Dionex ICS-1100 Ion Chromatography System Operator’s Manual Document No.
© 2012 by Thermo Fisher Scientific Inc. All rights reserved. AES, AMMS ICE, ASRS, Chromeleon, Dionex, IonPac, OnGuard, and SRS are registered trademarks of Thermo Fisher Scientific Inc. in the United States. Microsoft, Windows, Windows 2000, and Windows XP are registered trademarks of Microsoft Corporation in the United States and other countries. Adobe, Acrobat, and Adobe Reader are registered trademarks of Adobe Systems, Incorporated in the United States and other countries.
Contents 1 • Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 1.1 Introduction to Ion Chromatography (IC) . . . . . . . . . . . . . . . . . . . . . . . . 1 1.2 Overview of the Dionex ICS-1100 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 1.3 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.3.1 1.4 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . .
Dionex ICS-1100 Ion Chromatography System 2.4 System Component Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .26 2.4.1 Vacuum Degas Assembly (Optional) . . . . . . . . . . . . . . . . . . . .26 2.4.2 Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28 2.4.3 Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .28 2.4.4 Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Contents 3.7 Set System Operating Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46 3.8 Equilibrate the System and Verify Operational Status . . . . . . . . . . . . . 46 3.9 Prepare Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47 3.9.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . . . . 47 3.9.2 Pretreating Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48 3.9.
Dionex ICS-1100 Ion Chromatography System 4.8 Excessive System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73 4.9 Peak “Ghosting” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .74 4.10 Nonreproducible Peak Height or Retention Time . . . . . . . . . . . . . . . . .75 4.11 Abnormal Retention Time or Selectivity . . . . . . . . . . . . . . . . . . . . . . . .75 4.12 No Cell Response . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Contents 5.11 Replacing the Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106 5.12 Replacing the Column Heater . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107 5.13 Replacing the Column Heater Heat Exchanger . . . . . . . . . . . . . . . . . . 109 5.14 Replacing the Eluent Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110 5.15 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112 5.
Dionex ICS-1100 Ion Chromatography System A.13 Suppressors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .125 A.14 Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .126 A.15 System Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .126 B • TTL and Relay Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .129 B.1 TTL and Relay Connections . . . . . . . . .
Contents D.13 How do I clean a column? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141 D.14 Why is the conductivity high? . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141 D.15 How do I configure and operate the auxiliary valve? . . . . . . . . . . . . . 141 E • Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143 Index Doc.
Dionex ICS-1100 Ion Chromatography System viii Doc.
1 • Introduction 1.1 Introduction to Ion Chromatography (IC) The Thermo Scientific Dionex™ ICS-1100 Ion Chromatography System (Dionex ICS-1100) performs ion analyses using suppressed or non-suppressed conductivity detection. An ion chromatography system typically consists of a liquid eluent, a high-pressure pump, a sample injector, a guard and separator column, a chemical suppressor, a conductivity cell, and a data collection system.
Dionex ICS-1100 Ion Chromatography System A typical IC analysis consists of six stages (see Figure 1-1). 6. Data Analysis Conductivity Cell 5. Detection Suppressor 4. Suppression Eluent 1. Eluent Delivery 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 3. Separation • As the eluent and sample are pumped through the separator column, the sample ions are separated. In the Dionex ICS-1100, the mode of separation is called ion exchange. This is based on the premise that different sample ions migrate through the IC column at different rates, depending upon their interactions with the ion exchange sites. 4.
Dionex ICS-1100 Ion Chromatography System 1.2 Overview of the Dionex ICS-1100 The Dionex ICS-1100 is an integrated ion chromatography system containing a pump, injection valve, and conductivity detector. Other system components, including a guard column, separator column, and suppressor vary, depending on the analyses to be performed. The Dionex ICS-1100 can optionally be configured with a column heater for temperature control of the column.
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.
Dionex ICS-1100 Ion Chromatography System Appendix E Glossary 1.3.1 Defines terms commonly used in ion analysis. 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. Indicates an imminently hazardous situation which, if not avoided, will result in death or serious injury.
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.
Dionex ICS-1100 Ion Chromatography System 1.4 Safety and Regulatory Information The Dionex ICS-1100 was manufactured by Thermo Fisher Scientific at the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The Dionex ICS-1100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of a Dionex ICS-1100 in a manner not specified by Thermo Fisher Scientific may result in personal injury.
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.
Dionex ICS-1100 Ion Chromatography System 10 Doc.
2 • Features This chapter describes key Dionex ICS-1100 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 Dionex ICS-1100. Injection Port The sample to be analyzed can be injected manually into the injection port, using a syringe. For automated sample injection, the Dionex ICS-1100 must be connected to an autosampler. For more information about sample injection, see Section 3.10.
Dionex ICS-1100 Ion Chromatography System INJECT VALVE STATUS Load Module Connected Inject Acquiring Data Pump Suppressor ALARM Column Heater Figure 2-2. Status LEDs LED Label If On (Green) If Flashing Load Injection valve is in Load position. Valve error. Inject Injection valve is in Inject position. Valve error. Alarm This LED does not have an “on” (green) state. Error detected. Check the Chromeleon Audit Trail for the cause.
2 • Features 2.1.2 Top Cover Figure 2-3 illustrates the top cover of the Dionex ICS-1100. Reservoir Storage Eluent Reservoir The Dionex ICS-1100 top cover has room for up to three 2-L plastic reservoirs (P/N 044129) or one 4-L plastic reservoir (P/N 039164). Tubing Chase The tubing chase under the top cover routes tubing to the front of the Dionex ICS-1100. Figure 2-3. Dionex ICS-1100 (Top View) Doc.
Dionex ICS-1100 Ion Chromatography System 2.1.3 Component Panel Figure 2-4 shows the user-accessible components installed on the component panel behind the Dionex ICS-1100 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 the Alarm LED flashes. Pump Heads The Dionex ICS-1100 includes a dual-piston serial pump. The flow rate can be set to 0.00 mL/min or to between 0.05 and 5.00 mL/min.
Dionex ICS-1100 Ion Chromatography System Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either a Dionex AES™ Atlas Electrolytic Suppressor, Dionex SRS™ SelfRegenerating Suppressor, or Dionex MMS™ MicroMembrane™ Suppressor can be used with the Dionex ICS-1100. See Section 2.4.7 for details about the suppressor.
2 • Features 2.1.4 Right-Side Panel Figure 2-5 illustrates the RFIC-ER compartment on the right side of the Dionex ICS-1100. Figure 2-5. RFIC-ER Compartment (Cover Removed) The compartment houses the ER Controller (ERC 10) and various columns required for operation in the RFIC-ER mode. The ERC 10 electronics monitor the volume of electrolysis gases (such as hydrogen and oxygen) in the eluent stream.
Dionex ICS-1100 Ion Chromatography System special eluent bottle, etc.) required for RFIC-ER operation. For more information, refer to the manual shipped with the Installation Kit. 2.1.5 Rear Panel Figure 2-6 illustrates the Dionex ICS-1100 rear panel. Tubing Clips Power Switch Upper Chase Analog Output Connector Waste Lines (3) USB Connectors TTL and Relay Connector Strip Main Power Receptacle Lower Chase Figure 2-6.
2 • Features USB Connectors A USB receptacle is provided to allow connection to the Chromeleon computer. Two USB ports are provided for connecting to other USB devices. For connection instructions, refer to the Dionex ICS-1100 installation instructions. 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.
Dionex ICS-1100 Ion Chromatography System 2.2 Flow Schematics The following figures illustrate the liquid flow path through a Dionex ICS-1100 when using suppression in autorecycle mode. Two configurations are shown: • • Figure 2-7 illustrates the liquid flow path through components when performing conventional ion chromatography. Figure 2-8 illustrates the liquid flow path through components when operating in the RFIC-ER mode.
2 • Features WASTE 1 ELUENT OUT OUT 2 5 12 IN 7 SEPARATOR COLUMN PULSE DAMPER COLUMN HEATER (optional) SAMPLE 11 IN COND OUT CELL HEAT EXCHANGER IN 8 SUPPRESSOR OUT 6 GUARD 9 OUT 3 PUMP HEAD PUMP HEAD IN WASTE 4 OUT PRESS. XDUCER Figure 2-7. Dionex ICS-1100 Flow Schematic: Standard Configuration Doc.
Dionex ICS-1100 Ion Chromatography System Flow Description for RFIC-ER Mode • Eluent from the eluent reservoir flows first through the pump degas assembly (if it is installed) and then through the eluent valve to the pump. The eluent is then pushed through the pressure transducer, which measures the system pressure. • From there, the eluent is pushed through a pulse damper , which smooths minor pressure variations from the pump to minimize baseline noise.
2 • Features IN ER3b IN OUT 2 SUPPRESSOR IN 12 IN COND OUT CELL SAMPLE 9 ER3a IN HEAT EXCHANGER OUT OUT PULSE DAMPER 5 IN ER2 IN 8 7 SEPARATOR COLUMN ELUENT COLUMN HEATER (optional) ERC 10 1 6 IN 10 GUARD ER1 OUT 3 PUMP HEAD PUMP HEAD IN WASTE 4 OUT PRESS. XDUCER Figure 2-8. Dionex ICS-1100 Flow Schematic: RFIC-ER Mode Doc.
Dionex ICS-1100 Ion Chromatography System 2.3 Chromeleon and Chromeleon Xpress The Dionex ICS-1100 is controlled by a PC configured with Chromeleon Chromatography Management System or Chromeleon Xpress. Chromeleon Chromatography Management System provides complete instrument control, data acquisition, and data management. Chromeleon Xpress provides real-time control and monitoring of 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 Dionex ICS-1100 is connected to a Dionex AS, Dionex AS-AP, Dionex AS-DV, or Dionex AS-HV Autosampler) provides access to autosampler functions. To open the panel tabset, use one of the methods below: • • 2.3.
Dionex ICS-1100 Ion Chromatography System 2.4 System Component Details This section provides details about Dionex ICS-1100 system components, including the vacuum degas assembly (optional), RFIC-ER components, eluent valve, pump, injection valve, column heater (optional), suppressor, and conductivity cell. 2.4.1 Vacuum Degas Assembly (Optional) The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user.
2 • Features Select the Options tab (see Figure 2-10). . Figure 2-10. 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 Thermo Fisher Scientific 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.
Dionex ICS-1100 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). This lets you perform service procedures on pump components without eluent leaks occurring. Figure 2-11. 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 2-12. Dionex ICS-1100 Pump Components Secondary Pump Head The secondary pump head delivers eluent to the remainder of the chromatography system (the injection valve, column, and detector). The waste valve is located on the front of the secondary pump head (see Figure 2-12). To open the waste valve, turn the knob one-quarter to one-half turn counterclockwise.
Dionex ICS-1100 Ion Chromatography System Pressure Transducer Flow exiting the secondary pump head is directed to the pressure transducer (see Figure 2-12), 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. The system pressure should remain consistent (no more than a 3% difference from one pressure reading to the next).
2 • Features LOAD POSITION Sample In Sample In INJECT POSITION To Column To Column Sample Loop To Waste Sample Loop From Pump To Waste From Pump Figure 2-13. Injection Valve Flow Schematics Eluent flows through either the Load or Inject path, depending on the valve position. • • In the Load position, sample is loaded into the sample loop, where it is held until injection. Eluent flows from the pump, through the valve, and to the column, bypassing the sample loop.
Dionex ICS-1100 Ion Chromatography System Figure 2-14. Injection Valve Plumbing 2.4.5 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 2.4.6 Column Heater (Optional) The column heater provides temperature control for the separator and guard column. The heater temperature can be set to between 30 °C and 60 °C. However, the set temperature must be at least 5 °C above the ambient temperature. A thermistor mounted in the heater block monitors the temperature. Setting the temperature to 0 °C turns off the column heater.
Dionex ICS-1100 Ion Chromatography System 2.4.7 Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions, thereby increasing detection sensitivity. Either a Dionex Atlas Electrolytic Suppressor, Dionex Self-Regenerating Suppressor, or Dionex MicroMembrane Suppressor can be used with the Dionex ICS-1100. 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 2-4). 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. 2.4.
Dionex ICS-1100 Ion Chromatography System 36 Doc.
3 • Operation and Maintenance This chapter describes routine operating and maintenance procedures for the Dionex ICS-1100. The Dionex ICS-1100 is designed for IC (ion chromatography) applications and should not be used for any other purpose. Operation of the Dionex ICS-1100 in a manner not specified by Thermo Fisher Scientific may result in personal injury. 3.1 Operation Overview Figure 3-1 illustrates the basic steps for routine operation of the Dionex ICS-1100.
Dionex ICS-1100 Ion Chromatography System Sample Processing Overview Samples can be run manually (one at a time), or they can be grouped and run automatically in batches. Figure 3-2 shows the typical steps for manual and batch sample processing.
3 • Operation and Maintenance 3.2 Turning On the System Power Press the power switch on the Dionex ICS-1100 rear panel (see Figure 3-3) to turn on the system power. Table 3-2 shows the Dionex ICS-1100 conditions at power-up. Power Switch Also turn on the power to the computer and the autosampler (if used). Figure 3-3. Dionex ICS-1100 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.
Dionex ICS-1100 Ion Chromatography System 3.3 Connecting to Chromeleon NOTE If you are beginning operation of a Dionex ICS-1100 that has not been configured in a timebase, refer to the Dionex ICS-1100 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. Dionex ICS-1100 Control Panel on the Chromeleon Panel Tabset Doc.
Dionex ICS-1100 Ion Chromatography System 3.4 Set Up the Eluent Reservoir NOTE If you plan to operate the system in the RFIC-ER mode, disregard the instructions here. Follow the instructions provided with your RFIC-ER Installation Kit to set up the RFIC-ER eluent reservoir. 3.4.1 Prepare the Eluent Prepare the eluent according to the instructions in the column manual. Column manuals are included on the Dionex Reference Library CD-ROM (P/N 053891). 3.4.
3 • Operation and Maintenance 6. Install an end-line filter on the eluent line (see Section 3.4.3). 7. (Optional) Pressurize the reservoir. The Dionex ICS-1100 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).
Dionex ICS-1100 Ion Chromatography System 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 Dionex ICS-1100 does not automatically detect when the reservoir is filled, nor when it is empty. Enter the volume of liquid in the reservoir (in liters) Note: The Eluent Bottle field and slider gauge are updated as the liquid is depleted. Figure 3-5. Pump Settings Window: Setting the Eluent Level 3.4.
3 • Operation and Maintenance 3.6 Prime the Pump If you changed eluent or if the eluent lines are dry, prime the lines first with a syringe before following the procedure below to prime the pump. See Section 5.16.1 for instructions on priming the lines with a syringe. 1. Verify that the priming valve on the primary pump head (see Figure 3-6) is closed (turned all the way clockwise). 2. Open the waste valve on the secondary pump head by turning the knob onequarter to one-half turn counterclockwise.
Dionex ICS-1100 Ion Chromatography System 3.7 Set System Operating Conditions NOTE This section is an overview of the steps needed to start up the system and begin running samples. Actual operating parameters (flow rate, cell heater temperature, suppressor current, etc.) depend on the application to be run. Refer to the column manual for the required parameters for your application. Set or verify system operating parameters from the Chromeleon Control panel.
3 • Operation and Maintenance • • • If the pressure is less than the expected amount, gas may be trapped in the system. To release the gas, remove the pump fitting on the injection valve port, labeled P (2). Allow the air to escape and then reconnect the fitting. If the pressure fluctuates by more than about 0.13 MPa (20 psi), prime the pump. See Section 4.4 for additional troubleshooting information. If the pressure is too high, there may be a restriction in the system plumbing. See Section 4.
Dionex ICS-1100 Ion Chromatography System time. Refrigerating the samples at 4C (39 F) will reduce, but not eliminate, bacterial growth. Analyze samples containing nitrite or sulfite as soon as possible. Nitrite oxidizes to nitrate, and sulfite to sulfate, thus increasing the measured concentrations of these ions in the sample. In general, samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant changes in anion concentrations. 3.9.
3 • Operation and Maintenance 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 Dionex ICS-1100 front door.
Dionex ICS-1100 Ion Chromatography System 3.10.1 Loading Samples with a Syringe 1. Make sure the injection port on the Dionex ICS-1100 front door (see Figure 2-1) is connected to sample port S (5) on the injection valve (see Figure 3-7). Figure 3-7. Injection Valve Connections 2. Fill the 1 cc syringe (P/N 016388) provided in the Dionex ICS-1100 Ship Kit (P/N 057905) with a calibration standard or sample. 3. Insert the syringe into the injection port on the Dionex ICS-1100 front door (see Figure 2-1). 4.
3 • Operation and Maintenance 3.10.2 Loading Samples with a Vacuum Syringe 1. Disconnect the waste line from port W (6) of the injection valve (see Figure 3-7) and attach a shorter line: 25 to 30 cm (10 to 12 inches) of PEEK or PTFE (polytetrafluoroethylene) tubing. 2. Place the free end of the line into the sample. 3. Verify that the injection valve is in the Load position. 4.
Dionex ICS-1100 Ion Chromatography System 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). Automatically: Include the Inject command in a Chromeleon program. (If necessary, refer to the Chromeleon Help or user manual for assistance.) 3.
3 • Operation and Maintenance Saving Manual Data NOTE Chromeleon Xpress does not allow data to be saved. If you are using Chromeleon, data from manual processing is saved in the manual sequence under the timebase folder in the local datasource. To save the data from a manual run: 1. Select the manual folder and select File > Save As. 2. Enter a new name for the sequence. 3. Select the Save raw data check box. 4. Click Save. 3.11.
Dionex ICS-1100 Ion Chromatography System Summary of Automatic Sample Processing 1. Complete the instructions in Section 3.2 through Section 3.8 to prepare the Dionex ICS-1100 for operation and to prepare the sample for processing. 2. If an autosampler is installed, prepare and fill the sample vials and place them in the autosampler tray or cassette. Refer to the autosampler manual for detailed instructions. Autosampler manuals are provided on the Thermo Scientific Reference Library DVD (P/N 053891). 3.
3 • Operation and Maintenance 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.
Dionex ICS-1100 Ion Chromatography System • Check the waste container daily and empty when needed. Weekly • • • Once a week, check fluid lines for crimping or discoloration. Replace any pinched lines. Replace damaged lines. Check the junctions between the pump heads and the pump casting for evidence of liquid leaks. If the piston seal wash tubing is not connected, check the drain tubes at the rear of the pump heads for evidence of moisture.
3 • Operation and Maintenance • If a Dionex AS-DV Autosampler is installed, replace the tip and tubing. The Dionex AS-DV Preventive Maintenance Kit (P/N 055647) contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve. Instructions are included with the kit. Doc.
Dionex ICS-1100 Ion Chromatography System 58 Doc.
4 • Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the Dionex ICS-1100. Turn to the section of this chapter that best describes the operating problem or symptom that has been observed. Each section lists possible causes of the problem or symptom in order of probability. A systematic troubleshooting approach is the most effective way to determine the root cause.
Dionex ICS-1100 Ion Chromatography System The table below lists the most frequently observed Dionex ICS-1100 error messages. For troubleshooting assistance, refer to the page indicated in the table.
4 • Troubleshooting 4.2 Troubleshooting Error Messages COLUMN HEATER EXCEEDS SAFE TEMPERATURE This error occurs when the column heater temperature is higher than the maximum allowed. This error may occur if the Dionex ICS-1100 is operating in an extreme environment (greater than 40 °C (104 °F)). To troubleshoot: Refer to Section A.3 for environmental specifications. COLUMN HEATER OPEN CIRCUIT This error occurs when the column heater is unplugged from the component panel. To troubleshoot: 1.
Dionex ICS-1100 Ion Chromatography System To troubleshoot: 1. Retry the calibration. 2. If calibration still fails, the vacuum degas assembly may need to be replaced. Contact Thermo Fisher Scientific for assistance. HARDWARE NOT PRESENT This error indicates a problem in the Dionex ICS-1100 electronics. To troubleshoot: Contact Thermo Fisher Scientific for assistance. The Dionex ICS-1100 electronics components cannot be serviced by the user.
4 • Troubleshooting To troubleshoot: 1. If a sequence is being executed, terminate the sequence by selecting Batch > Stop in Chromeleon. 2. Try to toggle the valve from Load to Inject by clicking the Load and Inject buttons on the Dionex ICS-1100 Control panel in Chromeleon. 3. Turn off the Dionex ICS-1100 power briefly and then restart. 4. If the problem persists, repeat Step 2. 5. If the problem persists, contact Thermo Fisher Scientific for assistance.
Dionex ICS-1100 Ion Chromatography System PUMP PRESSURE HARDWARE ERROR This error indicates a problem in the pump controller electronics. To troubleshoot: Contact Thermo Fisher Scientific for assistance. The Dionex ICS-1100 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. 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. Restart the pump.
Dionex ICS-1100 Ion Chromatography System SUPPRESSOR NOT CONNECTED This error occurs if you turn on the suppressor and the Dionex ICS-1100 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 Thermo Fisher Scientific for assistance. There may be a problem in the suppressor controller electronics. The Dionex ICS-1100 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 Dionex ICS-1100 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 Thermo Scientific Reference Library DVD (P/N 053891). 3. If the error persists, replace the suppressor (see Section 5.11).
Dionex ICS-1100 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 Thermo Scientific Reference Library DVD (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 Thermo Scientific Reference Library DVD (P/N 053891). Replace any damaged fittings. 2. If the pressure transducer continues to leak, contact Thermo Fisher Scientific for assistance. The pressure transducer cannot be serviced by the user.
Dionex ICS-1100 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 If the Dionex ICS-1100 does not contain a vacuum degas assembly, degas the eluent manually (see Section 3.4.4).
4 • Troubleshooting 3. Verify that the Degas check box is selected. 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. • End-line filter is dirty or clogged When new, end-line filters (P/N 045987) are pure white.
Dionex ICS-1100 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 Dionex ICS-1100 and Chromeleon Verify that the USB cable is connected correctly. For connection and setup information, refer to the Dionex ICS-1100 installation instructions.
4 • Troubleshooting • Flow rate is set to 0 Set the flow rate from the Dionex ICS-1100 Control panel in Chromeleon. • Eluent valve is closed Open the eluent valve from the Dionex ICS-1100 Control panel in Chromeleon. • Pump not primed Prime the pump (see Section 5.17). • Broken pump piston Replace the piston (see Section 5.8). 4.7 Erratic Flow/Pressure Reading • Pump needs priming Prime the pump (see Section 5.17). • Damaged piston seal Replace the piston seal (see Section 5.7).
Dionex ICS-1100 Ion Chromatography System If you have trouble isolating the restriction, refer to Section 5.2. • Plugged or damaged fitting Isolate the faulty fitting by loosening fittings, one by one, until the pressure returns to normal. Repair or replace the fitting (see Section 5.3). • Flow rate through the columns too high Set the correct rate for your application. If an incorrect flow rate calibration is suspected, calibrate the flow (see Section 5.1.3).
4 • Troubleshooting • Incorrect or contaminated eluent Remake the eluent. If the system is not operating in the RFIC-ER mode, refer to the instructions in the column manual. The manual is included on the Thermo Scientific Reference Library DVD (P/N 053891). If this is an RFIC-ER system, refer to the instructions in the manual provided in your RFIC-ER Installation Kit. Install or replace the end-line filter on the end of the deionized water line (see Section 3.4.3).
Dionex ICS-1100 Ion Chromatography System • Contaminated or degraded sample Take appropriate precautions when preparing and storing samples to prevent contamination and degradation (see Section 3.9). • Contaminated column 1. Clean the column as instructed in the column manual. Column manuals are included on the Thermo Scientific Reference Library DVD (P/N 053891). 2. If cleaning is unsuccessful, replace the column. 4.
4 • Troubleshooting guidance. Suppressor manuals are included on the Thermo Scientific Reference Library DVD (P/N 053891). • Sample concentration too high Dilute the sample (see Section 3.9.3). • Wrong eluent Check that you are using the correct eluent for your application. RFIC-ER systems only: Replace the RFIC-ER columns, if necessary. An Audit Trail message will inform you when a column is approaching the end of its useful life span.
Dionex ICS-1100 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 Thermo Scientific Reference Library DVD (P/N 053891).
4 • Troubleshooting • Cell above or below temperature Contact Thermo Fisher Scientific 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 Dionex ICS-1100 device in the timebase and select Properties. 2. Select the Options tab (see Figure 4-3). . Figure 4-3. Dionex ICS-1100 Server Configuration Properties: Options 3.
Dionex ICS-1100 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.
5 • Service This chapter describes Dionex ICS-1100 service and repair procedures that the user can perform. All procedures not included here, including electronics-related repair procedures, must be performed by Thermo Fisher Scientific personnel. For assistance, contact Technical Support for Dionex products. In the U.S. and Canada, call 1-800-346-6390. Outside the U.S. and Canada, call the nearest Thermo Fisher Scientific office.
Dionex ICS-1100 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 Thermo Fisher Scientific 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 • Doc.
Dionex ICS-1100 Ion Chromatography System 5.1.2 Calibrating the Conductivity Cell When to Calibrate • After every 6 months of use NOTE Do not use this procedure to calibrate a new cell. If you are replacing a cell, see the instructions in Section 5.10 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.
5 • Service After calibration, the conductivity reading should be 147.00 ± 2 S and the cell constant should be between 120 and 180. If this is not the case, contact Thermo Fisher Scientific for help. 11. Click Log to record the new calibration values in the Audit Trail. 12. Flush the KCl solution from the system by pumping deionized water through the cell. When the conductivity drops to less than 1 S/cm, stop the pump. 13.
Dionex ICS-1100 Ion Chromatography System 5.1.3 Calibrating the Flow Rate When to Calibrate If you run the Dionex ICS-1100 Operational Qualification or Performance Qualification and it fails. Items Needed • 0.076-mm (0.003-in) ID yellow PEEK tubing (P/N 049715) to create 14 ± 2 MPa (2000 ± 300 psi) of backpressure (if needed) • 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 5.1.4 Calibrating the Vacuum Degas Assembly When to Calibrate • After every 6 months of use 1. Open the Dionex ICS-1100 Wellness Panel in Chromeleon (see Section 5.1.1). 2. On the Wellness Panel under Degas Calibration, select Calibrate. The degas pump runs for 90 seconds to allow a vacuum to be created. After 90 seconds, the vacuum degas pressure reading is recorded.
Dionex ICS-1100 Ion Chromatography System WASTE 1 ELUENT OUT OUT 2 5 IN 7 SEPARATOR COLUMN PULSE DAMPER COLUMN HEATER (optional) SAMPLE 11 IN COND OUT CELL HEAT EXCHANGER IN 8 SUPPRESSOR OUT 6 GUARD 9 OUT 3 PUMP HEAD PUMP HEAD IN WASTE 4 OUT PRESS. XDUCER Figure 5-2. Dionex ICS-1100 Flow Schematic: Standard Configuration 88 Doc.
5 • Service IN ER3b IN OUT 2 SUPPRESSOR IN 12 IN COND OUT CELL SAMPLE 9 ER3a IN HEAT EXCHANGER OUT OUT PULSE DAMPER 5 IN ER2 IN 8 7 SEPARATOR COLUMN ELUENT COLUMN HEATER (optional) ERC 10 1 6 IN 10 GUARD ER1 OUT 3 PUMP HEAD PUMP HEAD IN WASTE 4 OUT PRESS. XDUCER Figure 5-3. Dionex ICS-1100 Flow Schematic: RFIC-ER Mode Doc.
Dionex ICS-1100 Ion Chromatography System 5.3 Replacing Tubing and Fittings The Dionex ICS-1100 is plumbed with the tubing and tubing assemblies listed below. Tubing Size and Type Color Used For 0.125-mm (0.005-in) ID PEEK (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.
5 • Service 5.4 Rebuilding the Injection Valve or Auxiliary Valve Thermo Fisher Scientific 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.
Dionex ICS-1100 Ion Chromatography System Figure 5-4. Injection Valve Plumbing 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 Thermo Fisher Scientific. Electronics-related repair procedures must be performed by Thermo Fisher Scientific personnel.
5 • Service 4. Unscrew the black locking ring on the front of the valve (see Figure 5-5) and remove the ring. 5. Grasp the front of the valve pod and pull firmly to remove it from the Dionex ICS-1100. Black Locking Ring Figure 5-5. Unscrew the Valve Locking Ring 6. Check that the new pod (6-port, P/N 061947; 10-port, P/N 061948) has the correct number of ports for the valve being serviced. 7. Align the slots in the new pod with the runner in the valve holder on the Dionex ICS-1100 (see Figure 5-6).
Dionex ICS-1100 Ion Chromatography System 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. Tighten fittings as required (see Section 5.1.1). 12. Close the door. 94 Doc.
5 • Service 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 Dionex ICS-1100 Control panel in Chromeleon. 2.
Dionex ICS-1100 Ion Chromatography System 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.
5 • Service 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 5-10). To open the valve, turn the knob one-quarter to one-half turn counterclockwise. 2.
Dionex ICS-1100 Ion Chromatography System 5. Place the head (front end down) on a clean work surface and lift off the spacer to expose the piston seal (see Figure 5-8 or Figure 5-9).
5 • Service 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.
Dionex ICS-1100 Ion Chromatography System 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.
5 • Service Reinstalling the Head and Piston Thermo Fisher Scientific 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.
Dionex ICS-1100 Ion Chromatography System 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 Dionex ICS-1100 Control panel in Chromeleon. 2. Turn off the main power switch, to ensure that you do not unintentionally start the Dionex ICS-1100. 3.
5 • Service 4. If the O-ring is removed with the valve knob in Step 3, pull the O-ring off the end of the knob (see Figure 5-11). If the O-ring is not removed with the valve knob, insert a thin object (for example, the bent end of a paper clip) into the cavity in the pump head and carefully pull out the O-ring. 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 5-11.
Dionex ICS-1100 Ion Chromatography System 5.10 Replacing the Conductivity Cell 1. Turn off the Dionex ICS-1100 power. 2. Open the front door and disconnect the tubing from the CELL IN and CELL OUT fittings (see Figure 5-12, View A). Loosen the two screws on the cell front cover. The screws remain attached (see Figure 5-12, View B). Unscrew Disconnect Unscrew View B View A Figure 5-12. Removing the Cell Front Cover 3.
5 • Service 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 Dionex ICS-1100 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. Turn on the Dionex ICS-1100 power.
Dionex ICS-1100 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 Thermo Scientific Reference Library DVD (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. Turn off the pump from the Dionex ICS-1100 Control panel in Chromeleon. 3.
5 • Service 11. Align the top of the suppressor with the guide line printed on the component panel (see Figure 5-15) 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.
Dionex ICS-1100 Ion Chromatography System Thumbscrews (6) Figure 5-16. Dionex ICS-1100 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 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. In the field next to the Download button, verify that Current is selected and then click Download to download the new calibration values to the Dionex ICS-1100. d.
Dionex ICS-1100 Ion Chromatography System 7. Disconnect the heat exchanger outlet line from the guard column inlet. 8. Use an Allen wrench to remove the three screws from the heat exchanger metal plate and remove the plate (with the tubing) from the heater. 9. Remove the plastic backing from the new heat exchanger (P/N 059979, with 0.25-mm (0.010-in) ID tubing; P/N 060943, with 0.125-mm (0.005-in) ID tubing) and press the heat exchanger onto the heater. Replace the screws removed in Step 8. 10.
5 • Service 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 Dionex ICS-1100. Continue pulling until the connectors for the two cables are outside the panel (see Figure 5-19). Disconnect the cables. Disconnect cables Eluent Valve Eluent Valve Cable Figure 5-19. Eluent Valve Cable 8. Remove the mounting plate on the old valve by unscrewing and removing the two screws.
Dionex ICS-1100 Ion Chromatography System 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 Dionex ICS-1100. 14. Prime the pump (see Section 5.17). 5.15 Replacing the Leak Sensor 1. Turn off the power to the Dionex ICS-1100. 2. Open the Dionex ICS-1100 front door. 3. Loosen the screw on the front of the leak sensor (see Figure 5-21).
5 • Service 7. Connect the cable from the new leak sensor (P/N 058053) to the Dionex ICS1100 cable. 8. Feed the cables back inside the Dionex ICS-1100. Align the leak sensor with the component panel opening and fingertighten the screw. 9. Make sure the leak sensor does not touch the bottom of the drip tray. 5.16 Priming the Pump 1. Verify that the eluent reservoir is filled, the reservoir cap is installed and hand tightened, and the liquid line from the Dionex ICS-1100 to the reservoir cap is connected.
Dionex ICS-1100 Ion Chromatography System Secondary Pump Head Waste Valve (close) Port Primary Pump Head 10 mL Syringe (P/N 079803) Priming Valve (open) Figure 5-23. Priming the Eluent Lines 3. Open the priming valve by turning it one-quarter to one-half turn counterclockwise. 4. On the Dionex ICS-1100 Control panel in Chromeleon, click the Pump Settings button. The Pump Settings window opens (see Figure 3-5). 5. Under Eluent Flow Valve, click the Open button. 6.
5 • Service 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 5-24). Secondary Pump Head Waste Valve (open) Priming Valve (close) Primary Pump Head Figure 5-24. 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 5-24).
Dionex ICS-1100 Ion Chromatography System 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 079803) filled with isopropyl alcohol (IPA) to the port in the primary pump head (see Figure 5-25). 2. Open the waste valve on the secondary pump head (see Figure 5-25) by turning the knob onequarter to one-half turn counterclockwise.
5 • Service 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 Dionex ICS-1100.
Dionex ICS-1100 Ion Chromatography System 3. Replace the two fuses in the holder with new IEC 127 fast-blow fuses rated 3.15 amps (P/N 954745). Thermo Fisher Scientific 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. 118 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) Weight Decibel Level Control Modes USB Communication Protocol Doc. 065289-03 10/12 Height: 56.1 cm (22.1 in) Width: 22.4 cm (8.8 in) Depth: 53.3 cm (21.0 in) 24.
Dionex ICS-1100 Ion Chromatography System A.3 Environmental Operating Temperature Operating Humidity Operating Pressure A.4 A.5 5% to 95% relative humidity, noncondensing 35 MPa (5000 psi) maximum liquid path (tubing, valve, columns, etc.) Front Panel Power LED On when power is present; off when no power is present Inject Valve LEDs Indicates the injection valve position. Alarm LED Indicates an alarm state. Status LEDs Indicates the instrument status.
A • Specifications Pressure Ripple Eluent On/Off Valve Piston Seal Wash Pressure Alarm Limits <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.
Dionex ICS-1100 Ion Chromatography System A.6 Eluent Regeneration Eluent Regeneration Eluents Flow Rates Carbonate and carbonate/bicarbonate up to 20 mM MSA up to 34 mM 0.01 to 2.
A • Specifications Full-Scale Output Ranges Electronic Noise Filter Temperature Compensation A.8 Digital signal range: 0 to 15,000 S Analog signal range: 0 to 15,000 S ±0.1 nS/cm when background conductivity is 0 to 150 S/cm ±2 nS/cm when background conductivity is 151 to 3200 S/cm Rise times from 0 to 10 s; user-selectable Fixed at 1.7% per 1 °C at cell temperature Temperature Range Ambient +7 °C; 30 to 55 °C Temperature Stability <0.
Dionex ICS-1100 Ion Chromatography System 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 (Optional) Channel Pump Materials Single-channel degas channel with degas membranes Dual-stage diaphragm vacuum pump Wetted materials, PEEK, PTFE A.12 Column Heater (Optional) Operating Temperature 30 to 60 °C (86 to 140 °F); minimum 5 °C above ambient temperature.
A • Specifications A.
Dionex ICS-1100 Ion Chromatography System Void Volume SRS 300 (4 mm): <50 L SRS 300 (2 mm): <15 L MMS 300 (4 mm): <50 L MMS 300 (2 mm): <15 L AMMS ICE 300 (4 mm): <50 L AMMS ICE 300 (2 mm): <15 L Anion AES: <35 L Cation AES: <35 L A.
A • Specifications Data Trending Plots Virtual Column Simulator 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 Customizable System Control Panels Standard feature System Status Vir
Dionex ICS-1100 Ion Chromatography System 128 Customized Reporting Standard feature; unlimited report workbooks Automated System Qualification Detailed, comprehensive qualification reports Doc.
B • TTL and Relay Control B.1 TTL and Relay Connections A 12-pin connector strip for TTL/relay control is located on the Dionex ICS-1100 rear panel. The connector provides two relay outputs, two TTL outputs, and four TTL inputs (see Figure B-1).
Dionex ICS-1100 Ion Chromatography System The outputs can be used to control functions in external devices such as an autosampler or another Dionex module.
B • TTL and Relay Control b. Plug the connector into the 12-pin connector on the Dionex ICS-1100 rear panel. c. Connect the wires from the Dionex ICS-1100 connector plug to the TTL or relay connector pins on the other module(s). Additional connector plugs are provided with other Dionex modules. NOTE Check the polarity of each connection. Connect signal wires to signal (+) pins and ground wires to ground (-) pins. 3.
Dionex ICS-1100 Ion Chromatography System B.1.1 Selecting TTL Input Functions and Control Types To select TTL input functions and the control type, open the Chromeleon Server Configuration program and double-click the Dionex ICS-1100 icon under the timebase. Select the TTL Inputs tab (see Figure B-3). Figure B-3. Dionex ICS-1100 Server Configuration Properties: TTL Inputs TTL Input Control Types The Dionex ICS-1100 TTL inputs respond to four types of signals to accommodate different controlling devices.
B • TTL and Relay Control • Normal Edge: In normal edge operation, the negative (falling) edge of a signal turns on the function. For example, for the Load/Inject function, the negative edge switches the injection valve position to Load. 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).
Dionex ICS-1100 Ion Chromatography System B.2 Controlling TTL and Relay Outputs The Dionex ICS-1100 provides two TTL outputs and two relay contacts for control of functions in external devices, such as an integrator or autosampler. The relay outputs can be used to switch any low-voltage control. Switched current must be less than 200 mA and 60 V peak blocking. The relay-contact closures are normally open. When the relay is closed, current flows to the connected device.
C • Reordering Information Part Number Item Reservoirs 046548 2-L plastic reservoir assembly (includes stopper and cap) 039164 4-L plastic reservoir assembly (includes stopper and cap) Pump 057937 Primary pump head assembly 057938 Secondary pump head assembly 045721 Outlet check valve assembly, 10-32 045722 Inlet check valve assembly, 1/4-28 045994 Check valve cartridges 052840 Piston 055870 Piston seal 048722 Piston rinse seal 055752 O-ring for waste valve or priming valve 057945
Dionex ICS-1100 Ion Chromatography System Part Number Item 061947 Auxiliary valve pod assembly (6-port valve) 061948 Auxiliary valve pod assembly (10-port valve) Suppressors, Cell, and Column Heater 056116 Dionex AAES Anion Atlas Electrolytic Suppressor 056118 Dionex CAES Cation Atlas Electrolytic Suppressor 064554 Dionex ASRS 300 4-mm Anion Self-Regenerating Suppressor 064556 Dionex CSRS 300 4-mm Cation Self-Regenerating Suppressor 064555 Dionex ASRS 300 2-mm Anion Self-Regenerating Suppres
C • Reordering Information Part Number Item Preventive Maintenance Kits 057954 Dionex ICS-1100 Preventive Maintenance Kit 060581 Dionex AS Preventive Maintenance Kit 055647 Dionex AS-DV Preventive Maintenance Kit Doc.
Dionex ICS-1100 Ion Chromatography System 138 Doc.
D • FAQ D.1 How do I hook up an autosampler? For instructions on how to connect the Dionex ICS-1100 to an autosampler, refer to the Dionex ICS-1100 installation instructions. Also refer to the autosampler operator’s manuals, which are included on the Thermo Scientific Reference Library DVD (P/N 053891). D.2 How do I print? Click the Print toolbar button in Chromeleon. D.
Dionex ICS-1100 Ion Chromatography System D.6 When should I remake eluents? Eluents should be remade every two or three weeks. D.7 How do I start Chromeleon? Click Start on the Windows taskbar, and then select All Programs > Chromeleon > Chromeleon. D.8 How do I delete data? In the Chromeleon Browser, highlight the sequence you want to delete and then select File > Delete. D.9 How do I back up data? In Chromeleon, select File > Export/Backup. Back up the data and indicate the backup source. D.
D • FAQ D.13 How do I clean a column? See the troubleshooting section of the column manual. D.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. The suppressor needs regeneration. See the suppressor manual for troubleshooting information. The suppressor manual is included on the Thermo Scientific Reference Library DVD (P/N 053891). • The cell is out of calibration. See Section 5.1.
Dionex ICS-1100 Ion Chromatography System 142 Doc.
E • Glossary Analytical Column Synonymous with Separator Column. Band Spreading The broadening of the sample band as it travels through the column. Band spreading can also occur in the injection valve, detector cell, and interconnecting tubing. Calibration Curve A graph showing detector response in peak height or area versus analyte concentration. Capacity Factor (k´) The number of column volumes of eluent, pumped through the column, required to elute an analyte.
Dionex ICS-1100 Ion Chromatography System Cell Constant (k) A factor determined experimentally by measuring the conductance (G) of a standard solution of known equivalent conductivity (k). k = G The value of k depends upon the surface area of, and distance between, the electrode faces in the conductivity detector cell.
E • Glossary of relatively clean sample. This allows large volumes of sample to be injected, lowering concentration detection limits. Conductivity A measure of the ease with which electrical current flows through a liquid contained between two opposite charged electrodes. Conductivity is a characteristic of ions in solution. 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.
Dionex ICS-1100 Ion Chromatography System Packing The material that fills a chromatographic column; usually a resin or silica-based material. Pellicular Resin A resin with a solid, nonporous core coated with a thin layer of more porous material. The exchange sites of pellicular ion exchange resins are located only on the surface layer of the bead. These resins have a low ion-exchange capacity. Pre-Column Synonymous with Guard Column.
E • Glossary Siemens (S) Unit measure of conductance; the reciprocal of the electrical resistance of a solution. Suppressor A device used to minimize eluent conductivity and convert sample species to a common form, thus increasing detection sensitivity. Temperature Coefficient The percent of change in the conductivity of a solution with a 1 oC change in temperature. Every solution has a characteristic temperature coefficient which is determined experimentally. Theoretical Plates (N) See Column Efficiency.
Dionex ICS-1100 Ion Chromatography System 148 Doc.
Index A Air particulate samples, 48 Alarm conditions, 61 – 67 See also Error messages Ambient temperature, 78 Analog output, 130 Connector, 18 Anion separations, 47 Application Wizard, 54 AS Autosampler, 49 Maintenance, yearly, 56 Sample injection, 51 AS-DV Autosampler, 49 Maintenance, yearly, 57 Sample injection, 51 AS-HV Autosampler, 49 Atlas Electrolytic Suppressor, 16 See also Suppressor Audit Trail Error messages, 59 Icons, 59 Autosampler Loading samples with, 51 See also AS Autosampler See also AS-DV
Dionex ICS-1100 Ion Chromatography System Cation separations, 47 Cell See Conductivity cell Cell calibration, 84 Check valves Cleaning procedure, 95 – 96 Replacement procedure, 95 – 96 Chromatogram, 3 Chromeleon, 24 Alarm conditions, 61 Application Wizard, 54 Audit Trail, 59 Audit Trail error messages, 59 Commands, 53 Degas options, 79 Error messages, 61 Interface, 24 Overview, 24 Panel tabset, 24 Programs, 51 Quantification method, 55 Starting, 40 Timebase, 24 Wellness panel, 81 Chromeleon Server Starting,
Index Audit Trail description, 59 Column heater exceeds safe temperature, 61 Column heater open circuit, 61 Column heater short circuit, 61 Degas calibration failed, 61 Hardware not present, 62 Leak sensor wet, 62 Load/inject valve error, 62 Option not installed, 63 Pump motor lost control, 63 Pump over pressure, 64 Pump pressure hardware error, 64 Pump stopped due to lost USB communication, 64 Pump under pressure, 65 Second valve error, 65 Suppressor not connected, 66 Suppressor over current, 66 Suppressor
Dionex ICS-1100 Ion Chromatography System G Ghosting, 74 Guard column, 16 H Hardware not present error, 62 Heater, column, 33 See also Column heater High pressure alarm, 64 Humidity, operating, 120 I Injecting samples, 49 Via autosampler, 51 Via syringe, 50 Via vacuum syringe, 51 Injection port, 11 Injecting via syringe, 50 Injection valve, 15, 30 Leaking, 69 Passages blocked, 74 Plumbing connections, 31 Rebuilding, 91 Specifications, 123 Troubleshooting, 62 Installation Priming, 113, 115 TTL and relay c
Index O Offsetting background conductivity, 46 Operating features, 11 Operating humidity, 120 Operating ranges Cell heater, 15 Column heater, 16 Flow rate, 15 Operating temperature, 120 Operation Equilibration time, 46 Overview, 37 Priming, 45, 115 – 116 Reservoir setup, 42 Sample preparation, 47 Sample processing, 38 Setting operating conditions, 46 Starting Chromeleon, 40 System power-up, 39 Operational status verification, 46 Option not installed error, 63 Oven See Column heater Overview of system, 4 P
Dionex ICS-1100 Ion Chromatography System Programs (Chromeleon), 25 Controlling an autosampler, 51 Pulse damper, 20, 22, 30 Pump, 28 Flow rate, 15 Leaks, 68 Over pressure alarm, 64 Primary pump head, 28 Priming, 45, 113 Priming problems, 70 Secondary pump head, 29 Stopped due to lost USB communication, 64 Troubleshooting, 72 Under pressure alarm, 65 Pump check valve leaking, 68 Pump degas See Vacuum degas assembly Pump head waste valve Leaking, 69 O-ring replacement procedure, 102 Pump heads, 95 Pump motor
Index Sample processing, 38, 52 – 53 Batch, 38, 53 Manual, 38, 52 With Chromeleon, 52 – 53 Samples Collecting and storing, 47 Diluting, 48 Filtering, 47 Injecting, 49, 51 Loading, 49 Pretreating, 48 Saving data, 53 Schematics, 20 Seal replacement, 98 Second valve Troubleshooting, 65 Second valve error, 65 Selectivity Troubleshooting, 75 Self-Regenerating Suppressor, 16 See also Suppressor Separation process, 3 Separator column, 16 Sequence Control panel, 25 Sequence Wizard, 55 Server Configuration program S
Dionex ICS-1100 Ion Chromatography System Replacement procedure, 106 Suppressor alarms Suppressor not connected, 66 Suppressor over current, 66 Suppressor over power, 67 Suppressor stopped for zero flow rate, 67 Supressor specifications Chemical suppression, 125 Displacement chemical regeneration, 125 Electrolytic suppression, 125 Sequential suppression for anions, 125 Suppression capacity, 125 Suppressor wear parts, 125 Void volume, 125 Syringe injection, 50 Vacuum, 51 System Shutdown, 140 Startup, 39 Stat
Index Troubleshooting, 70 Valve See Auxiliary valve See Eluent valve See Injection valve See Waste valve W Warranty, voiding, 81, 91 – 92 Waste lines Blocked, 68 Waste valve, 29 Opening, 29, 97 O-ring replacement procedure, 102 Water samples, 48 Weekly maintenance, 56 Weight, 119 Wellness, 25 Wellness panel, 81 Y Yearly maintenance, 56 Doc.
Dionex ICS-1100 Ion Chromatography System Index-10 Doc.
