Description for KOH, LiOH, MSA, or NaOH Eluent Generation Refer to Figure 2-10 for the flow path number locations. • Deionized water from the reservoirn flows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
ICS-2100 Ion Chromatography System To the pump Degas In EGC Vent 6 EGC II K2CO3 1 Deionized Water Inlet Outlet Eluent Out 8 7 Regen Out EGC Degas Eluent In 18 EPM Regen In 17 Degas In 14 Suppressor Cell Out 16 Eluent Out Regen In 15 Heat Exchanger Regen Out Eluent In Degas Out Conductivity Cell Cell In Column Heater 9 Pulse Damper Valve L Press. 4 Xducer.
2 • Features Flow Description for Carbonate/Bicarbonate Eluent Generation Refer to Figure 2-11 for the flow path number locations. • Deionized water from the reservoirn flows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
ICS-2100 Ion Chromatography System To the pump Degas In EGC Vent 6 EGC II K2CO3 1 Deionized Water Inlet Outlet 7 EGC Degas 16 Degas In 13 Suppressor Cell Out 15 Eluent Out Regen In 14 Heat Exchanger Conductivity Cell Cell In Regen Out Eluent In Degas Out Column Heater 8 11 L 10 W L Separator Pulse Damper Valve S Press. 4 Xducer.
2 • Features Flow Description for Carbonate Eluent Generation Refer to Figure 2-12 for the flow path number locations. • Deionized water from the reservoirnflows first through the pump degas assembly and then through the eluent valveo to the pumpp . The water is then pushed through the pressure transducerq, which measures the system pressure. From there, the water flows through a pulse damperr , which smooths minor pressure variations from the pump to minimize baseline noise.
ICS-2100 Ion Chromatography System 2.3 Chromeleon and Chromeleon Xpress The ICS-2100 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. 2.3.
2 • Features • • • 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 if the ICS-2100 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: • • 2.3.
ICS-2100 Ion Chromatography System 2.4 System Component Details This section provides details about ICS-2100 system components, including the vacuum degas assembly, pump, eluent generator, injection valve, column heater, suppressor, auxiliary power supply, and conductivity cell. 2.4.1 Vacuum Degas Assembly (Optional) The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user.
2 • Features Select the Options tab (see Figure 2-14). . Figure 2-14. Server Configuration Properties: Degas Options Degas Options • Always Off: The degas pump is always off. • Always On: The degas pump is always on. This setting is for test purposes by a Dionex Service Representative. Do not use this setting for routine operation. • Cycle: The degas pump cycles on and off according to the times specified in the Cycle On and Off fields.
ICS-2100 Ion Chromatography System 2.4.2 Eluent Valve The eluent valve controls the flow from the eluent reservoir. The valve opens automatically when the pump is started and closes when the pump is turned off. The valve can also be opened and closed manually from the Chromeleon Control panel (see Section 2.3.1) or the touch screen PUMP page (see Section B.7). This lets you perform service procedures on pump components without eluent leaks occurring. Figure 2-15. Eluent Valve 2.4.
2 • Features Outlet Check Valve Secondary Pump Head Primary Pump Head Waste Valve Priming Valve Inlet Check Valve Pressure Transducer Figure 2-16. ICS-2100 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 2-16). To open the waste valve, turn the knob one-quarter to one-half turn counterclockwise.
ICS-2100 Ion Chromatography System Pressure Transducer Flow exiting the secondary pump head is directed to the pressure transducer (see Figure 2-16), which measures the system pressure. Pressure readings indicate that the pumping system is delivering smooth, accurate flow. Pressure readings can be monitored from the Chromeleon Control panel or the touch screen HOME page. The system pressure should remain consistent (no more than a 3% difference from one pressure reading to the next).
2 • Features 2.4.4 Eluent Generator The eluent generator produces high-purity eluents online, using only deionized water as the carrier. The eluent generator consists of an eluent generator cartridge (EGC) that generates the eluent, and a high-pressure degas tubing assembly that removes electrolysis gases created during eluent generation. NOTE A gas separator waste tube (P/N 045460) should be connected to the system waste line during installation (see Section B.10.1).
ICS-2100 Ion Chromatography System You can select the concentration of eluent to be generated from either the Chromeleon Control panel or from the touch screen HOME page (see Section B.4). The allowable eluent concentration depends on several factors: the flow rate, suppressor type, EluGen cartridge type, and cartridge configuration. For details, refer to Table 2-2 and Table 2-3. Single-Cartridge Configuration In the single-cartridge configuration, the ICS-2100 contains one EluGen cartridge.
2 • Features details, refer to the EluGen cartridge manual. Cartridge manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). EluGen Cartridges Eluent Concentration Range Comment K2CO3/EPM Electrolytic pH Modifier 0.1 to 15 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 2.0 mL/min flow X = 15/flow The total of the eluent concentrations from both the EluGen cartridge and the EPM must not exceed the specified range. The EPM concentration must not exceed 10 mM.
ICS-2100 Ion Chromatography System Tubing and fittings for plumbing the cartridge, degas assembly, CR-TC, and EPM are included with the holder. For connection instructions, refer to the ICS-2100 installation instructions. Backpressure Coil (Optional) The EluGen cartridge requires at least 14 MPa (2000 psi) of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal.
2 • Features EPM Electrolytic pH Modifier and EGC CO3 Mixer The EGC II K2CO3 EluGen Cartridge can be used with an EPM Electrolytic pH Modifier (P/N 063175) (see Figure 2-17) and an EGC CO3 Mixer (P/N 061686) to produce a carbonate/ bicarbonate mixture. The carbonate/bicarbonate mixture is used with carbonatebased IonPac columns for anion exchange separations. EluGen Cartridge EPM Figure 2-17.
ICS-2100 Ion Chromatography System the EPM to achieve the desired 3.50 mM K2CO3/1.00 mM KHCO3 mixture. 2.4.5 Auxiliary Power Supply (Optional) The EGC-2 power supply can be configured as an auxiliary power supply for the operation of an electrolytic device such as a water purifier. The power supply operates in constant current mode and can be configured from 0 to 200 mA, with a maximum voltage of 35 V. 2.4.6 Injection Valve The injection valve (P/N 057968) is a six-port, electrically-activated valve.
2 • Features syringe or automated sampler line (if installed), through the valve, and into the sample loop. Excess sample flows out to waste. • In the Inject position, sample is swept to the column for analysis. Eluent flows from the pump, through the sample loop, and on to the column, carrying the contents of the sample loop with it. Section 3.10 describes how to inject samples. Figure 2-19 shows the injection valve connections.
ICS-2100 Ion Chromatography System 2.4.7 Auxiliary Valve (Optional) The auxiliary valve is a high-pressure Rheodyne valve. The electricallyactivated, 2-position PEEK valve is offered in both 6-port and 10-port models (6-Port Valve Kit, P/N 069472; 10-Port Valve Kit, P/N 069473).
2 • Features 2.4.8 Column Heater 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. A thermistor mounted in the heater block monitors the temperature. Setting the temperature to 0 °C turns off the column heater.
ICS-2100 Ion Chromatography System 2.4.9 Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either an Atlas Electrolytic Suppressor, Self-Regenerating Suppressor, or MicroMembrane Suppressor can be used with the ICS-2100. For details about any of the suppressors or for information about selecting a suppressor for your application, refer to the suppressor manuals.
2 • Features DS6 Heated Conductivity Cell Components The cell front cover provides CELL IN and CELL OUT fittings for connecting the cell to the suppressor (see Figure 2-8). The remaining cell components are mounted behind the component panel. To replace, the cell remove the screws on the cell front cover and pull the entire cell assembly out through the component panel. See Section 5.10 for cell replacement instructions. Doc.
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3 • Operation and Maintenance This chapter describes routine operating and maintenance procedures for the ICS2100. The ICS-2100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of the ICS-2100 in a manner not specified by Dionex may result in personal injury. 3.1 Operation Overview Figure 3-1 illustrates the basic steps for routine operation of the ICS-2100.
ICS-2100 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.
3 • Operation and Maintenance 3.2 Turning On the System Power Press the power switch on the ICS2100 rear panel (see Figure 3-3) to turn on the system power. Table 3-4 shows the ICS-2100 conditions at power-up. Power Switch Also turn on the power to the computer and the autosampler (if used). Figure 3-3. ICS-2100 Rear Panel Feature Power-Up Condition Pump Injection valve Cell Suppressor Cell heater Off Load position Reading current value Off* Set to the last value used.
ICS-2100 Ion Chromatography System 3.3 Connecting to Chromeleon NOTE If you are beginning operation of an ICS-2100 that has not been configured in a timebase, refer to the ICS-2100 installation instructions for Chromeleon setup instructions. 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 .
3 • Operation and Maintenance Figure 3-4. ICS-2100 Control Panel on the Chromeleon Panel Tabset Doc.
ICS-2100 Ion Chromatography System 3.4 Set Up the Eluent Reservoir The ICS-2100 does not require pressurized reservoirs. However, if eluent is manually degassed or is sensitive to contamination, Dionex recommends pressurizing the reservoir with helium or nitrogen. The air regulator accessory bracket and other items needed for pressurizing the eluent reservoir must be ordered separately (P/N 060054). For more information, refer to the ICS-2100 installation instructions. 3.4.
3 • Operation and Maintenance In order for the level displayed in the Eluent Bottle box and gauge to be accurate, you must enter the level when the reservoir is filled. The ICS-2100 does not automatically detect when the reservoir is filled, nor when it is empty. Enter the volume of liquid in the reservoir Note: The Eluent Level field is updated as the liquid is depleted. Figure 3-5.
ICS-2100 Ion Chromatography System See Section B.6 for details about the STATUS PAGE. Figure 3-7. Status Page 3.4.4 Connect the Reservoir If it is not already connected, connect the ELUENT BOTTLE OUT line from the reservoir cap to the ELUENT IN line, which extends from the plumbing and cable chase on the top of the ICS-2100 (see Figure 3-8). ELUENT BOTTLE OUT ELUENT IN Figure 3-8. Reservoir Connections 56 Doc.
3 • Operation and Maintenance 3.5 Check All Connections 1. Make sure the eluent reservoir is filled and the tubing connecting the reservoir to the ICS-2100 tubing is securely connected (see Figure 3-8). 2. Make sure the eluent generator electrical cable (blue) is connected to the EGC-1 connector. 3. Make sure the CR-TC electrical cable (black) is connected to the CR-TC connector. 3.
ICS-2100 Ion Chromatography System reminder message appears. The pump will begin pumping at approximately 3 mL/min. 4. Continue priming the ICS-2100 until all air and previous eluent are purged and no air bubbles are exiting the waste line. 5. Press Pump Off. 6. Close the waste valve. Do not overtighten. The pump is now ready for operation. 3.7 Set System Operating Conditions NOTE This section is an overview of the steps needed to start up the system and begin running samples.
3 • Operation and Maintenance 5. Verify that the column heater is set to the correct value. Automatically Turning on the Suppressor and Eluent Generator You can set up the ICS-2100 to turn on the suppressor, eluent generator, and CR-TC automatically when the pump is turned on. To do this: • • For the suppressor, select the Automatically turn on with pump option from the SUPPRESSOR page. For the eluent generator and CR-TC, select the option from the ELUENT GENERATOR page.
ICS-2100 Ion Chromatography System • If the pressure is too high, there may be a restriction in the system plumbing. See Section 4.7 for troubleshooting information. 5. Verify that the baseline conductivity is at the expected reading for your application and is stable. 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. See Section 4.12 for troubleshooting information if the conductivity is too high. See Section 4.
3 • Operation and Maintenance Analyze samples containing nitrite or sulfite as soon as possible. Nitrite oxidizes to nitrate, and sulfite to sulfate, thus increasing the measured concentrations of these ions in the sample. In general, samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant changes in anion concentrations. 3.9.
ICS-2100 Ion Chromatography System 3.10 Loading and Injecting Samples NOTE Samples can be injected using either the standard injection valve or the optional auxiliary valve, if installed. For more information, see the Chromeleon Help or user’s manual. The two techniques for loading samples into the sample loop are: (1) with an autosampler or (2) with a syringe or vacuum syringe through the injection port on the ICS-2100 front door.
3 • Operation and Maintenance Setup for an AS-HV Autosampler For setup information for the AS-HV Autosampler, see the AS-HV Autosampler Operator’s Manual (Document No. 065125). The manual is provided on the Dionex Reference Library CD-ROM (P/N 053891). 3.10.1 Loading Samples with a Syringe 1. Make sure the injection port on the ICS-2100 front door (see Figure 2-1) is connected to sample port S (5) on the injection valve (see Figure 3-10). Figure 3-10. Injection Valve Connections 2.
ICS-2100 Ion Chromatography System 3.10.2 Loading Samples with a Vacuum Syringe 1. Disconnect the waste line from port W (6) of the injection valve (see Figure 3-10) and attach a shorter line: 25 to 30 cm (10 to 12 inches) of PEEK or Teflon® tubing. 2. Place the free end of the line into the sample. 3. Verify that the injection valve is in the Load position. 4.
3 • Operation and Maintenance 3.10.4 Injecting Samples After loading the sample in the sample loop, use one of the following methods to switch the injection valve to the Inject position: • • Manually: Click the Inject button on the Chromeleon Control panel (see Figure 3-4) or touch the Inject button on the HOME page. Automatically: Include the Inject command in a Chromeleon program. (If necessary, refer to the Chromeleon Help or user manual for assistance.) 3.
ICS-2100 Ion Chromatography System 4. Click the Autozero button on the Control panel or the touch screen HOME page. 5. Inject the sample (see Section 3.10.4). 6. In Chromeleon, monitor the chromatogram on the Control panel and select Control > Acquisition Off when sample data is collected. NOTE Data from Chromeleon manual processing is saved in the MANUAL sequence folder under the local datasource. This data is overwritten each time a new manual sample is processed.
3 • Operation and Maintenance Summary of Automatic Sample Processing 1. Complete the instructions in Section 3.2 through Section 3.8 to prepare the ICS-2100 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. Autosampler manuals are provided on the Dionex Reference Library CD-ROM (P/N 053891). 3.
ICS-2100 Ion Chromatography System 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.
3 • Operation and Maintenance 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). • Check the end-line filter (P/N 045987) and change if needed. When new, endline filters are pure white. If the system is in continuous operation, change the end-line filter weekly, or whenever it becomes discolored.
ICS-2100 Ion Chromatography System 70 Doc.
4 • Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the ICS-2100. 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. A systematic troubleshooting approach is the most effective way to determine the root cause.
ICS-2100 Ion Chromatography System The table below lists the most frequently observed ICS-2100 error messages. For troubleshooting assistance, refer to the page indicated in the table.
4 • Troubleshooting Alarms and Error Conditions See Option not installed page 81 Pressure slope calibration error page 81 Pump motor lost control page 81 Pump over pressure page 82 Pump pressure hardware error page 82 Pump stopped due to lost USB communication error page 82 Pump under pressure page 83 Second valve error page 83 Suppressor not connected page 84 Suppressor over current page 84 Suppressor over power page 85 Suppressor over voltage page 85 Suppressor stopped for zero
ICS-2100 Ion Chromatography System 4.2 Troubleshooting Error Messages AUXILIARY POWER SUPPLY DISCONNECTED This error occurs when the auxiliary power supply is configured as active, but no device is connected. To troubleshoot: 1. Connect the cable for the auxiliary device to the EGC-2 power supply connector. 2. If there is no auxiliary device, open the Chromeleon Server Configuration program and remove this option from the ICS-2100 timebase.
4 • Troubleshooting AUXILIARY POWER SUPPLY OVER VOLTAGE This error occurs when the device connected to the auxiliary power supply is attempting to operate at a higher voltage than is allowed (35 V). To troubleshoot: 1. Check the cable connecting the device to the power supply for damage or a faulty connection. 2. If the error persists, refer to the manual provided by the device vendor for assistance.
ICS-2100 Ion Chromatography System COLUMN HEATER OPEN CIRCUIT This error occurs when the column heater is unplugged from the component panel. To troubleshoot: 1. Check that the column heater is plugged into the component panel. 2. If the error persists, the column heater may be faulty. Replace the column heater (see Section 5.12). COLUMN HEATER SHORT CIRCUIT This error occurs when there is a short circuit on the thermistor input used to measure the column heater temperature.
4 • Troubleshooting CR-TC STOPPED FOR ZERO FLOW RATE This message appears when you click the Shutdown button on the Chromeleon Control panel. The message also appears when you turn off the pump flow while the EGC current (and CR-TC) are on. The CR-TC is automatically turned off. To troubleshoot: If the pump stopped unexpectedly, see Section 4.6 for pump troubleshooting information. DEGAS CALIBRATION FAILED This error occurs when the degas vacuum does not reach the expected level during calibration.
ICS-2100 Ion Chromatography System EGC-1 CALIBRATION ERROR EGC-2 CALIBRATION ERROR This error occurs if the measured current is outside the expected range when running the eluent generator calibration procedure. To troubleshoot: 1. Review the procedure to verify that you set up the ICS-2100 correctly and then rerun the calibration. 2. If the error message reappears, contact Dionex for assistance.
4 • Troubleshooting your application. Reset the eluent concentration and/or the flow rate to the recommended values. EGC-1 INVALID FLOW RATE ERROR EGC-2 INVALID FLOW RATE ERROR This error occurs if the flow rate is set to a value not supported by the eluent generator. The ICS-2100 allows a flow rate range of 0.00 to 5.00 mL/min without an eluent generator. With an eluent generator, the allowed range is 0.10 to 3.00 mL/min.The recommended operating range is 0.40 to 2.00 mL/min.
ICS-2100 Ion Chromatography System HARDWARE NOT PRESENT This error indicates a problem in the ICS-2100 electronics. To troubleshoot: Contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user. LEAK SENSOR WET The leak sensor is installed in the drip tray at the bottom of the component panel (see Figure 2-8). If liquid accumulates in the tray, the sensor signals the problem and this error message appears. To troubleshoot: 1.
4 • Troubleshooting 3. Turn off the ICS-2100 power briefly and then restart. 4. If the problem persists, repeat Step 2. 5. If the problem persists, contact Dionex for assistance. OPTION NOT INSTALLED This error occurs if a command is issued to control an option that is not installed. To troubleshoot: Check the Chromeleon Server Configuration program to verify that the option is enabled.
ICS-2100 Ion Chromatography System PUMP PRESSURE HARDWARE ERROR This error indicates a problem in the pump controller electronics. To troubleshoot: Contact Dionex for assistance. The ICS-2100 electronics components cannot be serviced by the user. PUMP OVER PRESSURE If the system pressure exceeds the set limit for at least 0.5 second, this error message appears and the pump stops. Pressure limits can be set in the Chromeleon Server Configuration or in the control program.
4 • Troubleshooting PUMP UNDER PRESSURE If the system pressure falls below the low pressure limit, the pump stops and this error message appears. Pressure limits can be set in the Chromeleon Server Configuration or in the control program. The limits can also be set on the touch screen PUMP page (see Section B.7.1). To troubleshoot: 1. Make sure the eluent reservoir is full. 2. Check for liquid leaks (see Section 4.3). 3. Check that the waste valve is closed. 4. Prime the pump (see Section 5.16). 5.
ICS-2100 Ion Chromatography System SUPPRESSOR NOT CONNECTED This error occurs if you turn on the suppressor and the ICS-2100 cannot establish a connection with the suppressor. To troubleshoot: 1. Check the suppressor cable connection (see Section 5.11). 2. If the error persists, contact Dionex for assistance. There may be a problem in the suppressor controller electronics. The ICS-2100 electronics components cannot be serviced by the user.
4 • Troubleshooting SUPPRESSOR OVER POWER This error occurs when, in order to maintain the selected current, the ICS2100 is required to apply a higher voltage than the suppressor can support. To troubleshoot: 1. Reduce the flow rate. 2. Rehydrate the suppressor. Refer to the suppressor manual for instructions. Suppressor manuals are included on the Dionex Reference Library CDROM (P/N 053891). 3. If the error persists, replace the suppressor (see Section 5.11).
ICS-2100 Ion Chromatography System 4.3 Liquid Leaks • Leaking fitting Locate the source of the leak. Tighten or, if necessary, replace the liquid line connection (see Section 5.3). 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). • Broken liquid line Replace the line and fittings with the same length and internal diameter tubing (see Section 5.3).
4 • Troubleshooting • Leaking pressure transducer 1. Make sure the liquid line connections into the pressure transducer are tight. Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements. The manual is 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.
ICS-2100 Ion Chromatography System 4.4 Pump Difficult to Prime or Loses Prime Excessive pressure fluctuations (more than 3% difference from one pressure reading to the next) indicate that the pump is out of prime. • Empty eluent reservoir and/or no eluent connected Fill the reservoir. Make sure all connections are secure. • Eluent improperly or insufficiently degassed Check the vacuum degas settings: 1. Open the Chromeleon Server Configuration program.
4 • Troubleshooting 4. Check the Degas settings. Select either the Monitor option or the Cycle option. If you select Cycle, set the time On to 30 seconds and the time Off to 600 seconds. If Cycle is already selected, try increasing the time on or decreasing the time off. NOTE Degas options can also be selected from the touch screen PUMP page (see Section B.7). • End-line filter is dirty or clogged When new, end-line filters (P/N 045987) are pure white.
ICS-2100 Ion Chromatography System 4.5 Pump Does Not Start • No power (front Power LED indicator is not lit) Check that the power cord is plugged in. Check the main power fuses and replace, if needed (see Section 5.18). • No communication between ICS-2100 and Chromeleon Verify that the USB cable is connected correctly. For connection and setup information, refer to the ICS-2100 installation instructions.
4 • Troubleshooting Waste Valve Priming Valve Figure 4-2. Waste and Priming Valves • Flow rate is set to 0 Set the flow rate from the ICS-2100 Control panel in Chromeleon or from the touch screen HOME page. • Eluent valve is closed Open the eluent valve from the ICS-2100 Control panel in Chromeleon or from the touch screen PUMP page. • Pump not primed Prime the pump (see Section 5.17). • Broken pump piston Replace the piston (see Section 5.8).
ICS-2100 Ion Chromatography System • 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). • Leaking liquid lines or fittings Check the liquid lines and fittings for small leaks. Tighten or, if necessary, replace the liquid line connection (see Section 5.3). Refer to Installation of Dionex Liquid Line Fittings (Document No. 031432) for tightening requirements.
4 • Troubleshooting • Plugged injection valve or auxiliary valve passages Rebuild the valve (see Section 5.4). 4.9 Peak “Ghosting” “Ghosting” is the appearance of extraneous peaks in a chromatogram. These may be late-eluting peaks from a previous injection. They may also be the result of a contaminated standard or eluent, or a malfunctioning injection valve. These peaks may co-elute with peaks of interest, resulting in nonreproducible peak heights/areas.
ICS-2100 Ion Chromatography System 4.10 Nonreproducible Peak Height or Retention Time • Column overloading Dilute the sample (see Section 3.9.3). • Liquid leaks Locate and eliminate the leaks (see Section 4.3). • Incomplete or imprecise filling of the sample loop 1. Fill the sample loop until excess sample exits the waste line. 2. Inspect the 1-cc syringe (P/N 016388) and replace if damaged. • Pump not primed properly Prime the pump (see Section 5.17). 4.
4 • Troubleshooting • No flow from pump This condition has several possible causes; see Section 4.5 and Section 4.6 for details. • Cell electronics malfunctioning Use the Chromeleon Wellness Panel diagnostics to test the electronics (see Section 5.1 and the Chromeleon Help for instructions). If the variance reading is outside the tolerance range (less than 1 μS), the electronics are malfunctioning. Contact Dionex for assistance. The ICS-2100 electronics cannot be serviced by the user. 4.
ICS-2100 Ion Chromatography System 4.14 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).
4 • Troubleshooting • Cell above or below temperature Contact Dionex for assistance. • Damaged piston seal Replace the piston seal (see Section 5.7). 4.15 Vacuum Degas Assembly Does Not Run • Degas option not enabled in Chromeleon 1. Open the Chromeleon Server Configuration program. Right-click the ICS-2100 device in the timebase and select Properties. 2. Select the Options tab (see Figure 4-3). . Figure 4-3. ICS-2100 Server Configuration Properties: Options 3.
ICS-2100 Ion Chromatography System 4. Under Degas, verify that the Always Off option is not selected. If it is, select one of the following settings instead: • Cycle; also select On: 30 seconds and Off: 10 minutes • Monitor 5. If the Degas settings are correct, but the degas assembly still does not run, test the assembly by selecting the Always On option. The pump should turn on immediately. If it does not, the vacuum degas assembly may need to be replaced. Contact Dionex for assistance.
5 • Service This chapter describes ICS-2100 service and repair procedures that the user can perform. All procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office. Before replacing any part, refer to the troubleshooting information in Chapter 4 to isolate the cause of the problem.
ICS-2100 Ion Chromatography System 5.1.1 Chromeleon Wellness Panel Overview NOTE Do not open a System Wellness Control panel if the name includes “Service.pan.” These Wellness panels are reserved for use by Dionex Service Representatives. To Open the Wellness Panel 1. 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).
5 • Service Use the Wellness Panel to perform the following functions: • Calibrate the pump flow rate • Calibrate the vacuum degas assembly • Calibrate the conductivity cell • Test the conductivity cell electronics, using a dummy cell • Upload calibration values from the ICS-2100 to the Chromeleon Wellness database After completing a calibration procedure from the touch screen, always update the Chromeleon Wellness database by clicking the Upload button on the Chromeleon Wellness Panel (see Figu
ICS-2100 Ion Chromatography System 5.1.2 Diagnostic and Calibration Touch Screen Overview Select DIAGNOSTIC from the touch screen menu of pages. The DIAGNOSTIC page opens (see Figure 5-2). From there, you can access individual diagnostic and calibration pages. NOTE The Service button provides access to service functions that are performed only by Dionex personnel. A code is required to access the service pages. . Figure 5-2.
5 • Service 5.1.3 Calibrating the Conductivity Cell When to Calibrate • After every 6 months of use NOTE Do not use this procedure to calibrate a new cell. If you are replacing a cell, see the instructions in Section 5.10 to install the new cell and calibrate it. Items Needed Description 1.0 mM KCl solution Prepare by dissolving 0.07456 g of reagentgrade KCl in 1 liter of 18-megohm DI water. Backpressure tubing to provide at least 7 MPa (1000 psi) Use 0.076-mm (0.
ICS-2100 Ion Chromatography System 2. On the Wellness Panel under Electric Conductivity Cell Calibration, click Offset Cal, or touch Run Offset Cal on the ICS2100 touch screen. 3. When the offset calibration is complete, click Slope Cal on the Wellness Panel, or touch Run Slope Cal on the ICS-2100 touch screen. 4. If you are using the Wellness Panel, click Log to record the new calibration values in the Audit Trail. 5. Disconnect the pump output line from the injection valve. 6.
5 • Service let it stabilize. When the temperature has stabilized, “=” is displayed to the right of the temperature reading on the CONDUCTIVITY CELL page. 11. Select 1.00 mL/min to begin pumping 1.00 mM KCl through the cell at 1.0 mL/min. 12. Wait until the total conductivity reading stabilizes (in about 15 minutes) and then select Calibrate on the Wellness Panel or the touch screen CONDUCTIVITY CELL page. After calibration, the conductivity reading should be 147.
ICS-2100 Ion Chromatography System 5.1.4 Calibrating the Flow Rate When to Calibrate If you run the ICS-2100 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) • High purity ASTM filtered, Type I (18 megohm-cm) deionized water • Balance capable of weighing more than 10 g with 0.001 g readability • Tared beaker To Calibrate 1.
5 • Service 3. On the Chromeleon Wellness Panel under Pump Flow Rate Calibration, select Reset Cal, or touch Reset Cal on the touch screen. 4. Select 1 mL/min to set the flow rate and begin pumping deionized water. 5. Allow the pump to stabilize for 20 minutes. 6. If you are using the Wellness Panel, click 5.00 min to start the timer. If you are using the touch screen, start an external timer. Immediately start collecting water into the tared beaker. 7. Collect the water for exactly 5.00 minutes. 8.
ICS-2100 Ion Chromatography System 5.1.5 Calibrating the Vacuum Degas Assembly When to Calibrate • After every 6 months of use 1. Open the ICS-2100 Wellness Panel in Chromeleon (see Section 5.1.1), or open the ICS-2100 touch screen PUMP DEGAS page (see Figure 5-6). Figure 5-6. Pump Degas Page 2. On the Wellness Panel under Degas Calibration, select Calibrate, or touch Calibrate on the ICS-2100 touch screen. The degas pump runs for 90 seconds to allow a vacuum to be created.
5 • Service 5.2 Isolating a Restriction in the Liquid Lines A restriction in the liquid plumbing will cause excessive system backpressure. 1. Begin pumping eluent through the system (including the columns). 2. Follow the flow schematics in Figure 5-7, Figure 5-8, or Figure 5-9 and work backward through the system, beginning at the suppressor Regen Out port. One at a time, loosen each fitting and observe the pressure. The connection at which the pressure drops abnormally indicates the point of restriction.
ICS-2100 Ion Chromatography System To the pump Degas In EGC Vent 6 EGC II KOH, LiOH, MSA, or NaOH 1 Deionized Water NOTE: The EGC Degas fittings cannot be serviced by the user. Inlet Outlet Regen In 8 Regen Out Eluent 7 EGC Degas Eluent Out 16 CR-TC 17 From the pulse damper Degas In To the inject valve port P(2) Column Heater Degas Out 13 Suppressor Cell Out 15 Eluent Out Regen In 14 Heat Exchanger Conductivity Cell Cell In 5 Pulse Damper Valve 10 W L Press. 4 Xducer.
5 • Service To the pump Degas In EGC Vent 6 NOTE: The EGC degas fittings cannot be serviced by the user EGC II K2CO3 1 Deionized Water Inlet Outlet Eluent Out 8 7 Regen Out EGC Degas Eluent In 18 EPM Regen In 17 Degas In 14 Suppressor Cell Out 16 Eluent Out Regen In 15 Heat Exchanger Regen Out Eluent In Degas Out Conductivity Cell Cell In Column Heater 9 Pulse Damper Valve L Press. 4 Xducer.
ICS-2100 Ion Chromatography System To the pump Degas In EGC Vent 6 NOTE: The EGC degas fittings cannot be serviced by the user EGC II K2CO3 1 Deionized Water Inlet Outlet 7 EGC Degas 16 Degas In 13 Suppressor Cell Out 15 Eluent Out Regen In 14 Heat Exchanger Conductivity Cell Cell In Regen Out Eluent In Degas Out Column Heater 8 11 L 10 W L Separator Pulse Damper Valve S Press. 4 Xducer.
5 • Service 5.3 Replacing Tubing and Fittings The ICS-2100 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 (P/N 044221) Red Connection from pump pulse damper to pressure transducer 0.25-mm (0.010-in) ID PEEK (P/N 042690) Black Connections between other system components 0.50-mm (0.020-in) ID PEEK (P/N 042855) Orange Connection from injection port to injection valve 0.75-mm (0.
ICS-2100 Ion Chromatography System 5.4 Rebuilding the Injection Valve or Auxiliary Valve Dionex recommends rebuilding the injection valve and the auxiliary valve (if installed) annually. The Injection Valve Rebuild Kit (P/N 057896) contains all required replacement parts for one valve. NOTE If you prefer, you can replace the auxiliary valve “pod,” instead of rebuilding the valve. Replacing the pod is easier and faster than rebuilding the auxiliary valve. For instructions, see Section 5.5.
5 • Service Figure 5-10. Injection Valve Plumbing NOTE A backpressure coil may be installed between port P and the line labeled TO INJECT VALVE - P. Doc.
ICS-2100 Ion Chromatography System 5.5 Replacing an Auxiliary Valve Pod This procedure describes how to replace the mechanical part (the “pod”) of the optional auxiliary valve. This procedure is an alternative to rebuilding the valve (see Section 5.4). NOTE If the valve electronics require service, contact Dionex. Electronics-related repair procedures must be performed by Dionex personnel. Substituting non-Dionex parts may impair performance, thereby voiding the product warranty.
5 • Service 8. Also verify that the two splines on the pod align with the matching splines inside the valve holder (see Figure 5-12). If necessary, twist the end of the pod to adjust the position of the splines. Valve Pod Valve Holder Slot (larger) Runner (larger) Splines Figure 5-12. Valve Pod and Pod Holder 9. Push the pod into the holder until it clicks into place. Replace the black locking ring. 10. Reconnect all liquid lines to the valve. 11. Turn on the pump flow. Check for leaks from the valve.
ICS-2100 Ion Chromatography System 5.6 Cleaning and Replacing the 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. Replacing Check Valves 1. Close the eluent valve from the ICS-2100 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 2.
5 • Service 6. If you are installing new cartridges (P/N 045994) in the existing check valve housings, place the cartridge in the inlet check valve housing with the double-hole end of the cartridge visible and place the cartridge in the outlet housing with the single-hole end visible. 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.
ICS-2100 Ion Chromatography System 5.7 Replacing a Pump Piston Seal and Piston Rinse 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 5-16).
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 5-14 or Figure 5-15). Priming Valve Knob (P/N 055709) Outlet Check Valve Assembly (P/N 045721) O-Ring (P/N 055752) Piston Seal (P/N 055870) Spacer with Drain (P/N 057913) Primary Pump Head (P/N 055711) Piston Rinse Seal (P/N 048722) O-Ring (P/N 014895) O-Ring (P/N 059283) Piston (P/N 052840) Inlet Check Valve Assembly (P/N 045722) Seal Guide (P/N 058032) Figure 5-14.
ICS-2100 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. Installing the New Piston Rinse Seal 1. Remove the guide from the spacer to expose the piston rinse seal and O-ring. Remove the O-ring. 2. Remove the old piston rinse seal from the guide as follows: a.
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. If this is the primary pump head, install a 10-32 fitting plug (P/N 042772) on the outlet check valve. Tighten the plug. 4. If this is the secondary pump head, install a 10-32 fitting plug (P/N 042772) in both the inlet and outlet ports. Tighten the plugs.
ICS-2100 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. 2. Insert the piston so that 1/4 inch of the shaft is exposed. This ensures that the magnet in the follower picks up the piston.
5 • Service 5.9 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-2100 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page. 2. Turn off the main power switch, to ensure that you do not unintentionally start the ICS-2100. 3.
ICS-2100 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 5-17). 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. Do not scratch the cavity. Scratches in the cavity will cause leaks around the base of the knob while the pump is being primed. Valve Knob O-Ring (P/N 055752) Figure 5-17.
5 • Service 5.10 Replacing the Conductivity Cell 1. Turn off the ICS-2100 power. 2. Open the front door and disconnect the tubing from the CELL IN and CELL OUT fittings (see Figure 5-18, View A). Loosen the two screws on the cell front cover. The screws remain attached (see Figure 5-18, View B). Unscrew Disconnect Unscrew View B View A Figure 5-18. Removing the Cell Front Cover 3. Grip the two loosened screws and pull the cell cover toward you to remove it from the component panel.
ICS-2100 Ion Chromatography System 5. Slide the new cell assembly straight into the opening in the component panel until it stops and the cell cover is flush against the component panel. The cell’s electronic connector automatically plugs into a connector inside the ICS-2100 when you push the assembly into the opening. 6. Tighten the screws on the cell front cover fingertight. 7. Close the side panel door and tighten the two mounting screws. 8. Reconnect the inlet and outlet lines. 9.
5 • Service To calibrate the cell on the ICS-2100 touch screen DIAGNOSTIC page: a. Go to the DIAGNOSTIC page and touch Electric Conductivity Cell. b. On the ELECTRIC CONDUCTIVITY CALIBRATION page (see Figure 5-20), touch Run Offset Cal. Figure 5-20. Electric Conductivity Calibration Page c. When the offset calibration is complete, touch Run Slope Cal. d. Touch the Cell Constant field and enter the value printed on the front of the cell. e.
ICS-2100 Ion Chromatography System 5.11 Replacing the Suppressor Refer to the suppressor manual for guidance about when to replace a suppressor. Suppressor manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 1. Refer to the suppressor quick start guide (shipped with the suppressor) for instructions on preparing the suppressor before initial use and for additional installation details. 2.
5 • Service 10. Push the cables into the opening in the component panel. 11. Align the top of the suppressor with the guide line printed on the component panel (see Figure 5-22) and align the slots on the rear of the suppressor with the tabs on the panel. 12. Press the suppressor onto the tabs and then slide it down until it locks into place. Pull slightly on the center of the suppressor to verify that it is securely fastened. Note: Some suppressors require more force to secure them onto the tabs. 13.
ICS-2100 Ion Chromatography System Thumbscrews (6) Figure 5-23. ICS-2100 Column Heater Cover Removed d. Remove the columns from the column heater. e. Pull the column heater straight toward you to remove it from the component panel. 4. Before installing the new column heater, write down the two calibration values (offset and slope) recorded on the back of the heater. 5.
5 • Service 9. Enter the column heater calibration values in Chromeleon or on the ICS-2100 touch screen DIAGNOSTIC page as follows. To enter the calibration values in Chromeleon: a. Open the Wellness Panel (see Section 5.1.1) and click Calibration Details. b. Under Column Heater Calibration Values, enter the Column Heater Offset and Column Heater Slope values recorded in Step 4. c.
ICS-2100 Ion Chromatography System c. To ensure the calibration values are recorded in the ICS-2100 memory, do not turn off the ICS-2100 power for at least 1 minute after entering the values. d. Record the calibration values in the Chromeleon Wellness database. To do this, open the Wellness Panel (see Section 5.1.1) and click Upload under Update Wellness Database. 5.13 Replacing the Column Heater Heat Exchanger 1. Turn off the ICS-2100 power. 2. Open the front door of the ICS2100. 3.
5 • Service tubing) and press the heat exchanger onto the heater. Replace the screws removed in Step 8. 10. Connect the new heat exchanger inlet line to port C on the injection valve and connect the outlet line to the guard column inlet. 11. Reinstall the top metal plate and the heater cover. 5.14 Replacing the Eluent Valve 1. Turn off the power to the ICS-2100. 2. Open the ICS-2100 front door. 3.
ICS-2100 Ion Chromatography System 6. Pull the valve straight out from the component panel and begin pulling the attached cable out of the opening in the panel. 7. The cable is connected to a matching cable inside the ICS-2100. Continue pulling until the connectors for the two cables are outside the panel (see Figure 5-27). Disconnect the cables. Disconnect cables Eluent Valve Eluent Valve Cable Figure 5-27. Eluent Valve Cable 8.
5 • Service 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-2100. 14. Prime the pump (see Section 5.17). 5.15 Replacing the Leak Sensor 1. Turn off the power to the ICS2100. 2. Open the ICS-2100 front door. 3. Loosen the screw on the front of the leak sensor (see Figure 5-29). Note: The screw remains attached to the sensor. Leak Sensor Loosen Screw Figure 5-29.
ICS-2100 Ion Chromatography System 7. Connect the cable from the new leak sensor (P/N 058053) to the ICS-2100 cable. 8. Feed the cables back inside the ICS-2100. 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. 5.16 Priming the Pump 1.
5 • Service Secondary Pump Head Waste Valve (close) Port Primary Pump Head 10 mL Syringe (P/N 054578) Priming Valve (open) Figure 5-31. Priming the Eluent Lines 3. Open the priming valve by turning it one-quarter to one-half turn counterclockwise. 4. On the ICS-2100 Control panel in Chromeleon, click the Pump Settings button. The Pump Settings window opens (see Figure 3-6). 5. Under Eluent Flow Valve, click the Open button. 6. Draw the syringe back to begin pulling eluent through the flow path.
ICS-2100 Ion Chromatography System 5.16.2 Priming with the Prime Button NOTE Perform this procedure after priming the eluent lines (see Section 5.16.1). 1. Check that the priming valve on the primary pump head is closed (see Figure 5-32). Secondary Pump Head Waste Valve (open) Priming Valve (close) Primary Pump Head Figure 5-32. Priming the Pump 2. Open the waste valve on the secondary pump head by turning the knob one-quarter to one-half turn counterclockwise (see Figure 5-32).
5 • Service 5.17 Priming the Pump with Isopropyl Alcohol NOTE Prime the pump heads with isopropyl alcohol only if the two standard priming procedures described in Section 5.16 are unsuccessful. 1. Connect a 10-mL syringe (P/N 054578) filled with isopropyl alcohol (IPA) to the port in the primary pump head (see Figure 5-33). 2. Open the waste valve on the secondary pump head (see Figure 5-33) by turning the knob onequarter to one-half turn counterclockwise.
ICS-2100 Ion Chromatography System Isopropyl alcohol may damage some columns. Be sure to thoroughly rinse the alcohol from the pump, using the process described in Step 7. 8. Close the waste valve. Do not overtighten. 9. Select the flow rate required for the analysis. 10. In the Pump Settings window, click Pump Off. 5.18 Changing Main Power Fuses 1. Turn off the main power switch. HIGH VOLTAGE—Disconnect the main power cord from its source and also from the rear panel of the ICS-2100.
5 • Service 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. 5. Reconnect the main power cord and turn on the power. 5.19 Replacing an EluGen Cartridge The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), or a corrosive acid (MSA).
ICS-2100 Ion Chromatography System 4. Remove the EluGen cartridge VENT line (see Figure 5-35) from the EluGen cartridge by unscrewing the luer lock from the luer adapter. Luer Adapter Luer Lock EGC Vent Line If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-35. EluGen Cartridge Vent Line and Luer Fitting 5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter.
5 • Service Figure 5-37. EluGen Cartridge in the Service Area 8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the EluGen cartridge (see Figure 5-38). EGC OUT EGC IN OUTLET Port INLET Port Figure 5-38. Disconnect the EluGen Cartridge Inlet and Outlet Port Lines 9.
ICS-2100 Ion Chromatography System 10. Remove the new EluGen cartridge from the shipping box. 11. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the EluGen cartridge INLET and OUTLET ports (see Figure 5-39). OUTLET INLET Figure 5-39. EluGen Cartridge Inlet and Outlet Ports 12. Set the EluGen cartridge in the service area on top of the ICS-2100 and orient it with the cable toward the EGC holder (see Figure 5-40). EluGen Cartridge Cable Figure 5-40.
5 • Service 14. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) in the ICS-2100 Ship Kit (P/N 064375). Backpressure Coil 15. Connect one end of this coil to the EluGen cartridge OUTLET port (see Figure 5-41). Leave the other end of the coil unconnected. OUTLET Port Figure 5-41.
ICS-2100 Ion Chromatography System 17. Slide the EluGen cartridge down into the holder until it stops. Make sure the cable and backpressure coil remain out of the holder (see Figure 5-42). NOTE To avoid crimping the lines inside the holder, do not twist the cartridge before you slide it into the holder. The lines are designed to coil inside the holder. Figure 5-42. Installing the EluGen Cartridge in the Holder 18. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure 5-43.
5 • Service 19. Remove the plug from the EluGen cartridge vent opening and connect the EluGen cartridge VENT line. Recording the EluGen Cartridge Serial Number in Chromeleon The serial number is printed on the EluGen cartridge label. 1. Open the Chromeleon Server Configuration program (select Start > All Programs > Chromeleon > Server Configuration). 2. Double-click the ICS-2100 system icon. The properties dialog box for the ICS-2100 appears. 3. Click the Eluent Generator tab (see Figure 5-44). 4.
ICS-2100 Ion Chromatography System Conditioning the EluGen Cartridge Always condition the EluGen cartridge before initial use. This requires directing the backpressure coil connected to the EluGen cartridge outlet to waste, and then generating 50 mM of eluent at 1.00 mL/min for 30 minutes. Follow the steps below: 1. Set a temporary waste container, such as a beaker, on top of the ICS2100 and direct the yellow backpressure coil from the EluGen cartridge OUTLET port to the container. 2.
5 • Service 11. Lift the EluGen cartridge out of the holder, turn it over, and set it in the service area. EGC OUT EGC IN OUTLET Port INLET Port 12. Disconnect the backpressure coil from the EluGen cartridge OUTLET port. 13. Connect the EGC OUT line from the holder to the OUTLET port (see Figure 5-45). Figure 5-45. EluGen Cartridge Inlet and Outlet Connections 14. Turn over the EluGen cartridge (fittings facing down). Check for bubbles.
ICS-2100 Ion Chromatography System 4. Remove the EluGen cartridge VENT line (see Figure 5-46) from the EluGen cartridge by unscrewing the luer lock from the luer adapter. Luer Adapter Luer Lock EGC Vent Line If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-46. EluGen Cartridge Vent Line and Luer Fitting 5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter.
5 • Service Figure 5-48. EluGen Cartridge In the Service Area 8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET fittings on the EluGen cartridge (see Figure 5-49). EGC OUT EGC IN OUTLET Port INLET Port Figure 5-49. Disconnect the EluGen Cartridge Inlet and Outlet Port Lines 9.
ICS-2100 Ion Chromatography System 10. Remove the new EluGen cartridge from the shipping box. 11. Orient the EluGen cartridge with the fittings facing up and remove the plugs from the EluGen cartridge INLET and OUTLET ports (see Figure 5-50). OUTLET INLET Figure 5-50. EluGen Cartridge Inlet and Outlet Ports 12. Set the EluGen cartridge in the service area on top of the ICS-2100 and orient it with the cable toward the EGC holder (see Figure 5-51). EluGen Cartridge Cable Figure 5-51.
5 • Service 15. Turn the EluGen cartridge over (with the fittings facing down). Shake the EluGen cartridge vigorously, and tap it with the palm of your hand 10 to 15 times. Check that all bubbles trapped in the eluent generation chamber are dislodged. The EluGen cartridge contains one of the following: a corrosive base (KOH, LiOH, or NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear protective eyewear and gloves when handling the cartridge.
ICS-2100 Ion Chromatography System 17. Remove the plug from the EGC-1 connector on top of the ICS-2100. 18. Orient the cartridge’s blue 4-pin electrical cable connector as shown in Figure 5-53. Push it onto the EGC-1 connector on the ICS2100. Twist the ring on the cable connector fingertight to secure it. Figure 5-53. Connecting the EluGen Cartridge Cable 19. Remove the plug from the EluGen cartridge vent opening and connect the EluGen cartridge VENT line. 156 Doc.
5 • Service Recording the EluGen Cartridge Serial Number in Chromeleon The serial number is printed on a label on the EluGen cartridge. 1. Open the Server Configuration program (select Start > All Programs > Chromeleon > Server Configuration). 2. Double-click the ICS-2100 system icon. The properties dialog box for the ICS-2100 appears. 3. Click the Eluent Generator tab. 4. Select the EGC-1 check box. 5. Enter the EluGen cartridge serial number. Verify that the cartridge type is Carb.
ICS-2100 Ion Chromatography System Continue on to one of the following sections, depending on the type of eluent to be generated: • • 158 For carbonate eluent, go to “Plumbing the EluGen Cartridge for Conditioning with Carbonate Eluent” on page 159. For carbonate/bicarbonate eluent, go to “Plumbing the EluGen Cartridge and EPM for Conditioning with Carbonate/Bicarbonate Eluent” on page 162. Doc.
5 • Service Plumbing the EluGen Cartridge for Conditioning with Carbonate Eluent Figure 5-55 illustrates the liquid flow path during the EluGen cartridge conditioning procedure with carbonate eluent. EGC VENT EGC II K2CO3 Send to waste Outlet Inlet EGC IN TO DEGAS ELUENT IN TO DEGAS ELUENT OUT EGC OUT EGC DEGAS TO EGC CO3 MIXER OUT TO INJ VALVE IN - P/ ELUENT OUT TO PUMP/ DAMPER 14 MPa (2000 psi) at 1.
ICS-2100 Ion Chromatography System 1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 2. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and a 10-32 to 10-32 coupler (P/N 042627) in the ICS2100 Ship Kit (P/N 064375). 3. Use the coupler to connect the TO INJ VALVE IN - P/ELUENT OUT line to one end of the backpressure coil (see Figure 5-56). 4. Direct the free end of the backpressure coil to a temporary waste container.
5 • Service Conditioning the EluGen Cartridge Always condition the EluGen cartridge for 30 minutes before initial use. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor and the auxiliary electrolytic device attached to the EGC-2 connector (if installed) are off. To avoid damaging the suppressor (and auxiliary electrolytic device, if installed), always turn them off before conditioning the EluGen cartridge.
ICS-2100 Ion Chromatography System Plumbing the EluGen Cartridge and EPM for Conditioning with Carbonate/Bicarbonate Eluent Figure 5-57 illustrates the liquid flow path through the eluent generator during conditioning with carbonate/bicarbonate eluent.
5 • Service 1. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and 10-32 to 1/4-28 coupler (P/N 042806) in the ICS2100 Ship Kit (P/N 064375). 2. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 3. Connect one end of the backpressure coil to the TO INJ VALVE IN P/ELUENT OUT line. 4. Connect the 10-32 to 1/4-28 coupler to the free end of the backpressure coil. 5. Disconnect the TO SRS/AES REGEN OUT line from the suppressor REGEN OUT port. 6.
ICS-2100 Ion Chromatography System Conditioning the EluGen Cartridge Always condition the EluGen cartridge for 30 minutes before initial use. 1. Make sure the eluent reservoir is filled with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor and the auxiliary electrolytic device (if installed) are off. To avoid damaging the suppressor (and auxiliary electrolytic device, if installed), always turn them off before conditioning the EluGen cartridge.
5 • Service 5.20 Replacing the CR-TC 1. Turn off the pump from the ICS-2100 Control panel in Chromeleon or from the touch screen HOME page. 2. Follow the instructions in Section 5.19.1, Step 2 through Step 8 to disconnect the EluGen cartridge and CR-TC cables, cap the EluGen cartridge vent opening, remove the EluGen cartridge from the holder, and disconnect the inlet and outlet tubing. 3.
ICS-2100 Ion Chromatography System 10. Check that none of the lines are caught under the CR-TC and then push the CR-TC onto the metal stud inside the EGC holder. Push down until the CR-TC snaps into place (see Figure 5-60). Figure 5-60. CR-TC Installed in Holder 11. Feed the CR-TC cable through the slot on the side of the EGC holder (see Figure 5-61). 12. Turn the EGC holder right-side up. CR-TC Cable Figure 5-61. CR-TC Cable 13.
5 • Service 15. Reinstall the EluGen cartridge in the holder. 16. Remove the cap on the luer adapter by twisting. Save the cap. 17. Twist the luer lock and EGC VENT line into the luer adapter. 18. Do not connect the EluGen cartridge cable until after hydrating the CR-TC. Hydrating the CR-TC The CR-TC must be hydrated before initial use by running ASTM filtered, Type 1 (18 megohm-cm) deionized water through the CR-TC for 10 minutes, while bypassing the columns and suppressor.
ICS-2100 Ion Chromatography System 1. Locate the 10-32 to 1/4-28 coupler (P/N 042806) in the ICS-2100 Ship Kit (P/N 064375). 2. Use the coupler to connect the line labeled TO INJ VALVE IN P/ELUENT OUT and the line labeled SRS/AES REGEN OUT. 3. Verify that the current to the suppressor and the auxiliary electrolytic device (if installed) is turned off. To avoid damaging the suppressor and auxiliary electrolytic device (if installed), always turn them off before hydrating the CR-TC.
5 • Service 5.21 Replacing the EPM Electrolytic pH Modifier 1. Turn off the pump from the ICS-2100 Control panel in Chromeleon or from the touch screen HOME page. 2. Disconnect the EPM electrical cable from the EGC-2 connector on the ICS2100 top cover. 3. Disconnect the four liquid lines from the ports on the EPM. 4. Lift up the mounting bracket with the EPM attached and remove the bracket and EPM from the EGC holder. 5. Pull the EPM off the mounting bracket. 6.
ICS-2100 Ion Chromatography System 5.21.1 Recording the EPM Serial Number in Chromeleon The serial number is printed on a label on the EPM. 1. Open the Server Configuration program (select Start > All Programs > Chromeleon > Server Configuration). 2. Double-click the ICS-2100 system icon. The properties dialog box for the ICS-2100 appears. 3. Click the Eluent Generator tab (see Figure 5-44). 4. Select the EGC-2 check box. 5. Enter the serial number of the EPM. 6. Verify that the cartridge type is pH Mod.
5 • Service 5.21.2 Plumbing the EPM for Hydrating and Conditioning Figure 5-57 illustrates the liquid flow path during hydration and conditioning.
ICS-2100 Ion Chromatography System 1. Disconnect the TO INJ VALVE IN - P/ELUENT OUT line from the EGC CO3 Mixer inlet. 2. Use a 10-32 to 10-32 coupler (P/N 042627) to connect the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) to the TO INJ VALVE IN - P/ELUENT OUT line. 3. Connect a 10-32 to 1/4-28 coupler (P/N 042806) to the free end of the backpressure coil. 4. Disconnect the TO SRS/AES REGEN OUT line from the suppressor REGEN OUT port. 5.
5 • Service 5.21.3 Hydrating and Conditioning the EPM Follow the steps below to hydrate the EPM for 5 minutes and then condition the EPM for 30 minutes. 1. Fill the eluent reservoir with ASTM filtered, Type I (18-megohm) deionized water. 2. Verify that the suppressor and the auxiliary electrolytic device (if installed) are off. To avoid damaging the suppressor and auxiliary electrolytic device (if installed), always turn them off before conditioning the EPM and EluGen cartridge.
ICS-2100 Ion Chromatography System 14. Reconnect the TO INJ VALVE IN - P/ELUENT OUT line to the EGC CO3 Mixer inlet. 15. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port. 5.22 Replacing the EGC CO3 Mixer 5.22.1 Installing the New EGC CO3 Mixer 1. Turn off the pump from the ICS-2100 Control panel in Chromeleon or from the touch screen HOME page. 2.
5 • Service 4. Connect the TO EGC CO3 MIXER IN line to the mixer inlet and connect the TO EGC CO3 MIXER OUT line to the mixer outlet. TO EGC CO3 MIXER OUT TO EGC CO3 MIXER IN Figure 5-67. ICS-2100 with an EGC CO3 Mixer Installed 5.22.2 Filling the EGC CO3 Mixer with Deionized Water Before initial use, follow the steps below to temporarily fill the EGC CO3 Mixer with deionized water.
ICS-2100 Ion Chromatography System TO PUMP/ DAMPER (Disconnect this line) Pump Outlet (Green tubing) Figure 5-68. Disconnect the Cartridge Inlet and Pump Outlet 3. Disconnect the TO EGC CO3 MIXER IN line from the TO INJ VALVE IN P/ELUENT OUT line. 176 Doc.
5 • Service 4. Connect the pump outlet to the mixer inlet (see Figure 5-69). Pump Outlet Mixer Inlet Figure 5-69. Pump Outlet Connected to Mixer Inlet for Mixer Hydration 5. Disconnect the mixer outlet line (labeled TO INJ VALVE PORT P) from port P (2) on the injection valve. 6. Direct the mixer outlet line to a temporary waste container, such as a beaker. 7. From the ICS-2100 Control panel in Chromeleon or the ICS-2100 touch screen HOME page, set the pump flow rate to 5.00 mL/min. 8.
ICS-2100 Ion Chromatography System 11. Run the pump until the mixer is filled and there is a consistent flow of water exiting the mixer outlet. It takes about 5 minutes to fill a 4-mm mixer and about 2 minutes to fill a 2-mm mixer. 12. Turn off the pump. 5.22.3 Filling the EGC CO3 Mixer with Eluent Before initial use, follow the steps in this section to fill the EGC CO3 Mixer with the eluent required for the application to be run.
5 • Service Filling the EGC CO3 Mixer with Carbonate Eluent Figure 5-70 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate eluent.
ICS-2100 Ion Chromatography System 1. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765) and a 10-32 to 10-32 coupler (P/N 042627) in the ICS2100 Ship Kit (P/N 064375). 2. Use the coupler to connect one end of the backpressure coil to the TO INJ VALVE IN - P/ELUENT OUT line. 3. Connect the other end of the backpressure coil to the coupler on the mixer inlet. NOTE The backpressure coil connection is temporary; it is required only during initial filling of the mixer. 4.
5 • Service 12. Run at these settings until a consistent flow of eluent is exiting the mixer outlet. At a flow rate of 1 mL/min it will take about 16 minutes to fill a 4-mm mixer and about 5 minutes to fill a 2-mm mixer. NOTE The void volume of the 4-mm mixer is about 16 mL. The void volume of the 2-mm mixer is about 5 mL. 13. Turn off the EGC-1 current. 14. Turn off the pump. 15. Remove the backpressure coil from the TO INJ VALVE IN - P/ELUENT OUT line and the mixer inlet. 16.
ICS-2100 Ion Chromatography System Filling the EGC CO3 Mixer with Carbonate/Bicarbonate Eluent Figure 5-71 illustrates the liquid flow path through the eluent generator components during initial filling of the EGC CO3 Mixer with carbonate/bicarbonate eluent.
5 • Service 1. Locate the following items in the ICS-2100 Ship Kit (P/N 064375): a yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil (P/N 053765), a 10-32 to 10-32 coupler (P/N 042627), and a 10-32 to 1/4-28 coupler (P/N 042806). 2. Use the 10-32 to 10-32 coupler to connect one end of the backpressure coil to the TO INJ VALVE IN - P/ELUENT OUT line (see Figure 5-72). 3. Connect the other end of the backpressure coil to the coupler on the mixer inlet. 4.
ICS-2100 Ion Chromatography System 5. Verify that the suppressor and the auxiliary electrolytic device (if installed) are off. To avoid damaging the suppressor and auxiliary electrolytic device (if installed), always turn them off before filling the mixer. The pump flow is on during filling; however, no flow reaches the suppressor or auxiliary electrolytic device. 6. Verify that the Automatically turn on with pump option is not selected on the touch screen SUPPRESSOR page (see Section B.9).
5 • Service 17. Reconnect the TO SRS/AES REGEN OUT line to the suppressor REGEN OUT port. 18. Reconnect the mixer outlet line to port P (2) on the injection valve. 5.23 Replacing the EGC Holder and Degas Assembly 5.23.1 Disconnecting and Removing the EluGen Cartridge 1. Turn off the power to the ICS-2100. 2.
ICS-2100 Ion Chromatography System 4. Remove the EGC VENT line (see Figure 5-73) from the EluGen cartridge by unscrewing the luer lock from the luer adapter. Luer Adapter Luer Lock EGC Vent Line If necessary, use a wrench to hold the luer adapter in place while unscrewing the vent line. Figure 5-73. EluGen Cartridge Vent Line and Luer Fitting 5. Install the luer cap (P/N 053981), provided with the EluGen cartridge, onto the luer adapter.
5 • Service 9. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the cartridge. 10. Lift the EGC holder out of the top cover and pull the liquid lines through the tubing chase (see Figure 5-75) to remove them from the ICS2100. Tubing Chase Figure 5-75. Top Cover Tubing Chase 11. If a CR-TC is installed, go on to Section 5.23.2. 12. If an EPM is installed, go on to Section 5.23.3. 13. If neither a CR-TC or EPM is installed, go on to Section 5.23.4. Doc.
ICS-2100 Ion Chromatography System 5.23.2 Removing the CR-TC and Reinstalling it in the New EGC Holder 1. Turn the holder upside down to view the CR-TC. 2. Grasp the top of the CRTC and lift up to disconnect it from the holder. Disconnect liquid lines from 4 ports 3. Disconnect the liquid lines from the four ports on the CR-TC (see Figure 5-59). Figure 5-76. Disconnecting CR-TC Liquid Lines 4. Turn the new holder upside down (see Figure 5-77) and connect the liquid lines to the CR-TC.
5 • Service 5. Check that none of the lines are caught under the CR-TC and then push the CR-TC onto the metal stud inside the EGC holder. Push down until the CR-TC snaps in place (see Figure 5-78). Figure 5-78. CR-TC Installed in Holder 6. Feed the CR-TC cable through the slot on the side of the EGC holder (see Figure 5-79). CR-TC Cable Figure 5-79. CR-TC Cable 7. Turn the EGC holder right side up and set it on top of the ICS-2100. 8.
ICS-2100 Ion Chromatography System 9. Feed the following liquid lines from the bottom of the holder through the tubing chase to the ICS-2100 front component panel. • • • TO SRS/AES REGEN OUT TO INJ VALVE IN - P/ELUENT OUT TO PUMP/DAMPER 10. Connect the lines to their respective locations: • Connect the line labeled TO SRS/AES REGEN OUT to the REGEN port on the suppressor. OUT • • Connect the line labeled TO INJ VALVE IN - P/ELUENT OUT to port P (2) on the injection valve.
5 • Service 4. Thread the three lines from the EPM (red, yellow, and blue labels) through the opening on the side of the new holder (see Figure 5-80). TO CR-TC/EPM ELUENT IN (red label) TO CR-TC/EPM ELUENT OUT (yellow label) TO CR-TC/EPM REGEN OUT (blue label) Figure 5-80. TO CR-TC/EPM Lines Outside of Holder 5. Turn the new EGC holder upside down (see Figure 5-81). NOTE To help retain the fittings and ferrules on the lines, remove the coupler from each line just before connecting the line to a port.
ICS-2100 Ion Chromatography System 8. Turn the EGC holder right side up and set it in place on top of the ICS-2100. 9. Slide the EPM mounting bracket and connected EPM onto the side of the EGC holder. 10. Feed the following liquid lines through the tubing chase to the ICS2100 front component panel. • • • TO SRS/AES REGEN OUT TO INJ VALVE IN - P/ELUENT OUT TO PUMP/DAMPER 11.
5 • Service • • Connect the line labeled TO INJ VALVE IN - P/ELUENT OUT to the EGC CO3 Mixer inlet. Connect the line labeled TO PUMP/DAMPER to the pulse damper. 4. Direct the WASTE, GAS SEPARATOR line from the top of the ICS2100 to the rear panel. Snap the line onto one of the tubing clips on the rear panel. Connect the line to the gas separator waste tube (see Section B.10.1). 5. Go on to Section 5.23.5. 5.23.5 Reinstalling the EluGen Cartridge 1.
ICS-2100 Ion Chromatography System 194 Doc.
A • Specifications A.1 Electrical Main Power Fuses A.2 100 to 240 Vac, 50 to 60 Hz (Auto-sensing power supply; no manual voltage or frequency adjustment required) Two 3.15 amp fast-blow IEC 127 fuses (P/N 954745) Physical Dimensions (Without reservoir or EluGen cartridge) Weight Decibel Level Control Modes USB Communication Protocol Doc. 065291-01 3/09 Height: 56.1 cm (22.1 in) Width: 22.4 cm (8.8 in) Depth: 53.3 cm (21.0 in) 24.
ICS-2100 Ion Chromatography System A.3 Environmental Operating Temperature Operating Humidity Operating Pressure A.4 35 MPa (5000 psi) maximum liquid path (tubing, valve, columns, etc.
A • Specifications Flow Accuracy Pressure Ripple Eluent On/Off Valve Piston Seal Wash Pressure Alarm Limits <0.1% typical <1% at 13.8 MPa (2000 psi) and 1.0 mL/min Standard feature Dual-pump head; wash can be continuous when connected to rinse solution supply • • Vacuum Degas Eluent Bottles Eluent Bottle Pressure Leak Detection Doc.
ICS-2100 Ion Chromatography System A.6 Eluent Generation Eluent Types Gradient Profiles Concentration Increments KOH, LiOH, NaOH, K2CO3, K2CO3/KHCO3, MSA Optional feature; combination of unlimited number of linear, convex, and concave positive and negative gradient profiles 0.01 mM Flow Rate 0.1 to 3.
A • Specifications EluGen Cartridges Eluent Concentration Range Comment K2CO3/EPM Electrolytic pH Modifier 0.1 to 15 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 2.0 mL/min flow X = 15/flow The total of the eluent concentrations from the EluGen cartridge and the EPM must not exceed the specified range. The EPM concentration must not exceed 10 mM. KOH/KOH KOH/MSA KOH/NaOH MSA/MSA MSA/NaOH NaOH/NaOH 0.1 to 50 mM at 0.1 to 1.0 mL/min flow 0.1 to X mM at 1.0 to 3.
ICS-2100 Ion Chromatography System A.7 Detector Electronics Type Cell Drive 1% up to 1 mS Resolution 0.00238 nS/cm Electronic Noise Filter Temperature Compensation • • Digital signal range: 0 to 15,000 μS Analog signal range: 0 to 15,000 μS ±0.1 nS/cm when background conductivity is 0 to 150 μS/cm ±2 nS/cm when background conductivity is 151 to 3200 μS/cm Rise times from 0 to 10 s; user-selectable Fixed at 1.
A • Specifications Operating Temperature Doc.
ICS-2100 Ion Chromatography System A.9 Injection Valve Injection Valve 6-port, 2-position Rheodyne valve with PEEK wetted components; electrically-activated A.10 Auxiliary Valve (Optional) Auxiliary Valve 6-port or 10-port, 2-position Rheodyne valve with PEEK wetted components; electrically-activated A.11 Vacuum Degas Assembly Channel Pump Materials Single-channel degas channel with degas membranes Dual-stage diaphragm vacuum pump Wetted materials, PEEK, Teflon A.
A • Specifications A.
ICS-2100 Ion Chromatography System Void Volume SRS 300 (4 mm): <50 μL SRS 300 (2 mm): <15 μL MMS 300 (4 mm): <50 μL MMS 300 (2 mm): <15 μL AMMS ICE 300 (4 mm): <50 μL AMMS ICE 300 (2 mm): <15 μL Anion AES: <35 μL Cation AES: <35 μL A.
A • Specifications System Wellness and Predictive Performance Data Trending Plots Virtual Column Simulator Standard feature Numerical device parameters can be plotted • • Evaluation mode: Standard feature Isocratic and gradient modes: Optional features Application Templates Standard feature Automation Support for Third-Party Vendors Fully controls over 300 different instruments from more than 30 manufacturers, including GC, HPLC, and MS 3D Software for PDA, MS, and ED Optional feature Customizab
ICS-2100 Ion Chromatography System 206 Storage of System Calibration Settings Factory, current, and previous calibration values are stored; the user can reset current values to factory or previous values Customized Reporting Standard feature; unlimited report workbooks Automated System Qualification Detailed, comprehensive qualification reports Doc.
B • Touch Screen Operation The LCD touch screen on the ICS-2100 front panel allows local control of most ICS-2100 functions. This chapter describes how to operate the ICS-2100 from the touch screen. When the ICS-2100 starts up, the touch screen displays a startup page. This is followed by the INFORMATION page, which displays version and serial numbers and a list of installed options. After a few seconds, the HOME page (see Figure B-1) is displayed.
ICS-2100 Ion Chromatography System • • • Edit fields and command buttons have blue text on a lightly shaded background. Fields that display status information are not shaded. Edit fields have square corners while command buttons are rounded. To edit a field or select a command button, touch and release the field or button with your fingertip. NOTE When you touch a button or edit field, the action takes effect when you lift your finger.
B • Touch Screen Operation • Touching the page name (for example, corner opens a menu of pages (see Figure B-3). ) in the bottom right Touch a page name to display the page. Figure B-3. ICS-2100 Touch Screen Menu of Pages • Touching a page name on the menu of pages displays the selected page. For example, touching SUPPRESSOR displays the SUPPRESSOR page (see Figure B-4). Touch to select a different option. Touch to return to the Home page. Touch to return to the previous page. Figure B-4.
ICS-2100 Ion Chromatography System • Touching returns you to the HOME page. • Touching opens a list of options (see Figure B-5). Touch an option to select it. Note: To cancel and retain the current selection, touch outside of the list. Figure B-5. Suppressor Page: Selecting an Option B.2 Using the Touch Screen with Chromeleon When the ICS-2100 is connected to a Chromeleon Control panel, the status field at the bottom center of the HOME page displays Remote Mode.
B • Touch Screen Operation B.3 Overview of ICS-2100 Touch Screen Pages Figure B-6 illustrates the organization of the ICS-2100 touch screen pages.
ICS-2100 Ion Chromatography System B.4 Home Page Status Field Edit Field Command Button (selected) Command Button (unselected) Figure B-7. ICS-2100 Touch Screen Home B.4.1 Page Home Page Pump Controls Pressure Display The HOME page indicates the current pressure reading from the pressure transducer. The pressure unit can be set to psi (the factory default), MPa, or bar (see Section B.7.1). The minimum and maximum pressure limits are displayed below the current pressure reading.
B • Touch Screen Operation Flow Rate The flow rate can be set to 0.00 (which turns off the pump) and to between 0.05 and 5.00 mL/min. The recommended operating flow rate is between 0.40 and 2.00 mL/min. Refer to the column manual for the flow rate to use with your column and application. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). Pump On/Off Control Touching the On button immediately starts the pump flow at the rate displayed in the Flow Rate field.
ICS-2100 Ion Chromatography System B.4.2 Home Page EGC Controls EGC-1 Cartridge Type EGC-2 Cartridge Type EGC-1 Eluent Concentration EGC-2 Eluent Concentration The EGC controls indicate the type and the eluent concentration of each installed EluGen Cartridge (EGC). The CR-TC field indicates whether the Continuously Regenerated Trap Column is on or off. To determine the eluent concentration for your application, refer to the column manual.
B • Touch Screen Operation B.4.4 Home Page Injection Valve Controls The Inject and Load buttons select the position of the injection valve. A dark background and white text on a button indicates the current valve position. For details about the valve positions, see Section 2.4.6. The ELAPSED TIME field displays the amount of time since the last injection. B.4.5 Home Page Detector Controls Conductivity Readings The offset conductivity is displayed in large numbers above the total conductivity.
ICS-2100 Ion Chromatography System Suppressor Controls The Suppressor controls indicate the suppressor current setting and the type of suppressor installed. To set the suppressor type, change the current setting, or turn the suppressor on or off, touch the suppressor button. The SUPPRESSOR page appears (see Section B.9). B.4.6 Other Home Page Controls This field displays Remote Mode when the ICS-2100 is connected to Chromeleon and Local Mode when the system is not connected to Chromeleon.
B • Touch Screen Operation B.5 Plot Page The PLOT page provides a real-time plot of the detector conductivity output. To open the page, touch the PLOT button on the HOME page, or select PLOT from the menu of pages. The page can display up to 60 minutes of data. Data older than 60 minutes is discarded. You can view the plot and adjust the display when the ICS-2100 is under either local or computer control. Figure B-8.
ICS-2100 Ion Chromatography System B.6 Status Page The STATUS page displays the current status of various operating parameters. To open this page, touch the STATUS button on the HOME page or select STATUS from the menu of pages. Figure B-9. Status Page Status Page Controls • • Pressure and conductivity readings are the same as those displayed on the HOME page. The eluent bottle depicts the level of liquid in the eluent reservoir.
B • Touch Screen Operation • • The fields to the right of the bottle display the status of four other operating parameters. You can choose from eight possible parameters to display here. Figure B-9 shows the default parameters: Eluent time, Flow rate, EGC conc, and Suppressor. To select different parameters, touch the Setup button. See Section B.6.1 for details about how to change the status parameters, and Section B.6.2 for a description of each parameter.
ICS-2100 Ion Chromatography System B.6.1 Viewing Other Status Parameters Follow the steps below to view the status of a parameter that is not currently displayed on the STATUS page. 1. Touch the Setup button. A drop-down list replaces the label for each field, and the Setup button changes to Apply (see Figure B-11). Figure B-11. Status Page Setup 220 Doc.
B • Touch Screen Operation 2. Touch the down arrow next to the field you want to change. A list of the available status parameters appears (see Figure B-12). Figure B-12. Status Page Parameter List 3. Touch the parameter you want to display. 4. When finished, touch the Apply button. B.6.2 Status Parameter Details Status Parameter Description Eluent time The number of hours the eluent supply will last, if the pump runs continuously at the current flow rate.
ICS-2100 Ion Chromatography System 222 Status Parameter Description EGC1 life EGC2 life The percentage of ions remaining in the EluGen cartridge (EGC1 or EGC2). When the EGC-2 power supply is configured as an auxiliary power supply, the EGC2 life field will display N/A. Cell temp The temperature of the cell heater (°C), followed by a status symbol (=, ↑, or ↓). Column temp The temperature of the column heater (°C), followed by a status symbol (=, ↑, or ↓). Doc.
B • Touch Screen Operation B.7 Pump Page Use the PUMP page to set parameters related to pump operation, including pressure limits, pressure unit, vacuum degas pump settings, and eluent valve control. To open this page, select PUMP from the menu of pages. The current system pressure is displayed at the top of the screen. Current system pressure Figure B-13. ICS-2100 Touch Screen Pump Page B.7.
ICS-2100 Ion Chromatography System • To change the low pressure limit, touch the LOW field and enter the desired limit on the number pad. To select the pressure unit for all touch screen pages that display pressure values, touch the pressure unit field and select the desired unit on the list (PSI, bar, or MPa) (see Figure B-14). Select the pressure unit Figure B-14. Pump Page: Selecting the Pressure Unit B.7.
B • Touch Screen Operation 3. Select the desired option: Always Off: The degas pump is always off. Always On: The degas pump is always on. This setting is reserved for test purposes by a Dionex Service Representative. Select the Degas, Always On option only when testing the vacuum degas assembly. Do not select the Always On option for routine use. Duty Cycle: The degas pump cycles on and off according to the times specified in the Duty Cycle and Time Off fields.
ICS-2100 Ion Chromatography System B.8 Eluent Generator Page Use the ELUENT GENERATOR page to set the eluent concentration of each installed EluGen cartridge (EGC). You can also enter the serial number and view the expiration date and remaining life of each cartridge. This page also provides on/off control of a Continuously Regenerated Trap Column (CR-TC). To open the page, touch the EGC button on the HOME page or select EGC from the menu of pages.
B • Touch Screen Operation If the ICS-2100 is not under Chromeleon control, enter the cartridge serial number by touching the Serial Number field on the ELUENT GENERATOR page (see Figure B-16) and entering the serial number on the keypad. If you are reinstalling a cartridge that was used previously, touch the down arrow instead of the number field. A list of the last five entered serial numbers drops down. Choose the serial number of the cartridge from the list.
ICS-2100 Ion Chromatography System NOTE When the EGC-2 power supply is configured as an auxiliary power supply, the EGC-2 Setpoint and Actual Concentration fields display zeros. B.8.3 Controlling the Eluent Generator Power • To manually control the eluent generator power, touch the EGC Off and On buttons on the ELUENT GENERATOR page. • To automatically control the eluent generator power simultaneously with the pump flow, select Auto turn on with pump.
B • Touch Screen Operation below 30%. At 0%, an error message informs you that the ion count is depleted and the cartridge must be replaced before continuing operation. NOTE When the EGC-2 power supply is configured as an auxiliary power supply, the EGC-2 Life Remaining field is blank. • Normalized Life Used (displayed when an EPM is installed) indicates how much the EPM has been used. The value starts at 0 and counts up with use.
ICS-2100 Ion Chromatography System B.9 Suppressor Page Use the SUPPRESSOR page to specify the type of suppressor installed in the ICS2100, turn the suppressor on and off, and select the amount of current supplied to the suppressor. To open this page, touch the suppressor button on the HOME page, or select SUPPRESSOR from the menu of pages. Figure B-18. Suppressor Page Suppressor Controls • • The suppressor type is typically selected at initial installation and does not need to be changed.
B • Touch Screen Operation NOTE When Chromeleon is used to control the ICS-2100, the Program Wizard automatically calculates the current required for the application. • • To manually control the suppressor power, touch the Off and On buttons. To automatically control the suppressor power simultaneously with the pump flow, select Automatically turn on with pump. NOTE The suppressor always turns off when the pump is off, regardless of whether the “Automatically turn on with pump” option is selected. B.
ICS-2100 Ion Chromatography System B.10.1 Setting the Data Rise Time The data rise time determines the amount of filtering performed on the conductivity data. The rise time is a measure of how quickly the detector responds to a change in signal, and is defined as the time it takes the output signal to rise from 10% of its final value to 90% of its final value.
B • Touch Screen Operation B.10.3 Setting Analog Out Options The analog output connector on the ICS-2100 rear panel outputs an analog voltage signal proportional to the conductivity measured by the cell. The output is filtered using the selected data rise time (see Section B.10.1). The analog output can be connected to an analog-todigital converter device, such as an integrator or a chart recorder.
ICS-2100 Ion Chromatography System B.11 Information Page The INFORMATION page displays the version numbers of the ICS-2100 control programs (Moduleware and Boot Block), the serial number of the ICS-2100, and the options that are installed in the ICS-2100. The INFORMATION page is displayed at start-up. You can open the page from the menu of pages at any time. Figure B-20. Information Page Moduleware is the firmware program installed in the ICS-2100 that controls instrument functions.
B • Touch Screen Operation B.12 Module Setup Page The MODULE SETUP page lets you select options for the touch screen display and conductivity readings. To open this page, select SETUP from the menu of pages. Figure B-21. Module Setup Page Module Setup Options • • Backlight Duration: Select 2-hour time-out to turn off the backlight after 2 hours if the touch screen is not used during that time. Select Always On to have the backlight remain on continuously.
ICS-2100 Ion Chromatography System B.13 Input/Output Page The INPUT/OUTPUT page provides control of the ICS-2100 TTL inputs and TTL and relay outputs. To open this page, select INPUT/OUTPUT from the menu of pages. For details about relay and TTL control, see Appendix C. Figure B-22. Input/Output Page B.14 Diagnostic and Calibration Pages Diagnostic and calibration functions can be performed either from the touch screen diagnostic and calibration pages or from the Chromeleon Wellness Panel.
B • Touch Screen Operation Figure B-23. System Diagnostic Menu Page NOTE When the EGC-2 power supply is configured as an auxiliary power supply, pressing the EGC2 Verification button has no effect. NOTE The Service button provides access to service functions that are performed only by Dionex personnel. An access code is required to go to the service pages. Doc.
ICS-2100 Ion Chromatography System 238 Doc.
C • TTL and Relay Control C.1 TTL and Relay Connections A 12-pin connector strip for TTL/relay control is located on the ICS-2100 rear panel. The connector provides two relay outputs, two TTL outputs, and four TTL inputs (see Figure C-1).
ICS-2100 Ion Chromatography System The outputs can be used to control functions in external devices such as an autosampler or another Dionex module.
C • TTL and Relay Control b. Plug the connector into the 12-pin connector on the ICS-2100 rear panel. c. Connect the wires from the ICS-2100 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. 3.
ICS-2100 Ion Chromatography System C.1.1 Selecting TTL Input Functions and Control Types To select TTL input functions and the control type from Chromeleon, open the Chromeleon Server Configuration program and double-click the ICS-2100 icon under the timebase. Select the TTL Inputs tab (see Figure C-3). Figure C-3. ICS-2100 Server Configuration Properties: TTL Inputs 242 Doc.
C • TTL and Relay Control To select TTL input functions and the control type from the touch screen, go to the INPUT/OUTPUT touch screen page (see Figure C-4). Select a Function Select a Control Type Figure C-4. Input/Output Page: Selecting TTL Functions TTL Input Control Types The ICS-2100 TTL inputs respond to four types of signals to accommodate different controlling devices. The default control type, Normal Edge, is compatible with the output signals provided by Dionex modules.
ICS-2100 Ion Chromatography System The action of the positive (rising) edge depends on the function: For the Load/Inject function, the rising edge switches the injection valve to the Inject position. For the Pump On function, the rising edge turns off the pump (and suppressor). For Autozero and Mark, the rising edge has no effect. • • Inverted Edge: The inverted edge mode works identically to the normal edge mode except that the positive and negative edges are reversed in function.
C • TTL and Relay Control C.2 Controlling TTL and Relay Outputs The ICS-2100 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. The relay-contact closures are normally open. When the relay is closed, current flows to the connected device.
ICS-2100 Ion Chromatography System C.3 Example Setup for Stand-Alone Operation This section describes an example setup for stand-alone operation (operation without Chromeleon software) with an AS Autosampler and a third-party analogto-digital converter and controller. If your configuration includes different devices, use the following steps as guidelines and refer to your product documentation for specific connection details.
C • TTL and Relay Control AS Rear Panel Connections ICS-2100 Rear Panel Connections + ANALOG OUTPUT - 1 RLY 2 OUT 2 RELAY OUT RLY 1 OUT 3 2 TTL 1 IN (+) TTL 2 IN (+) TTL 3 IN (+) TTL 4 IN (+) TTL 2 OUT (+) TTL 1 OUT (+) 1 TTL IN/OUT (-) 4 TTL OUT (+) TTL IN (+) TTL GND (-) 1 1 2 5 6 1 7 red: pos. 7,8,9 2 8 3 9 4 10 1 11 2 12 black: 2 3 4 5 6 7 8 9 10 11 12 black pos. 4,11,12,12 red pos. 1,3,5,6 Inject Pump On/Off Autozero Start/Continue Schedule pos.
ICS-2100 Ion Chromatography System Assign ICS-2100 Input Functions Go to the ICS-2100 INPUT/OUTPUT touch screen page and verify that the Inject function is assigned to TTL input 1, that Autozero is assigned to TTL input 2, and that the TTL Input Control Type is Normal Edge (see Figure C-7). Figure C-7. Input/Output Page Enable AS Control of the Injection Valve 1. On the AS front panel, press Menu and 0 to go to the TIME FUNCTION OUT screen. In the LOAD/INJECT VALVE: TTL 1 field, select ENABLED.
C • TTL and Relay Control Connect the Analog Output 1. Locate the analog cable for the third-party analog-to-digital converter and controller. 2. Connect the analog input connector on the third-party controller to the ANALOG OUTPUT connector on the ICS-2100 rear panel (see Figure C-6). Configure the ICS-2100 Analog Output Go to the ICS-2100 DETECTOR touch screen page and select the settings shown in Figure C-9: Figure C-9.
ICS-2100 Ion Chromatography System Timed Event Notes: • • • • At time INIT, the injection valve is set to Load. At time 0.00, the injection valve is set to Inject, an autozero is performed (TTL2=1), the data acquisition mark is sent (RLY1=1), and the pump is turned on (RLY2=1). At time 0.5, TTL2 and RLY1 are switched back to 0 to be ready for the next run. RLY2 remains at 1 to keep the pump on.
D • 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 Check valve cartridges 052840 Piston 055870 Piston seal 048722 Piston rinse seal 055752 O-ring for waste valve or priming valve 057945
ICS-2100 Ion Chromatography System Part Number Item 058069 EGC holder and degas assembly Sample Loop and Injection Valve 042857 25-μL sample loop 057968 Injection valve 024305 Luer adapter fitting, 1/4-28 (for manual injections) 016388 1-cc syringe (for manual injections) 057896 Injection Valve Rebuild Kit Auxiliary Valve 069472 Auxiliary Valve Kit (6-port valve) 069473 Auxiliary Valve Kit (10-port valve) 057896 Injection Valve Rebuild Kit (for use with auxiliary valve, also) 061947 Au
D • Reordering Information Part Number Item 043598 Twisted pair of wires Miscellaneous 954745 IEC 127 fast-blow fuses, rated 3.15 amps 060494 USB cable, 5 m (16 ft) 060392 External USB hub 057954 ICS-2100 Preventive Maintenance Kit 060581 AS Preventive Maintenance Kit 055647 AS-DV Preventive Maintenance Kit Preventive Maintenance Kits Doc.
ICS-2100 Ion Chromatography System 254 Doc.
E • FAQ E.1 How do I hook up an autosampler? For instructions on how to connect the ICS-2100 to an autosampler, refer to the ICS-2100 installation instructions. Also refer to the autosampler operator’s manuals, which are included on the Dionex Reference Library CD-ROM (P/N 053891). E.2 How do I print? Click the Print toolbar button in Chromeleon. E.3 Why are the retention times moving? Retention times can shift if the pump flow is erratic or if the column or eluent is contaminated. See Section 4.
ICS-2100 Ion Chromatography System E.6 When should I replace the eluent generator cartridge? The ICS-2100 monitors EluGen cartridge use and displays a message when it is time to replace the cartridge. The message appears on the front panel screen and in the Chromeleon Audit Trail. To view the remaining cartridge life, click EG Settings on the Chromeleon Control panel, or go to the touch screen ELUENT GENERATOR page (see Section B.8). E.
E • FAQ E.12 How do I know when a column is dirty? See the troubleshooting section of the column manual. E.13 How do I clean a column? See the troubleshooting section of the column manual. E.14 Why is the conductivity high? Possible reasons for high conductivity include: • • The suppressor is not on. Turn on the suppressor from the Chromeleon Control panel or the ICS-2100 touch screen SUPPRESSOR page. The suppressor needs regeneration. See the suppressor manual for troubleshooting information.
ICS-2100 Ion Chromatography System 258 Doc.
F • 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. Capacity Factor (k´) The number of column volumes of eluent, pumped through the column, required to elute an analyte.
ICS-2100 Ion Chromatography System Cell Constant (k) A factor determined experimentally by measuring the conductance (G) of a standard solution of known equivalent conductivity (k). k = κ⁄G The value of k depends upon the surface area of, and distance between, the electrode faces in the conductivity detector cell.
F • 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. Units are siemens. Counterion Ions carrying a charge opposite that of the sample ions (e.g., Na+) may be the counterion of a Cl- analyte.
ICS-2100 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. These resins have a low ion-exchange capacity. Pre-Column Synonymous with Guard Column.
F • 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 oC change in temperature. Every solution has a characteristic temperature coefficient which is determined experimentally. Theoretical Plates (N) See Column Efficiency.
ICS-2100 Ion Chromatography System 264 Doc.
Index Symbols % Offset (analog out), 233 A Adjusting the contrast, 12, 207 Air particulate samples, 61 Alarm conditions, 74 – 85 See also Error messages Ambient temperature, 96 Analog output, 231, 233, 240 % Offset, 233 Configuring, 233, 249 Connections, 249 Connector, 21 Full-scale, 233 Range, 233 Analog-to-digital controller, 249 Anion separations, 37, 60 Application Wizard, 67 AS Autosampler, 62 Connections for stand-alone operation, 246 Enabling injection valve control, 248 Maintenance, yearly, 69 Met
ICS-2100 Ion Chromatography System Backlight Time-out, 235 Backpressure, 36 Restriction in plumbing, 109 Troubleshooting, 92 Backpressure coil, 40 Backpressure, low How to increase, 40 Bar, 224 Baseline Drift, 96 Noise, 96, 232 Stability, 46 Zeroing, 215 Batch processing, 50 Blockages Liquid lines, 82, 109 Busy page, 235 C Cables Power cord, 142 Calibration, 99 Conductivity cell, 103 Flow rate, 106 Vacuum degas assembly, 108 Carbonate eluent, 23, 37, 41 Carbonate/bicarbonate eluent, 23, 37, 41 Cation separ
Index Conductivity cell, 19 – 20, 46 Calibrating, 103 Calibration constant, 128 High cell output, 95 Leaking, 87 No response, 94 Replacement procedure, 127 Setting the temperature, 215 Volume, 46 Conductivity cell specifications Active volume, 200 Cell body, 200 Chemical compatibility, 200 Electrodes, 200 Maximum pressure, 200 Temperature, 200 Conductivity polarity, 232 Contacting Dionex, 99 Contamination Column, 92, 94 Eluents, 93 Sample, 94 Standard, 93 Continuously Regenerated Trap Column See CR-TC Contr
ICS-2100 Ion Chromatography System E EGC, 16 Backpressure requirement, 40, 43 Concentration ranges, 38 Concentration upper limits, 78, 227 EGC-1 connector, 16, 148, 156 EGC-2 connector, 16 Eluent types, 37 Entering the serial number, 226 Expiration date, 228 Home page controls, 214 Life remaining percentage, 228 Service area, 17 See also Eluent generator EGC alarms EGC board not present, 77 EGC-1 calibration error, 78 EGC-1 disconnected error, 78 EGC-1 invalid concentration vs.
Index Column heater open circuit, 76 Column heater short circuit, 76 CR-TC over current error, 76 CR-TC stopped for zero flow rate, 77 Degas calibration failed, 77 EGC board not present, 77 EGC-1 calibration error, 78 EGC-1 disconnected error, 78 EGC-1 invalid concentration vs.
ICS-2100 Ion Chromatography System I ICS, 52 Information page, 234 Injecting samples, 62 Via autosampler, 64 Via syringe, 63 Via vacuum syringe, 64 Injection port, 11 Injecting via syringe, 63 Injection valve, 19, 42 Controlling with an AS, 248 Home page controls, 215 Leaking, 87 Passages blocked, 93 Plumbing connections, 43 Rebuilding, 114 Specifications, 202 Troubleshooting, 80 Input/Output page, 236, 248 Installation Analog output connection, 249 Priming, 138, 140 Stand-alone operation setup, 246 – 247
Index MPa, 224 MSA EGC, 37 N NaOH EGC, 37 Nitrite in samples, 61 Noise, baseline, 232 Normal edge TTL input control, 243 Normal pulse TTL input control, 244 O Offset conductivity, 235 Offset percentage (analog out), 233 Offsetting background conductivity, 59, 215 Operating features, 11 Operating humidity, 196 Operating ranges Cell heater, 19, 215 Column heater, 20, 214 Eluent concentration, 78, 227 Flow rate, 19, 213 Operating temperature, 196 Operation Equilibration time, 59 Overview, 49 Priming, 57, 140
ICS-2100 Ion Chromatography System Replacing tubing and fittings, 113 Troubleshooting, 109 Polarity Selecting the conductivity polarity, 232 Potassium carbonate eluent, 41 Potassium hydroxide eluent, 37 Power cord, 142 Power receptacle, 22 Power requirements, 195 Pressure Home page display, 212 Limit, 83, 212, 223 System, 83, 223 Unit (selecting), 223 Pressure transducer, 19, 36 Leaking, 87 System backpressure, 36 Prime button, 213 Priming, 57, 138, 140 – 141 Pump is out of prime, 89 With a syringe, 138 Wit
Index R Range, 217, 233 Rear panel, 21 Analog output connector, 21 Power receptacle, 22 USB connections, 21 Rebuilding the auxiliary valve, 114 Rebuilding the injection valve, 114 Recorders Analog output setting, 233 Relay connections Rear panel connector, 22, 239 Relay outputs Controlling, 245 Voltage and current specifications, 240 Remote Mode, 216 Reordering information, 251 Reproducibility, 46 Reservoir Connecting, 56 Monitoring liquid level in, 54 Restriction in liquid lines, 82, 109 Retention time Ad
ICS-2100 Ion Chromatography System Rebuilding the auxiliary valve, 114 Rebuilding the injection valve, 114 Replacing tubing and fittings, 113 Suppressor replacement, 130 Tubing and fittings replacement, 113 Waste valve O-ring replacement, 125 Signal-to-noise ratio, 232 Sodium hydroxide eluent, 37 Software control, 30 Modes of, 31 Software specifications Application templates, 204 Automated procedure wizards, 204 Automation support for third-party vendors, 204 Customizable system control panels, 204 Customiz
Index T Technical Support, 71, 99 Temperature Cell heater, 46, 215 Column heater, 20, 45, 214 Minimizing the effect of variations, 46 Temperature compensation, 46 Temperature, operating, 196 Timebase, 30 Time-out (screen), 235 Top cover, 16 Total conductivity, 215, 235 Touch screen, 11, 207 Adjusting the contrast, 12, 207 Number keypad, 13, 208 Operation, 12, 207 Specifications, 196 Time-out, 235 Using with Chromeleon, 210 Touch screen pages Busy page, 235 Detector page, 231 Diagnostic pages, 236 Eluent Ge
ICS-2100 Ion Chromatography System See Waste valve Version number, 234 W Warranty, voiding, 99, 114, 116 Waste container, 185 Waste lines Blocked, 86 Gas separator waste tube, 37 Waste valve, 35 Opening, 35, 120 O-ring replacement procedure, 125 Water samples, 61 Weekly maintenance, 68 Weight, 195 Wellness, 31 Wellness panel, 99 Y Yearly maintenance, 69 Z Zero position (analog out), 233 Zeroing the baseline, 215 Index-12 Doc.