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ICS-1000 Ion Chromatography System Operator`s Manual

1. Min Pressure 0 psi 0 088 uS Eluent Level 0 001 Suppressor Current Figure B 36 Chromeleon Control Panel Pump Settings 5 Draw the syringe back to begin pulling eluent through the flow path It may take several syringe draws to remove all air or previous eluent from the tubing NOTE Ifthe vacuum degas assembly is installed draw out an additional 20 mL of eluent After priming the lines thoroughly close the priming valve Do not overtighten the priming valve Close the eluent valve click Eluent Flow Valve Closed on the Control Panel Doc 031879 01 3 03 B 37 ICS 1000 lon Chromatography System B 14 2 Priming with the Prime Button NOTE Perform this procedure after priming the eluent lines see Section B 14 1 1 Check that the priming valve on the primary pump head is closed see Figure B 37 Secondary Pump Head Waste Valve a open 1 Primary 7 Pump Head Priming Valve close Figure B 37 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 B 37 Opening the valve directs the eluent flow path to waste and eliminates backpressure 3 Click Prime on the Chromeleon Control Panel see Figure B 36 The pump will begin pumping at approximately 3 0 mL min 4 Continue priming the ICS 1000 until
2. Figure B 23 Chromeleon Main Window and Browser B 26 Doc 031879 01 3 03 Setting Up a Chromeleon Application 3 Inthe Browser select File gt New and select Sequence using Wizard see Figure B 24 Vowo oon Control Panel Sequence using Wizard Cancel Sequence from UMS Worklist Query using Wizard Program File Help Method File Spectra Library Figure B 24 Creating a New Sequence The Sequence Wizard Welcome page appears see Figure B 25 Chromeleon Sequence Wizard Welcome x Welcome to the Sequence Wizard This wizard helps you to create a sequence It will guide you through the following steps o Choose a timebase o Specify standards and unknowns o Select method files o Store the sequence To continue click Next Cancel Help Figure B 25 Sequence Wizard Welcome Page Doc 031879 01 3 03 B 27 ICS 1000 lon Chromatography System NOTE For details about a Sequence Wizard step click the Help button on the Sequence Wizard page 4 Click Next gt The Sequence Wizard Timebase page appears see Figure B 26 Chromeleon Sequence Wizard Step 1 of 5 Timebase ICS 1000 Figure B 26 Example Sequence Wizard Step 1 5 Select the ICS 1000 timebase and click Next gt B 28 Doc 031879 01 3 03 Setting Up a Chromeleon Application The Unknown Samples page appears see Figure B 27
3. from Pos Stop Mode Pump On 500 psi Lom o Prime Inject Valve Inject Load Eluent Flow Valve 410 r T T T T T T T T T 1 Closed Open 0 00 0 50 1 00 1 50 2 00 2 50 3 00 3 50 4 00 4 50 5 00 Figure B 50 ICS 1000 Traditional System Control Panel Connected to the ICS 1000 B 52 Doc 031879 01 3 03 Installation Troubleshooting B 23 Installation Troubleshooting Problem When the ICS 1000 power is turned on for the first time a Windows message box appears asking for a USB configuration file cmwdmusb inf Possible Cause The USB cable was connected and the power turned on before Chromeleon was installed Solutions Use one of the methods below to resolve the problem e Click the Cancel button on the Windows message box Turn off the ICS 1000 power and unplug the USB cable Then install Chromeleon reconnect the USB cable and turn on the ICS 1000 power Windows will now automatically recognize the new USB device Leave the message box open and insert the Chromeleon CD into the CD ROM drive Click the Browse button on the message dialog box The cmwdmusb inf file is located in the Drivers folder on the CD Doc 031879 01 3 03 B 53 ICS 1000 lon Chromatography System B 54 Doc 031879 01 3 03 C TTL and Relay Control NOTE The ICS 1000 Ion Chromatography System is designed for use with IC ion
4. Action On TTL MS Vice smscusnuces INVERTED EDGE io y Action Off or No Effect TLD Vo mApm6e NORMAL PULSE gy Ll ll Action On Action Off is guaranteed to be detected A pulse width of 4 ms or less is guaranteed to be ignored The action for pulse widths that are greater than 4 ms and less than 50 ms is undefined C 4 Doc 031879 01 3 03 C TTL and Relay Control Inverted Pulse The inverted pulse mode operates identically to the normal pulse mode except that the positive and negative edges are reversed in function TTL V INVERTED PULSE 49 y Action On _Action Off Y C 2 Controlling TTL and Relay Outputs The ICS 1000 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 Relay loads in excess of 200 mA or with included power supplies over 60 V may damage the relay drivers on the CPU CAUTION The TTL outputs are normally at 5 volts Setting a TTL output to 0 volts turns on the action in the connected device Doc 031879 01 3 03 C 5 ICS 1000 lon Chromatography System The TTL and relay output states can be controlled either b
5. Figure B 45 Example Program for AS40 Control B 19 Analog Output Connection Optional The analog output connector on the ICS 1000 rear panel outputs an analog voltage signal proportional to the conductivity measured by the cell The output 1s filtered using the selected data rise time The analog output can be connected to an analog to digital converter such as an integrator or other recording device Refer to the documentation for the device for connection instructions Analog output is 0 to 1V scaled to the selected range For an example setup for ICS 1000 stand alone operation with an AS50 autosampler see Section C 3 B 20 Pressurizing the Eluent Reservoir Optional The ICS 1000 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 B 46 Doc 031879 01 3 03 Pressurizing the Eluent Reservoir Optional B 20 1 Connecting the Gas Source Optional 1 Locate the barbed fitting P N 030071 pipe thread reducer P N 030087 3 mm 1 8 in ID tubing P N 040793 and ICS 1000 air regulator accessory P N 060054 These parts must be ordered separately 2 Use the barbed fitting and pipe thread reducer to connect the 3 mm 1 8 in ID tubing to a clean ga
6. 3 22 Doc 031879 01 3 03 4 Troubleshooting This chapter is a guide to troubleshooting problems that may occur while operating the ICS 1000 Ion Chromatography System e Section 4 1 describes error messages and how to troubleshoot them Table 4 3 lists the messages and the page numbers where they are described e The remaining sections in this chapter describe other operating problems and how to resolve them Table 4 4 lists the operating problems and the page numbers where they are described If you are unable to eliminate a problem contact Dionex for help In the U S call Dionex Technical Support at 1 800 346 6390 Outside the U S call the nearest Dionex office Alarms and Error Conditions COLUMN HEATER EXCEEDS SAFE TEMPERATURE COLUMN HEATER OPEN CIRCUIT COLUMN HEATER SHORT CIRCUIT DEGAS CALIBRATION FAILED HARDWARE NOT PRESENT LEAK SENSOR WET LOAD INJECT VALVE ERROR OPTION NOT INSTALLED PRESSURE SLOPE CALIBRATION ERROR PUMP MOTOR LOST CONTROL PUMP PRESSURE HARDWARE ERROR PUMP OVER PRESSURE PUMP UNDER PRESSURE SUPPRESSOR OVER CURRENT SUPPRESSOR OVER VOLTAGE SUPPRESSOR OVER POWER SUPPRESSOR NOT CONNECTED See page 4 3 page 4 3 page 4 3 page 4 4 page 4 4 page 4 4 page 4 5 page 4 5 page 4 5 page 4 6 page 4 6 page 4 6 page 4 7 page 4 7 page 4 8 page 4 8 page 4 8 Table 4 3 ICS 1000 Alarms and Error Messages Summary Doc 031879 01 3 03 4 1 ICS 1000 lon Chromatography System
7. Connect GUARD OUT to the guard column outlet Push the guard column onto the back column clip Remove the union connecting COL IN and COL OUT and Dn Ro Connect COL IN to the separator column inlet Connect COL OUT to the separator column outlet Check the arrow on the column label It should point up flow toward the cell 7 Pushthe separator column onto the front column clips 8 Replace the top metal plate on the column heater if installed B 20 Doc 031879 01 3 03 Installing and Plumbing the Columns and Suppressor B 9 3 Installing the Suppressor 1 Locate the suppressor mounting tabs on the component panel see Figure B 19 Reach into the opening between the tabs and 1 Suppressor Mounting Tabs 2 Suppressor Cable pull the yellow Connector connector and attached 3 Guideline for AES cable slightly out of the opening 4 Guideline for SRS 2 Connect this cable to the cable from the suppressor align the pins on the two connectors and push them together Figure B 19 Suppressor Mounting Tabs and Guidelines 3 Orient the suppressor with the REGEN OUT fitting on top and the cable to the right 4 Feed the cable into the opening in the component panel 5 Align the top of the suppressor with the guideline printed on the component panel see Figure B 19 and align the slots on the rear of the suppressor with the tabs on the panel Doc 031879 01 3 03 B 21 ICS 1000 lon Chr
8. Dummy Cell Test Conductivity Cell Slope Cal Slope Cal Press for instructions aye Dummy Cell Current Calibration Date 3 19 2003 Last Calibration Date 3 19 2003 poo omms etr Instructions on e Log H Figure 5 1 Chromeleon Wellness Panel Doc 031879 01 3 03 5 Service Use the Wellness Panel to perform the following functions e Calibrate the pump flow rate Calibrate the vacuum degas assembly Calibrate the conductivity cell e Test the conductivity cell electronics using a dummy cell e Upload calibration values from the ICS 1000 to the Chromeleon Wellness database Doc 031879 01 3 03 5 3 ICS 1000 lon Chromatography System 5 1 2 Calibrating the Conductivity Cell When to Calibrate e 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 9 to install the new cell and calibrate it Items Needed Description 1 0 mM KCI solution Prepare by dissolving 0 07456 g of reagent grade KCl in 1 liter of 18 megohm DI water Backpressure tubing to provide Use 0 076 mm 0 003 in ID yellow PEEK at least 7 MPa 1000 psi tubing P N 049715 1 Open the ICS 1000 Wellness Panel in Chromeleon see Section 5 1 1 2 Onthe Wellness Panel under Electric Conductivity Cell Calibration click Offset Cal 3 When the offset ca
9. 0 to 3000 LS analog output 1 7 per C 8 kH square wave Correlation gt 0 999 RSD lt 5 to 800 uS A 7 Conductivity Cell with Heat Exchanger Cell Body Electrodes Active Volume Operating Temperature Maximum Pressure A 8 Injection Valve PEEK Passivated 316 stainless steel 1 0 uL 30 to 55 C 86 to 130 F must be at least 7 C above the ambient temperature 2 MPa 300 psi Injection Valve Two position six port electrically activated valve with PEEK wetted components A 9 Vacuum Degas Assembly Optional Channel Pump Materials Single channel degas channel with degas membranes Dual stage diaphragm vacuum pump Wetted materials PEEK PTFE Doc 031879 01 3 03 ICS 1000 lon Chromatography System A 10 Column Heater Optional Operating 30 to 60 C 86 to 140 F must be at least 5 C above the ambient Temperature temperature A 4 Doc 031879 01 3 03 B Installation This chapter provides instructions for the initial installation of the ICS 1000 Ion Chromatography System NOTE These installation instructions are also shipped with the ICS 1000 as a stand alone printed manual Document No 031915 NOTE The order of the steps is important It is especially important to install Chromeleon amp before connecting the USB cable and turning on the ICS 1000 power B 1 Facility Requirements Make sure the ICS 1000 installation site meets the power and environmental s
10. 2 Suppressor Cable Connector 3 Guideline for AES 4 Guideline for SRS Figure 5 12 Suppressor Guidelines and Mounting Tabs on Component Panel 5 11 Replacing the Column Heater Turn off the ICS 1000 power Open the front door of the ICS 1000 Follow the steps below to remove the existing column heater a Unscrew the two thumbscrews on the heater cover they remain attached to the cover b Pull the heater cover straight out to remove it Doc 031879 01 3 03 5 23 ICS 1000 lon Chromatography System c Unscrew the six thumbscrews on the top metal plate see Figure 5 13 and remove the plate x Thumbscrews 6 Figure 5 13 ICS 1000 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 Before installing the new column heater write down the two calibration values offset and slope recorded on the back of the heater Align the connector on the back of the new column heater P N 058060 with the connector on the component panel see Figure 2 4 and push the column heater onto the component panel Remove the heater cover and the metal plate on the new heater Install the columns in the new heater and replace the top metal plate and heater cover Turn on the ICS 1000 power 5 24 Doc 031879 01 3 03 5 Service 9 Enter the column heater calibration values in
11. 031879 01 3 03 Index R Rear panel 2 7 Analog output connector 2 7 Power receptacle 2 8 USB connections 2 7 Rebuilding the injection valve 5 10 Relay connections AS40 B 44 Rear panel connector 2 8 C 1 Relay outputs Controlling C 5 Voltage and current specifications C 2 Reordering information D 1 Reproducibility 2 27 Reservoir Connecting 3 8 Filling 3 8 Monitoring liquid level in 3 8 B 35 Storage on top cover 2 3 Restriction in liquid lines 4 6 5 7 Retention time Adjusting E 1 Moving E 1 Troubleshooting 4 17 Run time 2 15 Running samples 3 18 See also Processing samples S Safety messages 1 6 Sample loop 2 5 2 24 Changing 5 9 Injecting 2 24 Injection valve connections 2 24 5 10 Loading 2 24 Reordering D 1 Sample processing 3 2 3 18 3 19 Batch 3 2 3 19 Manual 3 2 3 18 With Chromeleon 3 18 3 19 Samples Collecting and storing 3 12 Diluting 3 13 Filtering 3 12 Injecting 3 14 3 16 Loading 3 14 Pretreating 3 12 Saving data 3 19 Schematic Flow 2 9 Seal replacement 5 14 5 16 5 17 Selectivity Troubleshooting 4 17 Self Regenerating Suppressor 2 6 See also Suppressor Separation process 1 3 Separator column 2 5 B 19 Installation B 20 Sequence 2 11 Creating 3 19 Sequence Wizard 3 19 Serial number B 16 Server Configuration program ASS50 configuration properties B 18 Starting 3 4 B 13 Timebase B 15 Server
12. Connecting the Power Cord B 11 Turning On the ICS 1000 Power B 12 Doc 031879 01 3 03 ICS 1000 lon Chromatography System B 8 B 9 B 10 B 11 B 12 B 13 B 14 B 15 B 16 B 17 B 18 B 19 B 20 Setting Up Chromeleon B 13 B 8 1 Assigning the ICS 1000 to a Timebase B 13 B 8 2 Assigning DX LAN Devices to the Timebase Optional B 16 Installing and Plumbing the Columns and Suppressor B 19 B 9 1 Column Heater Setup Optional B 19 B 9 2 Installing the Columns B 20 B 9 3 Installing the Suppressor B 21 Connecting the Waste Lines B 23 B 10 1 Installing the Gas Separator Waste Tube B 23 Setting Up the Eluent Reservoir B 25 Setting Up a Chromeleon Application B 26 B 12 1 Verifying Chromeleon Communication B 35 Setting the Eluent Level esporre a an ek E kee Reese B 35 Priming the Pump uui Ene IRR pate OS B 36 B 14 1 Priming the Eluent Lines with a Syringe B 36 B 14 2 Priming with the Prime Button B 38 Equilibrating the System B 39 Verifying Operational Status B 39 Connecting an AS50 Autosampl
13. Direct the flow to waste by opening the waste valve on the secondary pump head see Figure 5 7 To open the valve turn the knob one quarter to one half turn counterclockwise After rinsing close the waste valve Close the eluent valve from the ICS 1000 Control Panel in Chromeleon To prevent contamination of pump parts put on a pair of rubber gloves before disassembling the pump head Removing the Head and Piston 1 CAUTION MISE EN GARDE Turn off the main power switch to ensure that you do not unintentionally start the ICS 1000 Disconnect all tubing connections to the pump head Locate the open end wrench P N 014605 provided in the ICS 1000 Ship Kit P N 057905 Use the wrench to remove the two acorn nuts see Figure 5 4 from the pump head Slowly pull the head and allow it to separate from the housing Carefully disengage the head from the piston by pulling the head straight off and away from its mounting studs Lateral motion while disengaging the pump head from the piston may break the piston Un mouvement lat ral pendant la s paration de la t te et du piston peut casser le piston Vermeiden Sie Seitwartsbewegungen wenn Sie den Kopf vom Kolben l sen Andernfalls kann der Kolben brechen VORSICHT Doc 031879 01 3 03 5 13 ICS 1000 lon 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 5 or Figu
14. ICS 1000 lon Chromatography System TTL Input Control Types Inverted Pulse The ICS 1000 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 If the device connected to the ICS 1000 does not send a normal edge signal select the appropriate control type Refer to the documentation provided with the controlling device and the information below to select the correct type e 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 Action Off or No Effect TTL t5 V NORMAL Action On 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 e Inverted Edge The inverted edge mode works identically to the normal edge mode except that the positive and negative edges are reversed in function e Normal Pulse In normal pulse operation the negative falling edge of the TTL signal is the active edge and the positive rising edge is ignored A pulse width of 50 ms or more
15. Other system components including a guard column separator column and suppressor vary depending on the analyses to be performed The ICS 1000 can optionally be configured with a column heater for temperature control of the column ICS 1000 operation is controlled remotely by a personal computer running Windows 2000 or Windows XP and Chromeleon software version 6 5 SP2 or later Chromeleon also provides data acquisition and data processing functions For communication between the ICS 1000 and Chromeleon the ICS 1000 is connected to a USB Universal Serial Bus port on the computer or a USB hub For installation instructions see Section B 5 and also refer to Installing the Chromeleon IC System Document No 031883 1 4 Doc 031879 01 3 03 1 Introduction Chapter 1 Introduction Chapter 2 Features Overview Chapter 3 Operation and Maintenance Chapter 4 Troubleshooting Chapter 5 Service Appendix A Specifications Appendix B Installation Appendix C TTL and Relay Control Appendix D Reordering Information Appendix E FAQ Appendix F Glossary 1 3 About This Manual Introduces ion analysis and the ICS 1000 explains the conventions used in this manual including safety related information Provides an overview of ICS 1000 operating features and system components introduces the Chromeleon user interface Provides operating instructions and describes routine preventive maintenance p
16. 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 Connect the new heat exchanger inlet line to Port C on the injection valve and connect the outlet line to the guard column inlet Reinstall the top metal plate and the heater cover 5 13 Replacing the Eluent Valve 1 2 3 Turn off the power to the ICS 1000 Open the ICS 1000 front door To prevent an eluent leak during the procedure disconnect the eluent line from the reservoir cap Or plug the line on the left side of the valve with a union P N 039056 and a plug P N 037268 after disconnecting the liquid line from the valve see Step 4 Disconnect the two liquid lines connected to the eluent valve see Figure 5 15 Unscrew and remove the two screws that attach the valve to the component panel see Figure 5 15 Save the screws Remove Figure 5 15 Eluent Valve 5 26 Doc 031879 01 3 03 5 Service 10 11 12 13 14 Pull the valve straight out from the component panel and begin pulling the attached cable out of the opening in the panel The cable connects to a cable inside the ICS 1000 Continue pulling until the connectors for the two cables are outside the panel see Figure 5 16 Disconnect the cables Remove the mounting plate on the old valve by unscrewing and removing the two screws Save the screws Thread the cable fr
17. 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 Deionized water Balance capable of weighing more than 10 grams with 0 001 grams readability e Tared beaker To Calibrate 1 Open the ICS 1000 Wellness Panel in Chromeleon see Section 5 1 1 2 Verify that there is 14 1 4 MPa 2000 200 psi of backpressure 3 Onthe Chromeleon Wellness Panel under Pump Flow Rate Calibration select Reset Cal 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 Click 5 00 min to start the timer Immediately start collecting water into the tared beaker 7 Collect the water for exactly 5 00 minutes 8 Enter the weight of the water in grams 9 Click Calibrate to download the value to the ICS 1000 10 To recheck the value wait at least 15 minutes and then repeat the calibration 11 Click Log to record the new calibration value in the Audit Trail Doc 031879 01 3 03 5 Service 5 1 4 Calibrating the Vacuum Degas Assembly When to Calibrate e After every 6 months of use 1 Open the ICS 1000 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 re
18. Shutdown Stops the pump and suppressor The flow rate and suppressor current settings currently in effect are remembered and will be restored at system startup see above Doc 031879 01 3 03 ICS 1000 lon Chromatography System Audit Trail Audit Trail m 07 54 19 0 000 Pump ECD Autozero E307 54 19 0 000 ECD_1 AcqOn m 07 54 19 0 000 Pump_InjectValve InjectPosition Duration 30 00 07 54 49 0 500 Pump ECD Log Pressure 500 00 07 54 49 0 500 Pump ECD Log Background 0 24 __ __ 15 000 ECD 1 AcqOff The Audit Trail displays an account of every event that occurs during ICS 1000 operation This includes errors status messages operational events etc Pump ICS 1000 Pump Eljuent Bottle Eluent Bottle s gs noni 2 The entry field and gauge indicate the level a Connected of liquid in liters in the eluent bottle This H is a user controlled feature The level must T Mold Mode be entered by the user when the reservoir is B Stop Mode filled See Section 3 4 4 for details 0 Pump On Connected Connects the ICS 1000 to the Chromeleon 800 psi Control Panel enabling communication 1 00 m mi between the PC and the module Clearing the check box disconnects the ICS 1000 pro om the PC Hold Mode Indicates when an automatic batch run is on hold pump flow is not stopped Stop Mode Indicates when an automatic batch run is stopped
19. Update Wellness Database Press for instructions jv Connected zi Calibration Diagnostic Calibration Details Details Pump On Off Audit Trail 14 31 40 Wait at least 15 minutes before rechecking flow rate Press the Log button to record the new Calibration values into the Audit Trail Instructions Upload Loading Pump Flow Rate Calibration Press for instructions Reset Flow Rate Cal Set Flow Rate to 1 00 Current Pump Pressure 5 00 minute timer Enter new Flow Rate Cal Store Calibration Value Log Calibration Value Current Calibration Date Last Calibration Date Instructions Reset Cal 1 00 mL min 800psi 5 00 min Calibrate Log 3 9 2003 392003 Degas Calibration Conductivity Cell Calibration Press for instructions Instructions Press for instructions Degas Calibration Calibrate Set Cell Temp to 35 C Cell 35 C Log Calibration Value Log Set Flow Rate to 1 00 0 Degas Pressure Total Conductivity 0 061 pS Current Cal Date 3 19 2003 Cond Cell Calibration Calibrate Last Calibration Date 3 19 2003 Log Calibration Value Log Electric Conductivity Cell Calibration Press for instructions Instructions Last Calibration Date Current Calibration Date 3 19 2003 Instructions 1 00 mL min 3 19 2003 Conductivity Cell Offset Cal Offset Cal
20. 1 4 28 Check valve cartridges Piston Piston seal Piston rinse seal O ring for waste valve or priming valve Eluent valve 10 cc syringe for priming eluent lines Sample Loop and Injection Valve 25 uL sample loop Injection valve Luer adapter fitting 1 4 28 for manual injections 1 cc syringe for manual injections Injection valve rebuild kit Suppressors Cell and Column Heater AAES Anion Atlas Electrolytic Suppressor Doc 031879 01 3 03 D 1 ICS 1000 lon Chromatography System Part Number 056118 053946 053949 057985 058060 059979 060943 058062 923686 043598 954745 060494 060392 058053 055647 060581 057954 Item CAES Cation Atlas Electrolytic Suppressor ASRS Ultra 4 mm Anion Self Regenerating Suppressor CSRS Ultra 4 mm Cation Self Regenerating Suppressor DS6 heated conductivity cell Column heater assembly Column heater heat exchanger 0 25 mm 0 010 in ID tubing Column heater heat exchanger 0 125 mm 0 005 in ID tubing Column heater cover assembly Relay TTL 12 position connector plug Twisted pair of wires Miscellaneous IEC 127 fast blow fuses rated 3 15 amps USB cable 5 m 16 ft External USB hub Leak detector Maintenance Kits AS40 ASM preventive maintenance kit ASSO preventive maintenance kit ICS 1000 preventive maintenance kit Doc 031879 01 3 03 E FAQ E 1 How dol hook up an autosampler For instructions on how to connect the ICS 1000 to an AS50 aut
21. 2 NEN ICS 1000 ION CHROMATOGRAPHY SYSTEM OPERATOR S MANUAL O 2003 Dionex Corporation Document No 031879 Revision 01 March 2003 2003 by Dionex Corporation All rights reserved worldwide Printed in the United States of America This publication is protected by federal copyright law No part of this publication may be copied or distributed transmitted transcribed stored in a retrieval system or transmitted into any human or computer language in any form or by any means electronic mechanical magnetic manual or otherwise or disclosed to third parties without the express written permission of Dionex Corporation 1228 Titan Way Sunnyvale California 94088 3603 U S A DISCLAIMER OF WARRANTY AND LIMITED WARRANTY THIS PUBLICATION IS PROVIDED AS IS WITHOUT WARRANTY OF ANY KIND DIONEX CORPORATION DOES NOT WARRANT GUARANTEE OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES TRADEMARKS MMS MicroMembrane Suppressor is a trademark of Dionex Corporation AES Atlas Electrolytic Suppressor Chromeleon OnGuard and SRS Self Regenerat
22. 3 The priming procedure consists of two parts Priming the eluent lines with a syringe Perform this procedure at initial installation after changing eluents or when eluent lines are empty Priming the pump heads with the Prime button Perform this procedure after the eluent lines are primed B 14 1 Priming the Eluent Lines with a Syringe NOTE Prime the eluent lines after initial installation after changing eluents or when eluent lines are empty 1 Verify that the pump is turned off 2 Connect a 10 mL syringe P N 054578 to the port in the priming valve on the primary pump head see Figure B 35 Secondary Pump Head sh SK Waste Valve KL close i ml Primary FT Pump Head 10 mL Syringe os Y Priming Valve PIN 054578 open Figure B 35 Priming the Eluent Lines B 36 Doc 031879 01 3 03 Priming the Pump Open the priming valve by turning it one quarter to one half turn counterclockwise On the Chromeleon Control Panel click Pump Settings and then click Eluent Flow Valve Open see Figure B 36 A ICS 1000 System ICS 1000 AMAR ICS 1000 Pump Sample Pressure 1 00 ml min d 1000 Injector jr Flow Valve pex inject Max Pressure 5000 psi _ Injector Settings SIUM ES 1 Curr Pressure 800 psi 0 00 ump PumpSet ngs dete On os Prime Closed Open ICS 1000 Detector
23. Control menu and click the name of the ICS 1000 timebase from the list at the bottom of the menu Pump ECD DeviceType Pump Sample System Log Audit Trail on TimeBaseName ump PumpMode Datasource 1 Sample 1 Pump Settings Program 1 5 Total Program Time 5ystem PgmEn Connected Startup Shutdown Show Plot Pump_ECD DeviceType Injector Elapsed Program Time ystem Retentio P ror tra Syste Load Inject i olume d from Pos Position Injector Settings ump ECD DeviceType Detector ECD_1 Sig Suppressor Suppre 1 fessor Cur Detector Settings i Figure 3 5 ICS 1000 System Control Panel Unconnected Doc 031879 01 3 03 3 5 ICS 1000 lon Chromatography System Figure 3 6 shows a connected Control Panel for an ICS 1000 system IB ICS 1000 System CS 1000 Pump ICS 1000 AMAR Sampl B On Datasource 16 07 29 User AMar from AMAR 800 Wi sors has connected to timebase ICS 1000 Sequence 16 07 29 User AMar from AMAR Sample has acquired control over timebase ICS 1000 Pump Settings Settings Program CS 1000 Injector Elapsed Program Ti
24. E 2 Startup 3 3 Status 3 11 System backpressure 2 23 System components Descriptions 2 19 System Control Panel 3 5 B 51 See also Control Panel System overview 1 4 System properties dialog box B 16 T Technical Support 5 1 Temperature Cell heater 2 27 Column heater 2 5 2 26 Minimizing the effect of variations 2 27 Temperature compensation 2 27 A 3 Time 2 15 Timebase Chromeleon 3 5 Adding devices to a timebase B 16 B 17 Assigning the ICS to a timebase B 13 B 15 TO MODULE USB port connections B 10 Top cover 2 3 Troubleshooting 4 1 Alarm conditions 4 3 Baseline noise or drift 4 19 Calibrations 5 1 Diagnostics 5 1 Error messages 4 3 Excessive backpressure 4 15 Flow rate 4 14 High cell output 4 18 Installation B 53 Liquid leaks 4 9 No cell response 4 18 Peak ghosting 4 16 Peak height 4 17 Pump 4 11 4 13 Retention time 4 17 Selectivity 4 17 Vacuum degas assembly 4 20 TTL and relay connector C 1 Connection instructions C 2 Pin assignments C 1 TTL inputs Default function assignments C 2 Rear panel connector 2 8 Index 8 Doc 031879 01 3 03 Index TTL outputs Controlling C 5 Rear panel connector 2 8 Tubing Replacing 5 9 Requirements 5 9 Routing clips 2 8 Tubing connections Isolating a restriction 4 6 5 7 TUV 1 8 U Unassigned USB Devices B 13 Unpacking B 2 Computer B 4 USB cable B 10 USB connections 2 7 B 9 B 10 Una
25. Figure C 6 INIT LOAD Figure C 8 Example AS50 Method for Stand Alone Operation Doc 031879 01 3 03 C 9 ICS 1000 lon Chromatography System Timed Event Notes e At time INIT the injection valve is set to Load e 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 e Attime 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 e TTL does not need to be set in the timed events because the Load and Inject commands control the ICS 1000 injection valve automatically see Enable AS50 Control of the Injection Valve on page C 9 To run the above method set up an AS50 schedule The example in Figure C 9 includes a four point calibration Lines 1 4 followed by two samples Lines 5 and 6 Figure C 9 Example AS50 Schedule for Stand Alone Operation C 10 Doc 031879 01 3 03 Part Number 046548 039164 057937 057938 045721 045722 045994 052840 055870 048722 055752 057945 054578 042857 057968 024305 016388 057896 056116 D Reordering Information Item Reservoirs 2 L plastic reservoir assembly includes stopper and cap 4 L plastic reservoir assembly includes stopper and cap Pump Primary pump head assembly Secondary pump head assembly Outlet check valve assembly 10 32 Inlet check valve assembly
26. High Cell Outputs ees ost ces eked Re De Reade 4 18 Doc 031879 01 3 03 iii ICS 1000 lon Chromatography System 4 13 Baseline Noise or Drift 4 19 4 14 Vacuum Degas Assembly Does Not Run 4 20 5 Service 5 1 Diagnostic and Calibration Procedures 5 1 5 1 1 Chromeleon Wellness Panel Overview 5 2 5 1 3 Calibrating the Conductivity Cell 5 4 5 1 3 Calibrating the Flow Rate 5 6 5 1 4 Calibrating the Vacuum Degas Assembly 5 7 5 2 Isolating a Restriction in the Liquid Lines 5 7 5 3 Replacing Tubing and Fittings 5 9 5 4 Rebuilding the Injection Valve 5 10 5 5 Cleaning and Replacing the Pump Check Valves 5 11 5 6 Replacing a Pump Piston Seal and Piston Rinse Seal 5 13 5 7 Replacing a Pump Piston 5 17 5 8 Replacing the Waste Valve or Priming Valve O Ring 5 18 5 9 Replacing the Conductivity Cell 5 20 5 10 Replacing the Suppressor 5 22 5 11 Replacing the Column Heater 5 23 5 12 Replacing the Column Heater Heat Exchanger 5 25 5 13 Replacing the Eluent Valve 5 26 5 14 Rep
27. PRESSURE HARDWARE ERROR This error indicates an error in the pump controller electronics To troubleshoot e Contact Dionex for assistance The ICS 1000 electronics components cannot be serviced by the user PUMP OVER PRESSURE The ICS 1000 has a maximum system pressure limit of 34 5 MPa 5000 psi The pressure limit can be lowered from Chromeleon in the Server Configuration or in the control program If the system pressure exceeds the set limit for at least 0 5 seconds the pump stops and the Pump over pressure error message appears To troubleshoot 1 Check for blockages in the liquid lines by working your way backward from the cell to the pump See Figure 2 6 for the flow schematic 2 Check that the flow rate is set to the correct value 3 Check that the high pressure limit is set to the correct value 4 Restart the pump Doc 031879 01 3 03 4 Troubleshooting PUMP UNDER PRESSURE The ICS 1000 has a minimum pressure limit of 0 The low pressure limit can be raised from Chromeleon in the Server Configuration or in the control program If the system pressure falls below the low pressure limit the pump stops and the Pump under pressure error message appears To troubleshoot 1 2 3 4 5 Make sure the eluent reservoir is full Check for liquid leaks see Section 4 2 Check that the waste valve is closed Prime the pump see Section B 12 Restart the pump SUPPRESSOR OVE
28. Preferences dialog box see Figure B 5 Select the License tab and click Dongle Enter the Key Code exactly as it appears on the Chromeleon Software License key code sheet Click OK Preferences m e Figure B 5 Preferences License Page 6 Check the Server Monitor status It should now display Chromeleon Server is running idle see Figure B 6 Chromeleon Server Monitor Chromeleon Server is running ide BEI F3 EE Figure B 6 Server Running 7 Click Close to close the Server Monitor window 8 Go on to Section B 5 B 8 Doc 031879 01 3 03 Connecting the ICS 1000 to the Chromeleon PC B 5 Connecting the ICS 1000 to the Chromeleon PC The ICS 1000 rear panel provides a USB receptacle for connecting the ICS 1000 to a USB port on the Chromeleon PC The rear panel also provides two USB ports for connecting other Dionex USB compliant modules to the system IMPORTANT Do not turn on the power to the ICS 1000 or other USB module s until after you connect the USB cable Before connecting the USB cable verify that Chromeleon is installed If not Windows will be unable to identify the new USB device when the power is turned on See Section B 3 to install Chromeleon B 5 1 Connecting the ICS 1000 to the PC 1 Locate the USB cable P N 960779 in the ICS 1000 Ship Kit P N 057905 2 Plug the cable s A connector into a USB port on the Chromeleon PC and
29. Primary and Secondary Pump Heads with Drain Tubes Doc 031879 01 3 03 B 49 ICS 1000 lon Chromatography System b Push the 152 cm 60 in piece of clear tubing onto the drain tube on the top of the primary pump head This is the waste line Route this waste line through the lower tubing chase and out the back of the ICS 1000 c Push the 15 cm 6 in piece of clear tubing over the drain tube on the top the secondary pump head Push the other end of the tubing over the drain tube on the bottom of the primary pump head d Place a 10 mL syringe P N 054578 at the end of the waste line press the syringe against the line to form a seal and draw out all of the air e Push approximately 5 cm 2 in of black 0 25 mm 0 01 in ID tubing P N 057057 into the end of the waste line NOTE The black tubing creates a flow restriction Assuming a height difference of about 76 cm 30 in between the flush bottle and the waste container this setup provides a flow of one drop of flush solution every 5 to 30 seconds f Place the end of the waste line in a waste container g This completes the piston seal wash installation Periodically refill the flush bottle and empty the waste container as required Flush Tubing 117 cm 46 in long Bottle Y Secondary Pump Head A Tubing 152 cm 60 in long Tubing 15 cm 6 in long Insert black tubing into Waste end of waste li
30. Sequence Specify where to save the sequence Press Next to save it Name amp Title Remember to enter a new sequence name unless you want to overwrite an old sequence Sequence Name Installation Example Y Title M r Location Datasource AMAR _local Directory Browse EISE eram Figure B 31 Example Sequence Wizard Step 5 18 Click Next gt and then click Done on the last page of the Sequence Wizard The Browser appears displaying the sequence you created see Figure B 32 Notice the three files in the top pane of the Browser window AMAR local H DEMO MP AS17 Production Test Chromatogram pgm Hu Dionex Templates M 4817 Production Test Chromatogram ant 7 G ICs 1000 fq 1cS 1000_System pan 2f Ea Installation Example Method 4517 Produ Name A Sample 1 20 0 AS17 Produ Single Figure B 32 Example Browser with Open Sequence Doc 031879 01 3 03 B 33 ICS 1000 lon Chromatography System e The pgm file program contains commands and parameters for controlling the ICS 1000 controlling the autosampler if used and acquiring sample data e The qnt file quantification method contains peak identification and area determination parameters e The pan file Control Panel lets you control and or monitor the ICS 1000 and other modules that are connected to the timebase NOTE The sequence that you create here is i
31. Start Continue Schedule ICS 1000 TTL Inputs TTLIN 1 Inject TTL IN 2 Autozero TTL IN 3 Pump On Off TTL IN 4 Mark RELAY OUT Third Party Analog to Digital Converter and Controller Connection AS50 TTL Out 1 to ICS 1000 TTL In 1 AS50 TTL Out 2 to ICS 1000 TTL In 2 AS50 RLY Out 2 to ICS 1000 TTL In 3 AS50 RLY Out 1 to Third party DAC RLY In Third party ADC RLY OUT to AS50 TTL In 2 AS50 TTL Inputs TTL IN 1 unassigned TTL IN 2 Start Continue Schedule TTL IN 3 Tray Temp On Off TTL IN 4 Therm Compart On Off Figure C 6 Example Connections for Stand Alone Operation Doc 031879 01 3 03 C TTL and Relay Control Enable AS50 Control of the Injection Valve 1 On the ASSO front panel press Menu and 0 to go to the TIME FUNCTION OUT screen In the LOAD INECT VALVE TTL 1 field select ENABLED NABLED DISABLED Figure C 7 AS50 Time Function Out Screen 2 Turn the AS50 power off and then back on You can now issue commands from the AS50 to switch the ICS 1000 injection valve position 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 1000 rear panel see Figure C 6 Create an AS50 Method and Schedule Figure C 8 is an example of AS50 method timed events that can be used with the TTL Relay connections shown in
32. assembly P N 045722 on the bottom of the primary pump head Install the outlet check valve assembly P N 045721 on the top of the head Tighten the check valves fingertight and then use a wrench to tighten an additional one quarter to one half turn Overtightening may damage the pump head and check valve housing and crush the check valve seats CAUTION 8 Reconnect the liquid lines Turn on the ICS 1000 main power 9 Open the eluent valve from the ICS 1000 Control Panel in Chromeleon 10 Prime the pump see Section B 12 11 When the ICS 1000 is at operating pressure check for leaks from the check valves Tighten a check valve a little more only if it leaks Cleaning Check Valves 1 Carefully remove the check valve cartridges from the valve housings 2 Place the check valve housings and cartridges in a beaker with methanol Sonicate or agitate the parts for several minutes 3 Rinse each check valve housing and cartridge thoroughly with filtered deionized water 4 SeeStep 6 through Step 11 above to reinstall the check valves and complete the procedure 5 12 Doc 031879 01 3 03 5 Service 5 6 Re placing 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
33. aus VORSICHT B 48 Doc 031879 01 3 03 Pump Continuous Seal Wash Connections Optional B 21 Pump Continuous Seal Wash Connections Optional The pump includes a seal wash assembly that can be set up to continuously rinse the back of the piston seals to remove salt crystals and prolong the life of the seals Follow the steps below to set up this feature 1 Fill a flush bottle with either deionized water or a combination of deionized water and 10 or 20 isopropyl alcohol Isopropyl alcohol will inhibit bacterial growth in the water 2 Place the flush bottle on top of the ICS 1000 During operation gravity maintains flow through the pump heads 3 The flush solution is carried to the piston seal wash assembly and out to waste via 1 5 mm 0 06 in ID tubing P N 055847 Locate this tubing in the ICS 1000 Ship Kit and cut the tubing into three unequal pieces in the following lengths e 117 cm 46 in e 152 cm 60 in e 15 cm 6 in 4 Install the tubing as follows see Figure B 47 and Figure B 48 a Push the 117 cm 46 in piece of clear tubing onto the drain tube on the bottom of the secondary pump head Place the free end of this tubing in the flush bottle Make sure the end of the tubing is near the bottom of the bottle Drain Tube Drain Tube Primary Pump Head Note The drain tubes on the bottom of each pump head are not visible in the photo Secondary Pump Head li Figure B 47
34. can be run either manually one at a time or automatically in groups or batches 3 11 1 Manual Sample Processing To process samples manually select operating parameters and commands from the Chromeleon menu bar toolbars and Control Panel Commands are executed as soon as they are entered 1 Complete the steps in Sections 3 2 through 3 8 to prepare for operation and start up the ICS 1000 Load the sample using a syringe vacuum syringe or autosampler see Section 3 10 Select Acquisition On from the Control menu Chromeleon records the signal supplied by the detector and displays the signal plot on the Control Panel Click the Autozero button on the Control Panel Inject the sample see Section 3 10 4 Monitor the chromatogram on the Control Panel and select Acquisition Off from the Control menu 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 Doc 031879 01 3 03 3 Operation and Maintenance new manual sample is processed To save the data from a manual run select the MANUAL folder select Save As from the File menu and enter a new name for the sequence 3 11 2 Automatic Batch Sample Processing For batch processing you use Chromeleon to create a list of samples a sequence to be processed automatically For each sample the sequence includes a program with
35. ce que la prise de base soit situ e install e pr s du module et facilement accessible gt MISE EN GARDE STROMSCHLAGGEFAHR Zur Vermeidung von elektrischen Schlagen ist eine geerdete Steckdose zu verwenden Das Gerat darf nicht ohne Erdung betrieben bzw an Wechselstrom angeschlossen WARNUNG Werden Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist gt I gt VORSICHT Doc 031879 01 3 03 B 11 ICS 1000 lon Chromatography System B 7 Turning On the ICS 1000 Power Before turning on the ICS 1000 power verify that Chromeleon IMPORTANT Software is installed See Section B 3 for installation instructions If Chromeleon is not installed first Windows will be unable to identify the new USB device 1 Ifitis not already on turn on the computer power and log onto Windows 2000 or Windows XP as an administrator Power B switch 2 Press the power switch on the ICS 1000 rear panel see uu Figure B 9 to turn on the power Figure B 9 ICS 1000 Rear Panel 3 Windows automatically detects the new USB device A message flashes on the screen to inform you that new hardware was found Chromeleon Server Mon Installing 4 Go onto Section B 8 B 12 Doc 031879 01 3 03 Setting Up Chromeleon B 8 Setting Up Chromeleon NOTE This section provides brief instructions fo
36. 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 When the waste valve is in the open position all output is directed to waste NOTE The waste valve must be open when the pump is being primed using the Prime button For detailed priming instructions see Section B 12 2 22 Doc 031879 01 3 03 2 Features Pressure Transducer Flow exiting the secondary pump head is directed to the pressure transducer see Figure 2 12 which measures the system pressure Pressure measurements which can be monitored from the Chromeleon Control Panel indicate that the pumping system is delivering smooth accurate flow The system pressure should remain consistent no more than a 396 difference from one pressure reading to the next High and low pressure limits can be used to stop the pump flow if a limit is exceeded See Section 4 1 for troubleshooting information if a pressure limit is exceeded Pulse Damper Flow output from the pressure transducer continues to the pulse damper which smooths minor pressure variations From there flow is directed to the injection valve and then to the remainder of the chromatography system Piston Seal Wash The pump includes a piston seal wash assembly that can be set up to continuously rinse the back of the piston seals to remove salt crystals and prolong the lif
37. dialog box opens see Figure B 13 The General page shows the Device Name Pump_ECD the Mode Live and the Module Serial No Dionex ICS 1000 System x Solvents Eluent Generator State Devices Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General Options Signals Head Type amp Limits Device Name MR m Mode Live Module Serial No 200011 Download Moduleware version Virtual Use Live mode to control a physical module connected to the server Virtual mode can be used to demonstrate the software support for the module and allows one to create methods and panels without having a physical module attached to the server Figure B 13 ICS 1000 System Properties 13 Close the dialog box and then save the configuration select File gt Save Installation 14 Ifyouare going to add one or more DX LAN devices to the timebase go on to Section B 8 2 Otherwise exit the Server Configuration program and then go on to Section B 9 B 8 2 Assigning DX LAN Devices to the Timebase Optional Follow the instructions in this section if you are adding one or more devices to the timebase that are connected to the PC through a DX LAN interface not through USB connections 1 Follow the instructions in nstalling the Chromeleon IC System Document No 031883 to add the DX LAN card to the server configuration as a sharable device B 16 Doc 031
38. in Chromeleon See Section 4 1 for troubleshooting information The column heater can either be installed at the factory or ordered separately P N 058060 2 26 Doc 031879 01 3 03 2 Features 2 4 6 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 1000 For details about any of the suppressors or for information about selecting a suppressor for your application refer to the suppressor manuals The manuals are on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 2 4 7 DS6 Heated Conductivity Cell The ICS 1000 flow through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell Two passivated 316 stainless steel electrodes are permanently sealed into the PEEK cell body The cell design provides efficient sweep out low volume 1 pL and low dispersion Temperature control and compensation help ensure good peak reproducibility and baseline stability Temperature Control Temperature directly affects the conductivity of a solution For example laboratory heating and air conditioning systems can cause a regular slow cycling in the baseline This in turn can affect the reproducibility of an analysis The high
39. in the ICS 1000 Ship Kit P N 057905 e The cell is out of calibration See Section 5 1 2 for calibration instructions e See Section 4 12 for additional troubleshooting information Doc 031879 01 3 03 E 3 ICS 1000 lon Chromatography System E 4 Doc 031879 01 3 03 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 Capacity factor is a dimensionless measure of retention which is independent of column length or eluent flow rate It is calculated as follows Where t retention time t retention time of unretained solute column void volume Doc 031879 01 3 03 F 1 ICS 1000 lon 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 k I A Where length A area of one electrode the other electrode is equal to the first C
40. lon Chromatography System LED Label Load Inject Alarm Module Connected Acquiring Data Pump Suppressor Column Heater INJECT VALVE Load Inject 3 Module Connected Acquiring Data Pump O Suppressor O Column Heater STATUS Figure 2 2 Status LEDs If On Green Injection valve is in Load position Injection valve is in Inject position No on green state ICS 1000 is connected to a Chromeleon timebase Sequence or manual data acquisition is in progress Pump is on Suppressor is on and current is being applied to it Column heater is at set temperature If Flashing Valve error Valve error Error detected Check the Chromeleon Audit Trail for the cause Does not flash Sequence has stopped due to an error High or low pressure limit is exceeded The pump is turned off Continuity check failed or suppressor is over the voltage current or power limit The suppressor is turned off Column heater is transitioning to a new temperature Table 2 1 ICS 1000 Status LED States Doc 031879 01 3 03 2 Features 2 1 2 Top Cover Figure 2 3 illustrates the top cover of the ICS 1000 ui Figure 2 3 ICS 1000 Top View Reservoir Storage The ICS 1000 top cover has room for up to three 2 L plastic reservoirs P N 044129 Tubing Chase The tubing chase under the top cover routes tubing
41. plug the cable s B connector into the USB receptacle labeled FROM PC on the ICS 1000 rear panel see Figure B 7 B ICS 1000 A USB Cable Chromeleon PC Plug the USB cable s B Plug the USB cable s A connector into the FROM PC connector into the USB receptacle on the ICS 1000 port on the Chromeleon PC lt BI gt ini Figure B 7 Example Connections One ICS 1000 Connected to the Computer FROM PC USB receptacle on the ICS 1000 rear panel Doc 031879 01 3 03 B 9 ICS 1000 lon Chromatography System B 5 2 Connecting Additional USB Devices The ICS 1000 provides two USB ports for connecting additional Dionex USB compliant modules to the system To connect an additional USB module plug the A connector on a USB cable into an A port labeled TO MODULE on the ICS 1000 rear panel and plug the cable s B connector into the USB receptacle on the USB module see Figure B 8 B ICS 1 cs 8 A N USB Cables A Chromeleon PC Dionex Dionex USB Module USB Module Figure B 8 Example Connections Two Dionex USB Modules Connected to the ICS 1000 NOTE If the number of USB devices in the system exceeds the number of available USB ports connect the devices to the system with a USB compliant full speed external hub One or more hubs is also required if the ICS 1000 or other USB device is more than 5 meters 16 ft from the PC Refer to
42. reservoirs Manual Degassing of Eluent 1 Prepare the eluent required for the application and pour it into a vacuum flask 1 Pour the deionized water into a vacuum flask 2 Attach the flask to a vacuum pump or water aspirator 3 Vacuum degas the eluent deionized water for 5 to 10 minutes by shaking or sonication 4 Remove the flask from the vacuum Do not allow water to flow from the aspirator back into the flask 5 Pour the degassed eluent deionized water into a pressurizable reservoir Do not shake the eluent 6 Install an end line filter on the eluent deionized water line see Section 3 4 3 7 Pressurize the reservoir see Section B 20 3 4 3 Filter the Eluent Filtering removes small particulates in the eluent that may contaminate the pump check valves and cause erratic flow rates or loss of prime An end line filter P N 045987 is provided in the ICS 1000 Ship Kit P N 057905 for this purpose Install the end line filter on the end of the eluent line inside the reservoir Verify that the end of the filter extends to the bottom of the reservoir and that the filter is submerged in eluent This prevents air from being drawn through the lines Refer to the Pressurizable Reservoir Installation Instructions for details Doc 031879 01 3 03 3 7 ICS 1000 lon Chromatography System 3 4 4 3 4 5 Fill the Reservoir Fill the reservoir with the prepared eluent Set the Eluent Level After filling the
43. 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 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 The follower is the cylinder that holds the piston in place as it moves in and out of the pump head assembly Reinstall the head and piston assembly use a wrench to tighten the nuts evenly 12 in lb torque Completing the Procedure 1 2 3 4 Reconnect all liquid lines to the pump head Turn on the main power switch Open the eluent valve Prime the pump see Section B 12 5 7 Replacing a Pump Piston Continued leaking of the piston seal after installation of a new seal assuming the pump head is tight indicates a dirty scratched or broken piston Follow the instructions in Section 5 6 to install a new piston P N 052840 and piston seal P N 055870 Doc 031879 01 3 03 5 17 ICS 1000 lon Chromatography System 5 8 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 Control Panel in Chromeleon 2 Turn off the main power switch to ensure that you do not unintentionally start the ICS 1000 3 To remove the waste valve or priming valve from the pump head see Figure 5 7 turn the knob coun
44. valve see Figure 3 9 and attach a shorter line 25 to 30 cm 10 to 12 inches of PEEK or Teflon tubing Place the free end of the line into the sample Verify that the injection valve is in the Load position Insert the 1 cc syringe P N 016388 provided in the ICS 1000 Ship Kit P N 057905 into the injection port on the ICS 1000 front door see Figure 2 1 and pull out the plunger to draw the sample into the injection valve Switch the injection valve to the Inject position see Section 3 10 4 Loading Samples with an Autosampler 1 Verify that the autosampler output line is connected to port S 5 of the ICS 1000 injection valve Prepare and fill the sample vials and place them in the autosampler tray or cassette Refer to the autosampler manual for detailed instructions The sample loading process depends on the autosampler Refer to the autosampler manual for detailed instructions In general use one of the following methods Include the commands for controlling sample loading in a Chromeleon program See the examples in Section 3 10 5 e Enter the commands for loading the sample from the autosampler front panel Switch the injection valve to the Inject position see Section 3 10 4 NOTE If you are running the ICS 1000 without Chromeleon control see Section C 3 for stand alone setup and operation instructions using an AS50 autosampler Doc 031879 01 3 03 3 Operation and Maintenance 3 10 4 I
45. 3 2 19 ICS 1000 lon Chromatography System device icon under the timebase and select Properties from the Edit menu Select the Options tab see Figure 2 10 Dionex ICS 1000 System Ea Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General Options Signals Head Type amp Limits Solvents State Devices m Installed Options M Degas M Column Heater r Degas Mode C Always Off C Always On C Cycle On F 0 120 sec E 0 5940 sec Cancel Help Figure 2 10 Server Configuration Properties Degas Mode Options Degas Mode Options e Always Off The degas pump is always off e 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 e Cycle The degas pump cycles on and off according to the times specified in the Cycle On and Off fields Cycle On specifies for how long the degas pump runs during a cycle Cycle Off specifies the time between cycles e Monitor default mode The ICS 1000 monitors the degas pressure reading and turns the degas pump on and off as required 2 20 Doc 031879 01 3 03 2 Features 2 4 2 Eluent Valve Figure 2 11 Eluent Valve 2 44 3 Pump The eluent valve controls the flow from the eluent reservoir It opens automatically when the pump is running and closes when the pump is off The valv
46. 31879 01 3 03 Contents 3 10 Loading and Injecting Samples 3 14 3 10 1 Loading Samples with a Syringe 3 15 3 10 2 Loading Samples with a Vacuum Syringe 3 16 3 10 3 Loading Samples with an Autosampler 3 16 3 10 4 Injecting Samples 3 17 3 10 5 Example Chromeleon Commands for Loading and Injecting Samples 3 17 3 11 Process Samples 3 18 3 11 1 Manual Sample Processing 3 18 3 11 2 Automatic Batch Sample Processing 3 19 3 12 Maintenance coceesvceevept OPI PUO p ee OUR RR Ep S 3 21 4 Troubleshooting 4 1 Alarms and Error Conditions 4 3 4 2 Liquid Leaks sax ati munis DEREN dant deed 4 9 4 3 Pump Difficult to Prime or Loses Prime 4 11 4 4 Pump Does Not Start 4 13 4 5 NO FLOW aan nm fot ute nat en Me du E Damien een 4 14 4 6 Erratic Flow Pressure Reading 4 15 4 7 Excessive System Backpressure 4 15 4 8 Peak Ghosting 2 ota o ex e pere due nta Pi don ace Re d 4 16 4 9 Nonreproducible Peak Height or Retention Time 4 17 4 10 Abnormal Retention Time or Selectivity 4 17 4 11 No Cell Response 4 18 4 12
47. 879 01 3 03 Setting Up Chromeleon 2 Select the timebase that was created for the ICS 1000 see Figure B 14 then click the Add device icon a on the toolbar or select Edit gt Add Device Server Configuration Chromeleon Server Configuration Figure B 14 Example ICS 1000 Timebase The Add device to timebase dialog box appears 3 Ifit is not already selected select Dionex under Manufacturers and then select the device from the Devices list 1 Add device to timebase Dionex Fi AD20 Detector Figure B 15 Add Device to Timebase Dialog Box Doc 031879 01 3 03 B 17 ICS 1000 lon Chromatography System 4 Click OK A configuration properties dialog box for the device appears Figure B 16 shows an example of the properties for an AS50 Autosampler Dionex AS50 Autosampler Figure B 16 AS50 Configuration Properties 5 On the General tab page clear the Demo Mode check box if it is currently selected and then select the DX LAN Device ID number Note Devices display their DX LAN ID numbers when their power is turned on Click OK to close the dialog box Save the configuration select File gt Save Installation Exit the Server Configuration program en oO Go on to Section B 9 B 18 Doc 031879 01 3 03 Installing and Plumbing the Columns and Suppressor B 9 Installing and Plumbing the Columns and Suppressor NOTE This section provides brief installation and plum
48. Alarms and Error Conditions See SUPPRESSOR STOPPED FOR FLOW RATE page 4 9 Table 4 3 ICS 1000 Alarms and Error Messages Summary Continued Other Operating Problems See Liquid Leaks page 4 9 Pump Difficult to Prime or Loses Prime page 4 11 Pump Does Not Start page 4 13 No Flow page 4 14 Erratic Flow Pressure Reading page 4 15 Excessive System Backpressure page 4 15 Peak Ghosting page 4 16 Nonreproducible Peak Height or Retention Time page 4 17 Abnormal Retention Time or Selectivity page 4 17 No Cell Response page 4 18 High Cell Output page 4 18 Baseline Noise or Drift page 4 19 Vacuum Degas Assembly Does Not Run page 4 20 Table 4 4 Operating Problems Summary Doc 031879 01 3 03 4 Troubleshooting 4 1 Alarms and Error Conditions If any of the following alarm conditions occurs a message is displayed in the Chromeleon Audit Trail COLUMN HEATER EXCEEDS SAFE TEMPERATURE This error occurs when the column heater temperature is higher than the maximum allowed This error may occur if the ICS 1000 is operating in an extreme environment greater than 40 C To troubleshoot e Refer to Section A 3 for environmental specifications COLUMN HEATER OPEN CIRCUIT This error message occurs when the column heater is unplugged from the component panel To troubleshoot 1 Check that the column heater is correctly plugged into the component panel 2 Ifthe error persists the column heater may be faulty Re
49. Chromeleon Sequence Wizard Step 2 of 5 Unknown Samples mpata Figure B 27 Example Sequence Wizard Step 2 6 Select Use Template from the drop down list 7 Inthe Template for Sample Name field type Sample click the right arrow and select Sample Number n 8 Inthe Number of Vials field type 1 9 Use default settings for the remaining parameters on the page NOTE You can edit the sequence later to add more samples and select the injection parameters appropriate for your application Doc 031879 01 3 03 B 29 ICS 1000 lon Chromatography System 10 Click Apply Figure B 28 shows Sequence Wizard Step 2 after a sample is defined Chromeleon Sequence Wizard Step 2 of 5 Unknown Samples Use tenplte MN Sample n fA Sample 1 Figure B 28 Example Sequence Wizard Step 2 with Sample Defined 11 Click Next gt B 30 Doc 031879 01 3 03 Setting Up a Chromeleon Application The Standard Samples page appears see Figure B 29 Chromeleon Sequence Wizard Step 3 of 5 Standard Samples mpata Bie esee Sample 1 1 200 E starnaarals BILE DRISS Figure B 29 Example Sequence Wizard Step 3 12 Click Next gt to omit this step and define standard injections later Or define one or more standard injections and then click Next gt The Methods amp Reporting page appears Doc 031879 01 3 03 B 31 ICS 1000 lon Chromatogr
50. Chromeleon as follows 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 Inthe field next to the Download button verify that Current is selected and then click Download to download the new calibration values to the ICS 1000 d To ensure the new calibration values are recorded in the ICS 1000 memory do not turn off the ICS 1000 power for at least 1 minute after downloading the values 5 12 Replacing the Column Heater Heat Exchanger 1 Turn off the ICS 1000 power Open the front door of the ICS 1000 Unscrew the two thumbscrews on the column I a 1 heater cover they remain attached to the cover Pull the heater cover straight out to remove it Unscrew the six thumbscrews on the top metal plate see Figure 5 14 and remove the plate Disconnect the heat exchanger inlet line from Port C on the injection valve Figure 5 14 ICS 1000 Column Heater Cover Removed Disconnect the heat exchanger outlet line from the guard column inlet Doc 031879 01 3 03 5 25 ICS 1000 lon Chromatography System 10 11 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 Remove the plastic backing from the new heat exchanger P N 059979 with 0 25 mm 0 010 in ID tubing
51. Doc 031879 01 3 03 4 Troubleshooting e Under Installed Options verify that the Degas check box is selected Under Degas Mode verify that the Always Off option is not selected If it is select one of the following settings e Cycle and select On 30 seconds and Off 10 minutes Monitor If the Degas Mode 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 Select the Degas Mode Always On option only when testing the vacuum degas assembly Do not select the Always On option for routine use If the degas pump runs when you select Always On but does not run when Monitor mode is selected recalibrate the degas assembly see Section 5 1 4 Doc 031879 01 3 03 4 21 ICS 1000 lon Chromatography System 4 22 Doc 031879 01 3 03 5 e Service This chapter describes ICS 1000 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 IMPORTANT Subs
52. If the leak persists replace the waste valve O ring see Section 5 8 Leaking suppressor Refer to the suppressor manual for troubleshooting procedures Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 Leaking injection valve Make sure the liquid line connections to the transducer are tight Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is on the Dionex Reference Library CD ROM P N 053891 Replace any damaged fittings Liquid leaks from behind the valve stator may indicate a scratched rotor seal Rebuild the injection valve see Section 5 4 Leaking cell Check the waste lines for blockage trapped particles can plug the lines and cause a restriction and or leak If necessary clear the waste lines by reversing the direction of flow 4 10 Doc 031879 01 3 03 4 Troubleshooting Make sure the plumbing downstream from the cell is clear a blockage may overpressurize the cell causing it to leak If the problem continues contact Dionex for assistance 4 3 Pump Difficult to Prime or Loses Prime 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 e Eluent improperly or insuffic
53. Monitor B 6 Service chase 2 3 2 6 Service procedures 5 12 Check valve cleaning 5 11 5 12 Check valve replacement 5 11 Conductivity cell replacement 5 20 Fuse replacement 5 30 Injection valve rebuilding 5 10 Isolation of liquid lines restriction 5 7 Leak sensor replacement 5 28 Piston replacement 5 17 Piston seal replacement 5 13 Priming valve O ring replacement 5 18 Rebuilding the injection valve 5 10 Replacing tubing and fittings 5 9 Suppressor replacement 5 22 Tubing and fittings replacement 5 9 Waste valve O ring replacement 5 18 Doc 031879 01 3 03 Index 7 ICS 1000 lon Chromatography System Sharable device B 16 Software license B 5 B 6 Specifications Column heater A 4 Conductivity cell A 3 Electrical A 1 Environmental A 1 Injection valve A 3 Physical A 1 Pump A 2 Vacuum degas assembly A 3 Stand alone operation B 43 C 7 C 9 Analog output connection C 9 AS50 setup B 43 C 9 Example connections C 8 TTL and relay connections C 7 Standards When to remake E 2 Starting Chromeleon B 26 Sulfite in samples 3 12 Suppression description 1 3 Suppressor Controlling the current to 2 18 Description 2 6 2 27 Installation B 21 Leaking 4 10 Replacement procedure 5 22 Suppressor alarms Suppressor not connected 4 8 Suppressor over current 4 7 Suppressor over power 4 8 Suppressor stopped for zero flow rate 4 8 Syringe injection 3 15 Vacuum 3 16 System Shutdown
54. NOTE To prevent waste from siphoning back into the system check the lines periodically to be sure they are not bent pinched or elevated at any point B 10 1 Installing the Gas Separator Waste Tube l Locate the gas a R separator waste tube Connect ine assembly see WASTE GAS Figure B 21 in the A line ICS 1000 Ship Kit P N 057905 2 Connect the WASTE GAS SEPARATOR line to the 3 mm 1 8 in ID white Teflon tubing on the gas separator waste tube assembly Figure B 21 Gas Separator Waste Tube Assembly 3 Place the gas separator waste tube assembly into the waste container Make sure the tubing junction where the white Teflon tubing meets the black polyethylene tubing is above the top of the container and Doc 031879 01 3 03 B 23 ICS 1000 lon Chromatography System that the gas separator waste tube and the waste container are open to the atmosphere see Figure B 22 4 Go onto Section B 11 p D Waste Gas Separator Line Gas Separator Waste Waste Tube Assembly Container Figure B 22 Gas Separator Waste Tube Installation DO NOT CAP THE WASTE CONTAINER The ICS 1000 uses an electrolytic process that results in the production of small amounts of oxygen or hydrogen gas To ensure that the gas is not trapped in a closed container and allowed to concentrate install a 1 3 cm 0 52 in ID black gas separator waste tube P N 045460 in an uncapped waste container Connec
55. Place the reservoir on top of the ICS 1000 5 Install the cap and hand tighten NOTE The ICS 1000 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 See Section B 20 for instructions 6 Goon to Section B 12 Doc 031879 01 3 03 B 25 ICS 1000 lon Chromatography System B 12 Setting Up a Chromeleon Application Chromeleon provides application templates which you can use to quickly get started running To use the application templates you need to know the type of column and suppressor you will be using This section shows how to create a list of samples to be processed a sequence and how to use an application template 1 Identify the type of column and suppressor installed in the ICS 1000 2 Start Chromeleon select Start gt Programs gt Chromeleon gt Chromeleon The Chromeleon main window and Browser appear see Figure B 23 Chromeleon AMAR local Dionex Templates Browser File Edit View Workspace Qualification Batch Window Help DHl ES BEN HS es en re AS EEE Gr k dit oer hA JO e E FE AMAR _local Dionex Templates Browser ii AMAR local IC Applications 2 4 2003 11 18 32 A v Dionex Templates Panels 1 6 2003 3 05 51 PM IC Applications E Reports 2 4 2003 11 18 32 amp Ci Panels CN Reports ICS 1000 Ci AUDIT fi manual
56. R CURRENT This error may be caused by an exhausted or dirty suppressor or by a malfunction in the suppressor controller electronics To troubleshoot 1 Follow the instructions in the suppressor manual to regenerate the suppressor Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 Follow the instructions in the suppressor manual to clean the suppressor If a malfunction in the suppressor controller is suspected contact Dionex for assistance The ICS 1000 electronics components cannot be serviced by the user Doc 031879 01 3 03 4 7 ICS 1000 lon Chromatography System SUPPRESSOR OVER VOLTAGE This error appears if you turn on the suppressor and the ICS 1000 cannot establish a connection with the suppressor To troubleshoot 1 Check the suppressor cable connection see Section 5 10 2 Ifthe error persists replace the suppressor see Section 5 10 SUPPRESSOR OVER POWER This error appears when in order to maintain the selected current the ICS 1000 is required to apply a higher voltage than the suppressor can support To troubleshoot Reduce the flow rate Rehydrate the suppressor Refer to the suppressor manual for instructions Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 e Ifthe error persists replace the suppressor see S
57. S 1000 injection valve Connect the TTLs and Relays 1 Locate two twisted pairs of wires P N 043598 and 12 position connector plugs Position 1 P N 923686 see Locking Figure C 5 in the ICS 1000 oan and AS50 Ship Kits Position 12 2 Attach the wires to the connector plug positions indicated in Figure C 6 Figure C 5 12 Position Connector Plug To attach a wire to a connector plug strip the ends of the wire insert into the desired connector position and tighten the locking screw with a screwdriver When attaching wires to the connector plug be careful not to allow stray strands of wire to short to the adjoining position on the connector CAUTION 3 Plug the connector plugs into their respective TTL Relay connectors on the rear panel of each module Make sure the red wires connect to active pins on each module and the black wires connect to ground pins Doc 031879 01 3 03 C 7 ICS 1000 lon Chromatography System ICS 1000 Rear Panel Connections ANALOG OUTPUT TTL OUT TTLIN TTL GND e ALLEE III d i pos 41 12 12 AS50 Rear Panel Connections TTL 1 IN TTL 2 OUT TTL 1 OUT TTL 2 IN TTL3 IN o RLY 2 OUT TTL4IN RLY 1 F TTL IN OUT 8 9 10 red pos black pos 356 DIE 4 212 Analog Data Transfer Start Continue Schedule Start Acquisition ANALOG IN 29 System Function Inject Autozero Pump On Off Start Data Acquisition
58. 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 Regenerant A dilute acid or base that converts ion exchange sites in a MicroMembrane Suppressor back to the form that suppresses the eluent conductivity Resin See Ion Exchange Resin Resolution R A measure of the separation between two sample components This is expressed as the ratio ofthe distance between the two peak maxima to the mean value of the peak width at the baseline R 2 ty t W5 Wi Where t and t the retention times of components 1 and 2 respectively Wi and W the baseline width of peaks 1 and 2 respectively measured in the same units as the retention time R is proportional to the square root of efficiency N A value of R 1 5 represents baseline separation of the two peaks Retention Time The time from injection to peak maximum the basis for identification of a species in chromatographic analysis Separator Column The column used to perform a chromatographic separation also called an analytical column Doc 031879 01 3 03 F Glossary Siemens S Unit measure of condu
59. Verify that the USB cable is connected correctly See Section B 5 for installation instructions Pump is turned off Turn on the pump from the Chromeleon Control Panel Flow rate is set to 0 Set the flow rate from the Chromeleon Control Panel Doc 031879 01 3 03 4 13 ICS 1000 lon Chromatography System 4 5 No Flow e Pump waste or priming valve open see Figure 4 2 Close the valves by turning the knobs clockwise until fingertight DO NOT OVERTIGHTEN Overtightening may damage the valve and the pump head Priming Valve Waste Valve Figure 4 2 Waste and Priming Valves e Flow rate is set to 0 Set the flow rate from either the Chromeleon Control Panel Eluent valve is closed Open the eluent valve from either the Chromeleon Control Panel e Pump not primed Prime the pump see Section B 12 e Broken pump piston Replace the piston see Section 5 7 4 14 Doc 031879 01 3 03 4 Troubleshooting 4 6 4 7 Erratic Flow Pressure Reading Pump needs priming Prime the pump see Section B 12 Damaged piston seal Replace the piston seal see Section 5 6 Dirty pump check valve Clean or replace the check valve see Section 5 5 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 nstallation of Dionex Liquid Line Fittings Document No 031432 for tightening re
60. aphy System 13 Select the Use Application Template check box 14 From the drop down lists select the type of suppressor to be installed and then select the column In the example in Figure B 30 the 4 mm ASRS suppressor and AS17 column are selected Chromeleon Sequence Wizard Step 4 of 5 Methods amp Reporting x Methods amp Reporting Specify a method or select a pre defined template and indicate reporting preferences Applications includes method M Use Application Template Suppressor Type ARS 4mm fast 7 Production Test Chromatogram r Method Files T2raaram juantiGaam EO He program and quentticaton nes wibe imported coped mie te nevi sequence r Preferred Reporting Options Preferred Report T_local Dionex TemplatesXReportsNdefault Browse Preferred Channel These settings are used when you print a report for the sequence or double click a sample tea ree Figure B 30 Example Sequence Wizard Step 4 15 To select a report template click the Browse button go to the Dionex Templates Reports folder and select a template for example default letter 16 Click Next gt The Saving the Sequence page appears B 32 Doc 031879 01 3 03 Setting Up a Chromeleon Application 17 Enter a name for the sequence and a location see the example in Figure B 31 Chromeleon Sequence Wizard Step 5 of 5 Saving the Sequence x Saving the
61. ation failed alarm 4 4 Degassing eluents 2 19 3 6 Delay volume A 2 Detection description 1 3 Detector specifications Cell drive A 3 Linearity A 3 Range A 3 Temperature compensation A 3 Diagnostics 5 1 Dimensions A 1 Dionex Contacting 5 1 Direct control 2 11 Dongle B 6 Drip tray 2 5 DS6 Heated Conductivity Cell See Conductivity cell Duty cycle 2 20 E Electrical specifications Fuses A 1 Main power A 1 Eluent Aqueous 3 21 4 12 Degassing 2 19 Delivery process 1 2 Filtering 3 7 Preparing 3 6 When to remake E 2 Eluent bottle See Eluent reservoir Eluent level 3 8 B 35 Eluent reservoir Connecting 3 8 B 25 Filling 3 8 Gas connection B 47 Monitoring liquid level in 3 8 B 35 Pressurization B 48 Storage on top cover 2 3 Eluent valve 2 5 Replacing 5 26 End line filter See Filter end line Environmental specifications Humidity A 1 Operating pressure A 1 Operating temperature A 1 Equilibration time 3 11 Error messages 4 3 4 8 Column heater exceeds safe temperature 4 3 Column heater open circuit 4 3 Column heater short circuit 4 3 Degas calibration failed 4 4 Hardware not present 4 4 Leak sensor wet 4 4 Load inject valve error 4 5 Option not installed 4 5 Pressure slope calibration error 4 5 Pump motor lost control 4 5 Pump over pressure 4 6 Pump pressure hardware error 4 6 Pump under pressure 4 7 Suppressor not connected 4 8 Suppressor over current 4 7 Supp
62. bing instructions for the columns and suppressor Before beginning the installation refer to the column and suppressor manuals for detailed start up and installation instructions The manuals are provided on the Dionex Reference Library CD ROM P N 053891 which is located in the ICS 1000 Ship Kit P N 057905 Before beginning e Remove the guard column separator column and suppressor from their boxes e Remove the fitting plugs from the ends of each column and from all ports on the suppressor e Discard any tubing temporarily connecting the suppressor ports B 9 1 Column Heater Setup Optional Follow the steps below if the optional column heater is installed 1 Cut off the two shipping ties from the column heater a j Thumbscrew 2 and remove them p see Figure B 17 2 Loosen the two thumbscrews on the heater cover they remain attached to the cover 3 Pull the heater cover straight out to remove it Doc 031879 01 3 03 B 19 ICS 1000 lon Chromatography System 4 Unscrew the six thumbscrews on the top metal plate see Figure B 18 and remove the plate I Thumbscrew 6 5 Goonto Section B 9 2 Figure B 18 ICS 1000 Column Heater Cover Removed B 9 2 Installing the Columns 1 Remove the union connecting GUARD IN and GUARD OUT 2 Connect GUARD IN to the guard column inlet Check the arrow on the column label it should point down flow away from the injection valve
63. c steps for routine operation of the ICS 1000 Power up the system 4 4 Start Chromeleon Set up the reservoir Check all connections J C Prime the pump D Set operating conditions J Equilibrate the system Prepare samples D Verify operating status C Process samples Figure 3 1 ICS 1000 Operation Flow Chart Doc 031879 01 3 03 3 1 ICS 1000 lon Chromatography System Sample Processing Overview Samples can be run either 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 Samples can be loaded into the sample loop with an autosampler or with a syringe through the injection port on the ICS 1000 front door Manual Sample Processing Using Chromeleon Load the sample 4 Start data acquisition C Autozero inject the sample 4 Stop data acquisition d Save the manual Optional sequence data Batch Sample Processing Using Chromeleon Create a Sequence Sequence Wizard t to the Batch 4 4 Start the Batch E the Sequence Figure 3 2 Sample Processing Overview Doc 031879 01 3 03 3 Operation and Maintenance 3 2 Power Up the System Power Switch Press the power swi
64. ch the bottom of the drip tray 5 28 Doc 031879 01 3 03 5 Service 5 15 Priming with Isopropyl Alcohol NOTE Prime the pump heads with isopropyl alcohol only if the two standard priming procedures described in Section B 12 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 B 37 2 Open the waste valve on the secondary pump head see Figure B 37 by turning the knob one quarter to one half turn counterclockwise 3 Click Pump On on the Chromeleon Control Panel to turn on the pump motor 4 Open the priming valve on the primary pump head by turning it one quarter to one half turn counterclockwise 5 Use the syringe to slowly push alcohol through the pump NOTE Be careful not to push any air trapped in the syringe through the pump Check the waste line from the secondary pump head to verify that there are no air bubbles 6 Close the priming valve Do not overtighten Disconnect the syringe from the priming valve 7 Let the pump run for several minutes to purge alcohol from the pump heads and then click Prime and flush the heads with the desired eluent Isopropyl alcohol may damage some columns Be sure to thoroughly rinse the alcohol from the pump using the process described in Step 7 CAUTION 8 Close the waste valve Do not overtighten 9 Select the flow rate required for the analysis 10 Click Pump Off to turn
65. chromatography and BioLC applications and should not be used for any other purpose If there is a question regarding appropriate usage contact Dionex C 1 TTL and Relay Connections A 12 pin connector strip for TTL relay control is located on the ICS 1000 rear panel The connector provides two relay outputs two TTL outputs and four TTL inputs see Figure C 1 Connector Pin Function Position Description p 1 1 m Solid State Relay Contacts Output RELAY 2 OUT 3 2 eee Solid State Relay Contacts Output TTL OUT 1 5 TTL Output 1 1 KQ pull up to 5 100 mA sink 2 6 TTL Output 2 1 kO pull up to 5 100 mA sink 1 7 TTL Input 1 Inject Load TTLIN 2 8 TTL Input 2 Autozero 3 9 TTL Input 3 Pump Suppressor On 4 10 TTL Input 4 Mark TTL GND 1 11 Ground Note The TTL input functions can be reassigned 12 Ground to different inputs Figure C 1 TTL and Relay Connector on Rear Panel Relay loads in excess of 200 mA or with included power supplies over 60 V may damage the relay drivers on the CPU CAUTION Doc 031879 01 3 03 C 1 ICS 1000 lon Chromatography System The outputs can be used to control functions in external devices such as an autosampler or another Dionex module When connected to a controlling device the inputs can be programmed to perform the following ICS 1000 functions Switch the injection valve position load in
66. commands and parameters for controlling the ICS 1000 controlling the autosampler 1f used and acquiring sample data The sequence also includes a quantification method for peak identification and area determination Additional sample processing parameters are included in the sequence for example the sample name sample type injection volume etc After defining the sequence you can start batch processing 1 Complete the steps in Sections 3 2 through 3 8 to prepare for operation and to start up the ICS 1000 2 Create a new sequence or modify an existing one To create a new sequence a Inthe Browser select File New Select Sequence using Wizard and click OK b Complete the steps in the Sequence Wizard adding the desired number of samples and standards to the list For help with any of the steps click the Help button on the Sequence Wizard page NOTE A simple way to get started is to select the Use Application Template option in Step 4 of the Sequence Wizard This option lets you select a column and suppressor type from a list of applications The Wizard then copies a program and quantification method appropriate for the selected application to the sequence folder and adds them to the sequence definition Doc 031879 01 3 03 3 19 ICS 1000 lon Chromatography System 3 To start the sample processing make sure the System Control Panel is open see Section 3 3 and is the active window Then select Edit
67. conductivity Data Rate Sets the rate at which data points are recorded Supp Type Selects the type of suppressor installed SRS Current Sets the current supplied to the suppressor Cell Temp Sets the temperature of the cell SRS Mode Selects whether the suppressor is on or off Show Plot Displays the ICS 1000 detector signal plot in a separate window 2 18 Doc 031879 01 3 03 2 Features 2 4 System Component Details This section provides details about ICS 1000 system components including the vacuum degas assembly optional eluent valve pump injection valve column heater optional suppressor and conductivity cell 2 4 4 Vacuum Degas Assembly Optional The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user The assembly which must be installed in the ICS 1000 at the factory consists of A single channel degas chamber with degas membranes with internal capacity of 17 mL A dual stage diaphragm vacuum pump A solenoid valve An on board vacuum sensor The electronics required to operate the vacuum pump Tubing fittings and other accessories By default the ICS 1000 monitors the degas pressure reading and turns the degas pump on and off as needed A different degas operating mode can be selected from Chromeleon To select degas operating options from Chromeleon open the Server Configuration program select the ICS 1000 Doc 031879 01 3 0
68. control cable s 10 position connector plug to the RELAY CONTROL connector on the AS40 rear panel see Figure B 44 9 Plug the 12 position connector plug into the TTL and relay connector on the ICS 1000 rear panel see Figure B 44 Make sure the red wire connects to position and the green wire connects to position 2 ICS 1000 Rear Panel AS40 Rear Panel TTL Relay Connector RELAY CONTROL READY OUT TTL OUT TTLIN Relay Control Cable TTL GND Figure B 44 Example AS40 Autosampler Connection The AS40 Load relay is now dedicated to the ICS 1000 RELAY OUT 1 Use this relay for running with Chromeleon When you set up the ICS 1000 application see Section B 12 commands for controlling the AS40 Load relay and switching the ICS 1000 injection valve are included by default in the program file see Figure B 45 Doc 031879 01 3 03 B 45 ICS 1000 lon Chromatography System 812A Production Test Chromatogram Commands E E m Production Test Chromatogram Flow i 1 50 For A840 injection 2 300 Pump ECD Relay 1 Closed Duration 138 00 E Relay 1 turned on to start Relay 1 turned off after 0 000 Pump ECD Autozero the AS40 Load cycle and 138 seconds ECD l Acqon load the sample loop Pump InjectValve Inj dcl cM Duration 30 ee 15 000 ECD 1 Acqoff Injection valve Injection valve B switched to Inject switched back End to Load
69. corded When the vacuum degas assembly is running in monitor mode this calibration value is used to determine when to turn on the degas pump 3 Click Log to record the new calibration value in the Audit Trail 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 ICS 1000 flow schematic in Figure 5 2 and work backward through the system beginning at the suppressor Regen Out exit One at a time loosen each fitting and observe the pressure The connection at which the pressure drops abnormally indicates the point of restriction NOTE The numbers on the flow schematic indicate the order in which liquid flows through the system components If the restriction has caused such high pressure that the system cannot be operated you must work forward through the flow schematic adding parts one at a time until an abnormal pressure increase and hence the restriction is found 3 Ifthe restriction is in the tubing or fitting remove the restriction by back flushing or by replacing the tubing or fitting see Section 5 3 Doc 031879 01 3 03 5 7 ICS 1000 lon Chromatography System 9 WASTE ELUENT f OUT OUT e a PUMP 9 Y DEGAS D m Optional Q wn De z COND QUT F 5Sz 5 D 6 CELL B RS z o x TENES u a PULSE r
70. ctance the reciprocal of the electrical resistance of a solution Suppressor A device used to minimize eluent conductivity and convert sample species to a common form thus increasing detection sensitivity Temperature Coefficient The percent of change in the conductivity of a solution with a 1 C change in temperature Every solution has a characteristic temperature coefficient which is determined experimentally Theoretical Plates N See Column Efficiency Void Volume V9 The volume occupied by the eluent in a packed column This volume includes the volume between the injection valve and the column as well as between the column and the detector cell Unretained components are eluted in the void volume Doc 031879 01 3 03 F 5 ICS 1000 lon Chromatography System F 6 Doc 031879 01 3 03 A Air particulate samples 3 12 Air regulator B 47 B 48 Alarm conditions 4 3 4 8 See also Error messages Ambient temperature 4 19 Analog output C 2 Connections C 9 Connector 2 7 Analog to digital controller C 9 Anion separations 3 11 Applications 3 6 C 1 AS40 Automated Sampler Installation B 44 Sample injection 3 16 Yearly maintenance 3 22 ASS0 Autosampler Connections for stand alone operation C 7 Enabling injection valve control B 43 C 9 Installation B 40 Method for stand alone operation C 9 Sample injection 3 16 Schedule for stand alone operation C 9 Time Function Out screen B 43 C 9 Yea
71. ctivity 1s 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 CI analyte These ions preserve electrical neutrality in solution Crosslink Divinylbenzene content in a polystyrene divinylbenzene PS D VB resin this contributes to the mechanical strength of the resin and determines chromatographic properties Equivalent Conductivity The contribution of an ionic species to the total conductivity of a solution as measured in a standard cell having electrodes 1 cm in area and exactly 1 cm apart Guard Column A small column that prevents poisoning of the separator column by sorbing organic contaminants and removing particulates It is filled with the same packing as the separator column Synonymous with Pre Column HETP H Height Equivalent to a Theoretical Plate A measure of column efficiency which allows comparison between columns of different lengths HETP H L N Where L the column length in mm N the number of theoretical plates Ion Exchange Capacity The number of active ion exchange sites in a given weight or volume of resin this is usually expressed in meq g or meq mL Ion Exchange Resin An insoluble polymer matrix containing fixed charge exchange sites anionic or cationic IC resins are formed into small spherical particles beads Doc 031879 01 3 03 F 3 ICS 1000 lon Chromatography
72. e injury Indicates that the function or process of the instrument may be impaired Operation does not constitute a hazard Messages d avertissement en francais Signale une situation de danger imm diat qui si elle n est pas vit e entrainera des blessures graves mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrait gravement endommager l instrument mais qui n entrainera pas de blessures Doc 031879 01 3 03 1 Introduction ACHTUNG WARNUNG VORSICHT Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr Mifiachtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gef hrdung MiRachtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gefahrdung MiRachtung kann zu kleineren oder mittelschweren Verletzungen f hren Wird auch verwendet wenn eine Situation zu schweren Sch den am Ger t f hren kann jedoch keine Verletzungsgefahr besteht Notes Informational messages also appear throughout this manual These are labeled NOTE and are in bold type NOTE NOTES call attention to certain information They alert you to an unexpected result of an action s
73. e can also be opened and closed manually from the Chromeleon Control Panel see Section 2 3 2 This lets you perform service procedures on pump components without eluent leaks occurring The ICS 1000 pump is a microprocessor based isocratic eluent delivery system Its variable speed dual piston series design ensures pulse free pumping for the most demanding applications Primary Pump Head The primary pump head pumps mobile phase into the secondary head see Figure 2 12 The check valves which prevent reverse flow through the pump are located on the bottom inlet and top outlet of the primary pump head The priming valve is on the front of the pump head Doc 031879 01 3 03 2 21 ICS 1000 lon Chromatography System Outlet Check Pressure Valve Transducer Primary Pump Head Secondary Pump Head Priming Valve Inlet Check Waste Valve Valve Figure 2 12 ICS 1000 Pump Components To open the priming valve turn the knob one quarter to one half turn counterclockwise When the priming valve is open liquid can flow into and out of the primary pump head via the port in the front of the valve NOTE The priming valve must be open when the pump is being primed with a syringe or with isopropyl alcohol For detailed priming instructions see Section B 12 Secondary Pump Head The secondary pump head delivers eluent to the remainder of the chromatography system injection valve column and
74. e control of ICS 1000 operation Two modes of software control are available direct control and automated control e With direct control you select operating parameters and commands from the Chromeleon menu bar toolbars and Control Panels Direct control commands are executed as soon as they are entered Section 2 3 2 describes the commands available from the ICS 1000 Control Panels e With automated control you create a list of samples a sequence to be processed automatically The sequence includes programs with commands and parameters for controlling the ICS 1000 acquiring sample data and producing reports Section 3 11 2 describes automatic sample processing Doc 031879 01 3 03 2 11 ICS 1000 lon Chromatography System 2 3 4 The Chromeleon Main Window and Browser When you start Chromeleon the main window and the Chromeleon Browser appear see Figure 2 7 Chromeleon AMAR local Dionex Templates Browser File Edit View Workspace Qualification Batch Window Help D Ul ES mew m isinne AS i NNI htt hh O B EA me AMAR local Dionex Templates Browser AMAR ocal Nene ore DEMO IC Applications 2 4 2003 11 18 32 A 63 AAC CJ Panels 1 5 2003 3 05 51 PM i IC Applications Reports 2 4 2003 11 18 32 A Panels Reports Ca Ics 1000 AUDIT G manual Figure 2 7 Chromeleon Main Window and Browser NOTE The Chromeleon Browser loo
75. e leak sensor from triggering additional error messages 4 4 Doc 031879 01 3 03 4 Troubleshooting LOAD INJECT VALVE ERROR Ifthe injection valve fails to switch position within 1 second of being toggled the ICS 1000 Moduleware reports an error to Chromeleon and the Load Inject valve error message appears To troubleshoot 1 Ifa sequence is being executed terminate the sequence by selecting Stop on the Chromeleon Batch menu 2 Turn off the ICS 1000 power briefly and then restart 3 Try to toggle the valve from Load to Inject by clicking the Load and Inject buttons on the ICS 1000 Control Panel in Chromeleon 4 Ifthe 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 e Check the Chromeleon Server Configuration program to verify that the option is enabled PRESSURE SLOPE CALIBRATION ERROR This error occurs if you try to calibrate the pressure slope when the pressure is less than 3 MPa 500 psi To troubleshoot e This is a service level error message Contact Dionex for assistance Doc 031879 01 3 03 4 5 ICS 1000 lon Chromatography System PUMP MOTOR LOST CONTROL This error indicates an error in the pump controller electronics To troubleshoot e Contact Dionex for assistance The ICS 1000 electronics components cannot be serviced by the user PUMP
76. e of the seals To use this feature an external water source must be connected See Section B 21 for connection instructions For continued protection of the pump replace the piston rinse seals see Section 5 6 and O rings in the seal wash assembly every 6 months or whenever you replace the main piston seals for the ICS 1000 pump Doc 031879 01 3 03 2 23 ICS 1000 lon Chromatography System 2 4 4 Injection Valve The injection valve P N 057968 is a six port electrically activated valve A 25 uL sample loop P N 042857 is installed on the valve at the factory The valve has two operating positions Load and Inject see Figure 2 13 LOAD POSITION INJECT POSITION Sample In s Sample In To Column To Column Sample Sample Loop 5 si ae To Waste 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 e In the Load position sample is loaded into the sample loop where it is held until injection Eluent flows from the pump through the valve and to the column bypassing the sample loop Sample flows from the syringe or automated sampler line if installed through the valve and into the sample loop Excess sample flows out to waste e In the Inject position sample is swept to the column for analysis Eluent flows from the pump through
77. ection 5 10 SUPPRESSOR NOT CONNECTED This error appears if you turn on the suppressor and the ICS 1000 cannot establish a connection with the suppressor To troubleshoot 1 Check the suppressor cable connection see Section 5 10 2 Ifthe error persists contact Dionex for assistance There may be a problem in the suppressor controller electronics The ICS 1000 electronics components cannot be serviced by the user Doc 031879 01 3 03 4 Troubleshooting SUPPRESSOR STOPPED FOR ZERO FLOW RATE This error appears normally when you click the Shutdown button on the Chromeleon Control Panel The message also appears anytime you turn off the pump flow while the suppressor is on The suppressor is automatically turned off to prevent damage to the suppressor To troubleshoot e Ifthe pump stopped unexpectedly see Section 4 5 for pump troubleshooting information 4 2 Liquid Leaks e 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 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 e Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked Also if the blocked line
78. efer to Installing the Chromeleon IC System Document No 031883 to verify that the computer being used meets Chromeleon specifications The manual is on the Dionex Reference Library CD ROM P N 053891 Remove the central processing unit CPU keyboard mouse and all documentation from the computer box and place these items on a workbench Remove the monitor from its box and place it on the workbench Follow the instructions in the computer installation guide to hook up the monitor mouse keyboard and CPU If Chromeleon is not installed on the computer go on to Section B 3 Installing Chromeleon If Chromeleon is already installed on the computer go on to Section B 4 Installing the Chromeleon Software License B 4 Doc 031879 01 3 03 Installing Chromeleon B 3 Installing Chromeleon NOTES 10 Windows 2000 or Windows XP is required for controlling the ICS 1000 with Chromeleon Chromeleon version 6 5 SP2 or later is required To install Chromeleon you must log onto Windows 2000 or XP with administrator privileges Administrator privileges are not required to run Chromeleon Turn on the computer power Follow the Windows setup steps as they appear on the screen Verify that the monitor display is set to a minimum of 1024 x 768 with 16 bit color Insert the Chromeleon CD ROM into the CD ROM drive The Chromeleon Setup menu appears If the Setup menu does not appear automatically go to t
79. ell Tubing Chases The upper tubing chase routes tubing from the top cover to the component panel The lower tubing chase routes tubing from the component panel through the ICS 1000 interior to the rear panel Doc 031879 01 3 03 2 Features 2 1 4 Rear Panel Figure 2 5 illustrates the ICS 1000 rear panel Tubing Clips Analog Output Connector Power Switch USB Connections TTL and Relay Main Power Connector Strip Receptacle Waste Lines Figure 2 5 ICS 1000 Rear Panel Analog Output Connector The analog output connector outputs conductivity data scaled to 1 volt to an integrator or recording device See Section B 19 for connection and setup information USB Connections A USB receptacle is provided to allow connection to the Chromeleon computer Two USB ports are provided for connecting to other USB devices See Section B 5 for connection instructions Doc 031879 01 3 03 2 7 ICS 1000 lon Chromatography System CAUTION MISE EN GARDE VORSICHT 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 Tubing C
80. em operating parameters from the Chromeleon Control Panel Operating parameters can also be set automatically by loading a Chromeleon sequence NOTE Clicking the System Startup button on the Chromeleon Control Panel starts the pump and suppressor The flow rate and suppressor current settings that were in effect when the system was shut down are restored 1 Verify that the pump is on and set to the correct flow rate Verify that the suppressor current is on and that the setting is correct Verify that the cell heater is set to the correct value Bow ON Verify that the column heater is set to the correct value 3 10 Doc 031879 01 3 03 3 Operation and Maintenance 3 8 Equilibrate the System and Verify Operational Status 1 Allow the system to equilibrate During equilibration the Chromeleon Control Panel displays the background conductivity the conductivity of the eluent before sample injection and the system backpressure Monitor the background conductivity Refer to the column manual for the appropriate background conductivity for your application Offset the background and zero the reading by clicking the Autozero button on the Chromeleon Control Panel see Figure 3 4 Monitor the system pressure from the Control Panel to make sure it is at the expected pressure for the installed column refer to the column manual for details and it stable e Ifthe pressure is less than the expected amount gas may be t
81. ent or if the eluent lines are dry prime the lines first with a syringe before priming the pump See Section B 14 1 for instructions Verify that the priming valve on the primary pump head see Figure 3 8 is closed turned all the way clockwise 2 Open the waste valve on the secondary pump head by turning the knob one quarter to one half turn counterclockwise Opening the valve directs the eluent flow path to waste and eliminates backpressure Secondary Pump Head Waste Valve P 7 open v C Primary 7 Pump Head Priming Valve close Figure 3 8 Priming the Pump 3 Press Prime on the Chromeleon Control Panel A confirmation message is displayed asking if you opened the waste valve Select Yes The pump will begin pumping at approximately 3 0 mL min 4 Continue priming the ICS 1000 until all air and previous eluent are purged and no air bubbles are exiting the waste line Doc 031879 01 3 03 3 9 ICS 1000 lon Chromatography System 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 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 syst
82. eplace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent See the Pressurizable Reservoir Installation Instructions for more information about end line filters NOTE It is especially important to regularly replace end line filters when using aqueous eluents which may contaminate the filter with bacteria or algae The bacterial buildup may not be visible 4 12 Doc 031879 01 3 03 4 Troubleshooting Blockages in inlet tubing Kinked or clogged tubing causes the pump to be starved for eluent Replace the tubing and fittings see Section 5 3 Dirty check valve Clean or replace the pump check valve see Section 5 5 Liquid leaks at junction between pump head and pump casting Use the open end wrench P N 014605 provided in the ICS 1000 Ship Kit P N 057905 to tighten the two acorn nuts that attach the pump head to the pump housing see Figure 5 4 Tighten the nuts evenly 12 in lb torque If the leak persists replace the piston seal see Section 5 6 Liquid leaks from the seal wash port Replace the piston seal see Section 5 6 Scratched pump piston Check the pump pistons for scratches and replace if necessary see Section 5 7 4 4 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 16 No communication between ICS 1000 and Chromeleon
83. er Optional B 40 B 17 1 AS50 Configuration Requirements B 40 B 17 2 AS50 Connections B 41 B 17 3 Enable AS50 Control of the Injection Valve B 43 Connecting an AS40 Automated Sampler Optional B 44 Analog Output Connection Optional B 46 Pressurizing the Eluent Reservoir Optional B 46 vi Doc 031879 01 3 03 Contents B 21 B 22 B 23 B 20 1 Connecting the Gas Source Optional B 47 B 20 2 Pressurizing the Eluent Reservoir Optional B 48 Pump Continuous Seal Wash Connections Optional B 49 Manually Connecting to a Control Panel B 51 Installation Troubleshooting B 53 C TTL and Relay Control C 1 C 2 C 3 TTL and Relay Connections C 1 C 1 1 Selecting TTL Input Functions and Control Types C 3 Controlling TTL and Relay Outputs C 5 Example Setup for Stand Alone Operation C 7 D Reordering Information E FAQ E 1 How do I hook up an autosampler E 1 E 2 How do T print eos ALAN e REA bun RH een ed hse E 1 E 3 Why are the retention times moving E 1 E 4 How do I adjust retention times E 1 E 5 When should I re
84. er the conductivity the more pronounced the effect In ion analysis the effect of temperature variation is minimized by suppressing eluent conductivity To further reduce the effect of temperature variation the ICS 1000 provides temperature control to the cell A heater inside the cell regulates the temperature The cell heater can be set to between 30 C and 55 C The set temperature must be at least 7 C above the ambient temperature Setting the cell temperature to 0 C turns off the cell heater Temperature Compensation Built in preset temperature compensation of 1 7 per C helps minimize changes in the baseline or in peak heights if the operating temperature is different from the temperature at which the cell was calibrated Doc 031879 01 3 03 2 27 ICS 1000 lon Chromatography System 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 9 for cell replacement instructions 2 28 Doc 031879 01 3 03 3 Operation and Maintenance This chapter describes routine operating and maintenance procedures for the ICS 1000 Ion Chromatography System 3 1 Operation Overview Figure 3 1 illustrates the basi
85. etention Time or Selectivity Contaminated or incorrect eluent Remake the eluent using concentrated eluent and ASTM filtered Type I 18 megohm deionized water 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 Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 2 Ifcleaning is unsuccessful replace the column Doc 031879 01 3 03 4 17 ICS 1000 lon Chromatography System 4 11 No Cell Response Cell not properly installed Verify that the cell front cover is flush against the component panel If necessary tighten the two mounting screws When the cell is correctly installed and the screws tightened an electronics connector on the cell plugs into a receptacle inside the ICS 1000 No flow from pump This condition has several possible causes See Section 4 4 and Section 4 5 for details Cell electronics malfunctioning Use the Chromeleon Wellness Panel diagnostics to test the electronics see Section 5 1 and the Chromeleon online Help for instructions If the variance reading is outside the tolerance range less than 1 LS the electronics are malfunctioning Contact Dionex for assistance The ICS 1000 electronics cannot be serviced by the user 4 12 Hig
86. from the Batch menu The Batch dialog box opens see Figure 3 10 Batch ics 1000 Figure 3 10 Batch Dialog Box 4 Click the Add button on the Batch List tab and add the sequence you created in Step 2 See Figure 3 11 for an example Batch ics 1000 amarquardt Figure 3 11 Batch Dialog Box with an Example Sequence Added to the Batch List 5 To start the batch click Start 3 20 Doc 031879 01 3 03 3 Operation and Maintenance 3 12 Maintenance This section describes routine maintenance procedures that users may perform All other maintenance procedures must be performed by Dionex personnel As Needed e Regularly check the eluent reservoir to see if it needs to be refilled e Make fresh eluent as needed Daily e Check the ICS 1000 component mounting panel see Figure 2 4 for leaks or spills Wipe up spills Isolate and repair leaks see Section 4 2 Rinse off any dried eluent with deionized water e Check the waste container daily and empty when needed Weekly e Once a week check fluid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines e Check the junctions between the pump heads and the pump casting for evidence of liquid leaks If piston seal wash tubing is not connected check the drain tubes at the rear of the pump heads for evidence of moisture Normal friction and wear may gradually result in small liquid leaks around the p
87. front cover The screws remain attached see Figure 5 9 View B B eS Unscrew DS6 HEATED CONDUCTIVITY CELL SERIAL NO 1 CELL CONSTANT 1 CELL IN SERIALNO 02090682 CELL CONSTANT L 143 68 Unscrew Figure 5 9 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 Do not pull from the CELL IN and CELL OUT fittings 4 Continue pulling on the cover until the attached cell assembly slides out the front of the ICS 1000 see Figure 5 10 Figure 5 10 Removing the Cell Assembly 5 20 Doc 031879 01 3 03 5 Service 5 Slide the new cell assembly 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 1000 when you push the assembly into the opening po c CEN Tighten the screws on the cell front cover fingertight Reconnect the inlet and outlet lines Turn on the ICS 1000 power Calibrate the new cell in Chromeleon Cell calibration of a new cell consists of three parts S p G Run the offset calibration which measures the output of the cell electronics alone and determines an offset value to be applied to raw conductivity readings Run the slope calibration which measures the output of the cell electronics when a built in dummy cell wh
88. ges Refer to the Installation and Troubleshooting Guide for OnGuard Cartridges Document No 032943 for instructions 3 12 Doc 031879 01 3 03 3 Operation and Maintenance 3 9 3 Diluting Samples Because the concentrations of ionic species in different samples can vary widely from sample to sample no single dilution factor can be recommended for all samples of one type In some cases for example many water samples concentrations are so low that dilution is not necessary Use eluent or ASTM filtered Type I 18 megohm deionized water or eluent to dilute the sample When using carbonate eluents diluting with eluent minimizes the effect of the water dip at the beginning of the chromatogram If you dilute the sample with eluent also use eluent from the same lot to prepare the calibration standards This is most important for fluoride and chloride which elute near the water dip To improve the accuracy of early eluting peak determinations such as fluoride at concentrations below 50 ppb dilute standards in eluent or spike the samples with concentrated eluent to minimize the water dip For example spike a 100 mL sample with 1 0 mL of a 100 X eluent concentrate Doc 031879 01 3 03 ICS 1000 lon Chromatography System 3 10 Loading and Injecting Samples Samples can be loaded into the sample loop through the injection port on the front door using a syringe or vacuum syringe or they can be loaded using an auto
89. h they have a lifetime of only one week When should remake eluents Eluents should be remade every two or three weeks How do start Chromeleon Click Start on the Windows taskbar and then select Programs gt Chromeleon gt Chromeleon How do I delete data In the Chromeleon Browser highlight the sequence you want to delete and then select File gt Delete How do I back up data In Chromeleon select File gt Export Backup Back up the data and indicate the backup source How do I shut off the system In Chromeleon click the System Shutdown button on the ICS 1000 Control Panel see Figure 2 8 On the ICS 1000 turn off the power switch on the rear panel see Figure 2 5 How do I store columns Columns should be stored in eluent See the column manual for complete instructions The column manual is included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 E 2 Doc 031879 01 3 03 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 e The suppressor needs regeneration See the suppressor manual for troubleshooting information The suppressor manual is included on the Dionex Reference Library CD ROM P N 053891 located
90. h Cell Output Background not suppressed by suppressor Verify that the suppressor is turned on and the current is set to the correct value Refer to the suppressor manual for additional troubleshooting guidance Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 Sample concentration too high Dilute the sample Section 3 9 3 Wrong eluent Check that you are using the correct eluent for your application Background conductivity not offset from conductivity reading Before making an injection allow the background conductivity to equilibrate and then press Autozero on the Chromeleon Control Panel 4 18 Doc 031879 01 3 03 4 Troubleshooting 4 13 Cell out of calibration Recalibrate the cell see Section 5 1 2 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 on the Dionex Reference Library CD ROM P N 053891 Trapped gases Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them Also loosen and retighten the fittings to and from the suppressor eluent ports Pump not properly primed Prime the pump see Section B 12 Contaminated or incorrect e
91. h a Thermal Compartment TC or Chromatography Compartment CC and you are now going to use it with an ICS 1000 the injection valve is typically installed in the TC or CC not in the ASSO If this is the case verify that the correct Moduleware version is installed and enable control of the ICS 1000 injection valve see Section B 17 3 After the AS50 is configured for use with the ICS 1000 all ASSO modes of injection full loop partial loop and partial loop limited sample are supported In addition all AS50 injection valve commands whether B 40 Doc 031879 01 3 03 Connecting an AS50 Autosampler Optional issued from the ASSO front panel or from Chromeleon will control the ICS 1000 injection valve For Chromeleon control the AS50 must be added to the ICS 1000 timebase see Section B 8 For front panel control the AS50 and ICS 1000 can be set up for stand alone operation This requires a TTL cable connection between the AS50 and the ICS 1000 See Section C 3 for stand alone setup instructions B 17 2 AS50 Connections 1 Place the AS50 to the left of the ICS 1000 on the workbench 2 Open the ICS 1000 and AS50 doors 3 The needle seal line that extends from the inject port in the autosampler is coiled inside the AS50 door on the right side Route this line through the AS50 right side slot see Figure B 38 and the ICS 1000 left side slot to the ICS 1000 injection valve The needle seal line from the AS50 inject p
92. hanneling The preferential flow of liquid along more open less resistant paths through the column packing This causes Band Spreading Column Efficiency N A measure of the narrowness of analyte bands as they elute from the column High efficiency is desirable because resolution between closely spaced bands improves with greater efficiency For a symmetrical Gaussian peak column efficiency can be determined by the following N 5 54 t W 5 Where t the peak retention time in seconds Win the peak width at 1 2 height in seconds Column efficiency is proportional to column length for a given resin and column diameter increasing the column length increases the column efficiency Synonymous with Theoretical Plates Column Selectivity a Describes the relative separation of the band maxima between two adjacent peaks Selectivity can be determined by the following a ty to ty to Where t and t retention time of components 1 and 2 respectively tg retention time of unretained components void volume Concentrator Column A short column used to retain and concentrate analytes from a measured volume F 2 Doc 031879 01 3 03 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 Condu
93. he Autorun folder on the Chromeleon CD ROM and double click autorun exe Select Launch Chromeleon Setup Setup now guides you through the installation procedure follow the on screen instructions as they appear When prompted select whether to add the Chromeleon Server Monitor to the Startup group If you select yes the Server Monitor starts automatically when the computer is started and the program icon appears in the taskbar When complete go on to Section B 4 Installing the Chromeleon Software License Doc 031879 01 3 03 B 5 ICS 1000 lon Chromatography System B 4 IMPORTANT Installing DX LAN Devices If you will also be installing a module that requires a DX LAN interface connection verify that the following steps are completed before continuing If it is not already installed install the DX LAN card in the module Refer to the operator s manual for the module for installation instructions Install the DX LAN card in the computer Connect the module to the DX LAN Install the DX LAN card driver Instructions for Steps 2 through 4 are in Installing the Chromeleon IC System Document No 031883 Installing the Chromeleon Software License For the Chromeleon computer to control the ICS 1000 a valid software license must be installed To install the license you first install a dongle on the computer and then enter a license Key Code in Chromeleon A dongle is an adapter that is connec
94. he outlet line from the AS40 to port S 5 of the injection valve see Figure B 42 Figure B 42 ICS 1000 Injection Valve Locate the relay control cable P N 047946 supplied with the AS40 Remove the 2 position connector plug from the pair of wires labeled LOAD on the relay control cable Locate the 12 position connector plug P N 923686 in the ICS 1000 Ship Kit P N 057905 see Position 1 Figure B 43 Locking Screws Attach the red wire from the relay control cable to position 1 Position 12 on the plug and attach the green wire to position 2 This will be used to connect the AS40 LOAD Figure B 43 12 Position Connector Plug relay to RELAY OUT 1 on the ICS 1000 To attach a wire to the plug strip the end of the wire insert it into the plug and use a screwdriver to tighten the locking screw When attaching wires to the connector plug be careful not to allow stray strands of wire to short to the adjoining position on the connector B 44 Doc 031879 01 3 03 Connecting an AS40 Automated Sampler Optional NOTE If RELAY OUT 1 is not available you can connect to RELAY OUT 2 or to one of the TTL outputs For RELAY OUT 2 connect the red wire to position 3 and the green wire to position 4 For TTL OUT 1 connect the red wire to position 5 and the green wire to position 11 For TTL OUT 2 connect the red wire to position 6 and the green wire to position 12 8 Connect the relay
95. ich provides a constant conductivity reading of 21 uS is automatically enabled The slope value is applied to raw conductivity readings Enter the cell constant measured at the factory The ICS 1000 uses the cell constant to determine the measured conductivity Open the Wellness Panel see Section 5 1 1 Under Electric Conductivity Cell Calibration click Offset Cal When the offset calibration is complete click Slope Cal Click Calibration Details Under Conductivity Cell Cal Details enter the Cell Constant value printed on the front of the cell In the field next to the Download button verify that Current is selected and then click Download to download the new value to the ICS 1000 To ensure the new values are recorded in the ICS 1000 memory do not turn off the ICS 1000 power for at least 1 minute after downloading Doc 031879 01 3 03 5 21 ICS 1000 lon Chromatography System 5 10 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 located in the ICS 1000 Ship Kit P N 057905 1 Gee 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 Turn off the pump from the ICS 1000 Control Panel in Chromeleon Open the front door of the ICS 1000 Disconnect
96. icking a control often brings up another window in which you enter a value When you open a System Control Panel select a panel that matches your system configuration and choose the style that you prefer Doc 031879 01 3 03 2 13 ICS 1000 lon Chromatography System Km ICS 1000 Pump and Detector IC LELx Sample Audit Trail Datasource Elapsed Time 09 52 41 Manually acquired samples will be stored temporarily in sequence SEQ AAMAR local C S 2000Wm anual Sequence Run Time 09 52 42 Chromeleon server version 6 50 SP2 Build 957 Alpha started serial number 853 8 52 46 User AMar from AMAR has connected Server Configuration to this Sample System server mene Startup Shutdown ICS 1000 Pump ICS 1000 Detector Eluent Bottle 7 Connected Connected gnnected DEME 0 09962 ps Supp Typ 0 00 I 2 Hold Mode 190 15 i us Stop Mode 0 100 ee n 327 6 0 1 00 ml min Off On Prime 40 4 Inject Valve LoadPosition 2404 Inject Load Eluent Flow Valve ss si Closed Open PEST T T T T T T T T T 1 Chsed Omen 0 00 0 50 1 00 1 50 2 00 2 50 3 00 3 50 4 00 4 50 5 00 Figure 2 8 ICS 1000 System Control Panel Traditional ICS 1000 System 1000 AMAR _ ol x Sample System Log Audit Trail on ICS 1000 Pump On Datasource 909 52 41 Manually acquired samples will be stored tempora
97. iently degassed If the ICS 1000 does not contain a vacuum degas assembly degas the eluent manually see Section 3 4 2 If the ICS 1000 contains a vacuum degas assembly check the degas settings 1 Open the Chromeleon Server Configuration program select the ICS 1000 device icon under the timebase and select Properties from the Edit menu or double click the ICS 1000 device icon 2 Select the Options tab see Figure 4 1 Doc 031879 01 3 03 4 11 ICS 1000 lon Chromatography System Dionex ICS 1000 System Ea Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General Options Signals Head Type amp Limits Solvents State Devices r Installed Options M Degas M Column Heater r Degas Mode C Always Off C Always On Cycle On F 0 120 sec Off p 0 5940 sec Figure 4 1 ICS 1000 Server Configuration Properties Options 3 Verify that the Degas check box is enabled under Installed Options 4 Check the Degas Mode 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 10 minutes 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 If the system is in continuous operation change the end line filter weekly or whenever it becomes discolored R
98. ile the system is equilibrating Collecting and Storing Samples Collect samples in high density polyethylene containers that have been thoroughly cleaned with deionized DI water Do not clean containers with strong acids or detergents because these can leave traces of ions on the container walls The ions may interfere with the analysis If samples will not be analyzed on the day they are collected filter them through clean 0 45 um filters immediately after collection otherwise bacteria in the samples may cause the ionic concentrations to change over time Refrigerating the samples at 4 C 39 F will reduce but not eliminate bacterial growth Analyze samples containing nitrite or sulfite as soon as possible Nitrite oxidizes to nitrate and sulfite to sulfate thus increasing the measured concentrations of these ions in the sample In general samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant changes in anion concentrations Pretreating Samples Analyze rainwater drinking water and air particulate leach solutions directly with no sample preparation other than filtering and possibly diluting Filter groundwater and wastewater samples through 0 45 um filters before injection unless samples were filtered after collection Before injection pretreat samples that may contain high concentrations of interfering substances by putting them through Dionex OnGuard cartrid
99. in fittings P N 052267 and ferrules P N 048949 are used for connections to the suppressor REGEN OUT port and the eluent reservoir Doc 031879 01 3 03 ICS 1000 lon Chromatography System 5 4 Rebuilding the Injection Valve Dionex recommends rebuilding the injection valve annually The Injection Valve Rebuild Kit P N 057896 contains all required replacement parts NOTE Substitution of non Dionex parts may impair valve performance and void the product warranty 1 Turn off the pump from the ICS 1000 Control Panel in Chromeleon 2 Open the ICS 1000 front door 3 Disconnect each liquid line connected to the injection valve 4 Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 5 Reconnect all liquid lines to the injection valve see Figure 5 3 6 Close the door 7 Turn on the pump SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP Orange TO INJ VALVE c Black TO INJECT Green VALVE P Figure 5 3 Injection Valve Plumbing 5 10 Doc 031879 01 3 03 5 Service 5 5 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 cleani
100. ing Suppressor are registered trademarks of Dionex Corporation Teflon is a registered trademark of E I duPont de Nemours amp Co Windows is a registered trademark of Microsoft Corporation PRINTING HISTORY Revision 01 March 2003 Contents 1 Introduction 1 1 1 2 1 3 Introduction to Ion Chromatography IC 1 1 Overview of the ICS 1000 1 4 About This Manual 1 5 1 3 1 Safety Messages and Notes 1 6 1 32 Safety Labels zc esce Sac one rte A nn eic 1 8 2 Features 2 1 2 2 2 3 2 4 Operating Features 2 1 2 14 BrontPanel nioena AISNE Le EN edd RACER A ooh den 2 1 2 122 TOP COVER ses oe vetet ge py ots d ay tme vau ces 2 3 2 1 3 Component Panel 2 4 2 14 Rear Panels vehe ete le tnt I ER 2 7 Flow Schematie rieri oan SAGAS ERE ER EE E UE ex 2 9 The Chromeleon Interface 2 11 2 3 1 The Chromeleon Main Window and Browser 2 12 2 3 2 The ICS 1000 Control Panels 2 13 System Component Details 2 19 24 1 Vacuum Degas Assembly Optional 2 19 24 2 Elet Valve s sus eee Ene y bp riore ers 2 21 2 43 P UMP it ha eto ie tee Sie ere CE ane alt ea nan D 2 21 Doc 031879 01 3 03 ICS 1000 lon Chroma
101. into the 12 pin connector on the ICS 1000 rear panel C 2 Doc 031879 01 3 03 C TTL and Relay Control c Connect the wires from the ICS 1000 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 Ifyou connected a TTL input verify that the correct function is assigned to the input and that the correct input control type is selected Select different settings 1f necessary Input functions and control types are assigned from Chromeleon see Section C 1 1 C 1 4 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 ICS 1000 icon under the timebase Select the TTL Inputs tab see Figure C 3 Dionex ICS 1000 System x General Options Signals Head Type amp Limits Solvents State Devices Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics TTL Input Mode Normal edge TTL Input Functions TTL Input 1 Load iniect ave x TTL Input 2 aue x TTL Input 3 Pump Suppressor ON OFF 1x TTL Input 4 Recorder mark H Cancel Apply Help Figure C 3 ICS 1000 Server Configuration Properties TTL Inputs Doc 031879 01 3 03 C 3
102. is a waste line make sure it is not elevated at any point after it exits the ICS 1000 If a line is blocked replace it see Section 5 3 Loose pump check valve Make sure the check valves are firmly seated in the pump head If they are not tighten them carefully with an open end wrench just until the leak stops If the leak persists replace the check valve see Section 5 5 e Leaking seal wash port Leaking from the seal wash port indicates a leaking piston seal Replace the seal see Section 5 6 Doc 031879 01 3 03 4 9 ICS 1000 lon Chromatography System Damaged pump piston seal 1 Replace the piston seal see Section 5 6 2 Ifthe leak persists replace the piston see Section 5 7 Pump head not tight against casting Carefully tighten the pump head mounting nuts just until the leak stops DO NOT OVERTIGHTEN Leaking pressure transducer Make sure the liquid line connections into the pressure transducer are tight Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is on the Dionex Reference Library CD ROM P N 053891 Replace any damaged fittings The pressure transducer cannot be serviced by the user Contact Dionex for assistance Leaking pump head waste valve Make sure the waste valve is closed To close the valve turn the knob clockwise and tighten fingertight DO NOT OVERTIGHTEN Overtightening may damage the valve and the pump head
103. iston 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 6 e Check the end line filter P N 045987 and change if needed When new end line filters are pure white If the system is in continuous operation change the end line filter weekly or whenever it becomes discolored Replace the filter more often if bacterial buildup is visible or if the eluent does not contain solvent NOTE It is especially important to regularly replace end line filters when using aqueous eluents which may contaminate the filter with bacteria or algae The bacterial buildup may not be visible Doc 031879 01 3 03 3 21 ICS 1000 lon Chromatography System Every Six Months Calibrate the cell see Section 5 1 2 Calibrate the vacuum degas assembly see Section 5 1 4 e Replace the pump piston rinse seals and piston seals see Section 5 6 Yearly e Rebuild the injection valve see Section 5 4 e Replace the AS40 Automated Sampler tip and tubing The AS40 ASM 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 e Perform the ASSO preventive maintenance procedure The AS50 Maintenance Kit P N 060581 contains all ofthe required components and instructions for performing the procedure
104. ject Perform an autozero command set the conductivity to zero Turn the pump on and off also turns the suppressor on and off Send a chart mark signal to the analog output The mark is 10 of the full scale voltage and the duration is 0 5 seconds A mark can be used for example to indicate the injection Relay outputs 1 and 2 can be programmed to switch any low voltage control Switched current must be less than 200 mA and 42 V peak Connecting a TTL or Relay 1 CAUTION Locate the twisted pair of wires P N 043598 and the 12 position connector plug Position 1 P N 923687 see Figure C 2 in the ICS 1000 Ship Kit P N 057905 Follow these basic steps to connect the TTL or relays a b Locking Screws Position 12 For each relay or TTL to Figure C 2 12 Position Connector Plug be used connect an active wire red and a ground wire black to the 12 position connector plug at the appropriate pin locations Refer to Figure C 1 or the label on the ICS 1000 rear panel for the connector pin assignments To attach a wire to the plug strip the end of the wire insert it into the plug and use a screwdriver to tighten the locking screw If necessary multiple ground wires can be attached to a single TTL input output ground pin When attaching wires to the connector plug be careful not to allow stray strands of wire to short to the adjoining position on the connector Plug the connector
105. ks and functions like Windows Explorer but do not confuse the two If you copy files from the Chromeleon Browser into Explorer the files will be corrupted The Browser displays the directories in which chromatographic data is located and allows you to open move and delete data e The left pane of the Browser shows the directory tree structure By clicking the signs next to the folders and expanding the directory tree you can access sequences System Control Panels Wellness Panels and reports e The right pane displays information about the item selected in the left pane 2 12 Doc 031879 01 3 03 2 Features 2 3 2 The ICS 1000 Control Panels Chromeleon provides two types of Control Panels for the ICS 1000 e System Control Panels are used for controlling and monitoring ICS 1000 operation System Control Panels are described below e The Wellness Panel is used for performing calibration and diagnostic functions The Wellness Panel is described in Section 5 1 System Control Panels System Control Panels for the ICS 1000 are located in the Dionex Templates Panels Dionex_IC ICS 1000 folder Chromeleon provides panels for each ICS 1000 system configuration There are two styles of panels Traditional system panels see Figure 2 8 provide controls on a single window with minimal graphics e System panels see Figure 2 9 provide a more graphical interface than the traditional style On these panels cl
106. lacing the Leak Sensor 5 28 5 15 Priming with Isopropyl Alcohol 5 29 5 16 Changing Main Power Fuses 5 30 iv Doc 031879 01 3 03 Contents A Specifications A l A 2 A 3 A4 A 5 A 6 A 7 A 8 A 9 A 10 Electrical 25 uuu Re de Det A 1 Physical 352 diode Dt tei ode ea dads A 1 Environmental spna aiaa a a a a A lh A 1 Front Panel reia eenia aan a e a Peeper segs Byte ET A 2 Pump m aitete osa aa iius en a e a A 2 DetectoE Ske p he aa d uis ee CAM i A 3 Conductivity Cell with Heat Exchanger A 3 Injection Valve porse sapete Dorem p eme Pase e bine ere A 3 Vacuum Degas Assembly Optional A 3 Column Heater Optional A 4 B Installation B 1 B 2 B 3 B 4 B 5 B 6 B 7 Facility Requirements B 1 Unpacking the ICS 1000 System B 2 B 2 1 Unpacking the Computer North America only B 4 B 2 2 Unpacking the Computer outside North America B 4 Installing Chromeleon B 5 Installing the Chromeleon Software License B 6 Connecting the ICS 1000 to the Chromeleon PC B 9 B 5 1 Connecting the ICS 1000 to the PC B 9 B 5 2 Connecting Additional USB Devices B 10
107. leon is communicating with the ICS 1000 by clicking the Inject and then the Load button on the Control Panel If communication is occurring you will hear the valve actuate as it changes position Go on to Section B 13 B 13 Setting the Eluent Level After filling the reservoir enter the volume of liquid in the reservoir on the Chromeleon Control Panel see Figure B 34 The ICS 1000 determines the eluent usage by monitoring the flow rate and the length of time the pump is on and updates the Eluent Level field as the eluent is used up A warning appears if the level falls below 200 mL Warnings are repeated at 100 mL and 0 mL In order for the eluent level displayed on the Control Panel to be accurate the level must be entered by the user when the reservoir is filled The ICS 1000 does not automatically detect when the reservoir is filled nor when it is empty ICS 1000 Pump rEluent Bottle Enter the volume of liquid in the reservoir Note The Eluent Bottle field and slider gauge are updated as the liquid is used up Figure B 34 Setting the Eluent Level Doc 031879 01 3 03 B 35 ICS 1000 lon Chromatography System B 14 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 ICS 1000 to the reservoir cap is connected see Section B 11 2 Verify that the waste lines are directed to a waste container
108. libration is complete click Slope Cal on the Wellness Panel 4 Disconnect the pump output line from the injection valve 5 Disconnect the line from the suppressor ELUENT OUT port to the cell inlet and connect the pump output line directly to the cell inlet 6 Verify that there is a minimum of 7 MPa 1000 psi of backpressure 7 On the Wellness Panel under Conductivity Cell Calibration click Cell 35 C Allow the cell to reach this temperature and then wait an additional 5 minutes to let it stabilize 8 Select 1 00 mL min to begin pumping 1 0 mM KCl through the cell at 1 0 mL min 9 Wait until the total conductivity reading stabilizes in about 15 minutes and then select Calibrate on the Wellness Panel Doc 031879 01 3 03 5 Service After calibration the conductivity reading should be 147 00 2 uS and the cell constant should be between 120 and 180 If this is not the case contact Dionex for help Click Log to record the new calibration values in the Audit Trail Flush the KCI solution from the system by pumping deionized water through the cell When the conductivity drops to less than 1 uS cm stop the pump Reconnect the pump to the injection valve and reconnect the line from the suppressor to the cell inlet Doc 031879 01 3 03 5 5 ICS 1000 lon Chromatography System 5 1 3 Calibrating the Flow Rate When to Calibrate If you run the ICS 1000 Operational Qualification or Performance
109. lips The tubing clips hold tubing in place when routing it from the top cover Power Switch The power switch provides on off control of power to the ICS 1000 Main Power Receptacle The power supply cord plugs into the AC power receptacle The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the ICS 1000 and is easily accessible Le cordon d alimentation principal est utilis comme dispositif principal de d branchement Veillez ce que la prise de base soit situ e install e pr s du module et facilement accessible Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist 2 8 Doc 031879 01 3 03 2 Features 2 2 Flow Schematic Figure 2 6 illustrates the liquid flow path through an ICS 1000 when using suppression in autorecycle mode o WASTE ELUENT OUT OUT E e a PUMP 9 0 DEGAS a Optional IN DE T COND amp 53lz 5 CELL OUT T x8 e m lt Q rm ul Lui o a PULSE 2d S X DAMPER tor JET EI N o O X 9 o S L OUT o wO c o L RP PRESS 19 XDUCER g VALVE 9 LL w l J 2 aii R i PUMP PUMP HEAD HEAD M P WASTE n IN OUT Figure 2 6 ICS 1000 Flow Schematic Doc 031879 01 3 03 2 9 ICS 1000 lon Chromatograph
110. luent Remake the eluent using concentrated eluent and ASTM filtered Type I 18 megohm deionized water Rapid changes in ambient temperature Make sure the ambient temperature is between 4 and 40 C 40 and 104 F Make sure air conditioning and heating vents are directed away from the ICS 1000 and the ICS 1000 front door is closed Insufficient system equilibration following changes to operating parameters especially apparent when operating at high sensitivities Allow a longer system equilibration time up to 2 hours before starting operation Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 Doc 031879 01 3 03 4 19 ICS 1000 lon Chromatography System e Cell above or below temperature Contact Dionex for assistance e Damaged piston seal Replace the piston seal see Section 5 6 4 14 Vacuum Degas Assembly Does Not Run e Degas option not enabled in Chromeleon a Open the Chromeleon Server Configuration program Select the ICS 1000 device icon under the timebase and select Properties from the Edit menu or double click the ICS 1000 device icon Select the Options tab see Figure 4 3 Dionex ICS 1000 System Sonar nee ne Sorbo Figure 4 3 ICS 1000 Server Configuration Properties Options 4 20
111. make standards E 2 E 6 When should I remake eluents E 2 E 7 How do I start Chromeleon E 2 E 8 How do I delete data E 2 E 9 How do I back up data E 2 Doc 031879 01 3 03 vii ICS 1000 lon Chromatography System E 10 How do I shut off the system E11 How do I store columns E 12 How do I know when a column is dirty E 13 Howdolcleanacolumn E 14 Why is the conductivity high F Glossary m E 2 M E 2 b edit Hp n EE E 3 VAR eae tede ODE VEO leases s E 3 viii Doc 031879 01 3 03 1 Introduction 1 1 Introduction to lon Chromatography IC The Dionex ICS 1000 Ion Chromatography System ICS 1000 performs ion analyses using suppressed or non suppressed conductivity detection An ion chromatography system typically consists of a liquid eluent a high pressure pump a sample injector a guard and separator column a chemical suppressor a conductivity cell and a data collection system Before running a sample the ion chromatography system is calibrated using a standard solution By comparing the data obtained from a sample to that obtained from the known standard sample ions can be identified and quantitated The data collection system typically a computer running chromatograph
112. me ICS 1000 System Total Program Time Connected Startup Shutdown Show Plot Load Inject 10 0 from Pos Injector Settings CS 1000 DR CE x 0 108 uS Suppressor Off st O oma Detector Settings 0 00 0 50 1 50 2 00 Figure 3 6 ICS 1000 System Control Panel Connected NOTE The ICS 1000 Ion Chromatography System is designed for use for IC ion chromatography and BioLC applications and should not be used for any other purpose If there is a question regarding appropriate usage contact Dionex 3 4 SetUp the Eluent Reservoir 3 4 1 3 4 2 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 Degas the Eluent Eluent quality significantly affects the performance of the ICS 1000 To ensure optimal pump performance observe the following precautions 3 6 Doc 031879 01 3 03 3 Operation and Maintenance e Dionex strongly recommends vacuum degassing all eluents This helps prevent bubbles caused by outgassing from forming in the pump heads and the detector flow cell e The optional vacuum degas assembly provides programmable online degassing The degas assembly must be installed in the ICS 1000 at the factory If the ICS 1000 does not contain a degas assembly manually degas eluents daily following the instructions below and store it in pressurized
113. n AMAR _local Dionex Templates Browser File Edit View Workspace Qualification Batch Window Help DSUH ES BEN LOS e a nr AS DEBS OIM Rody oer ho e Bgm dE AMAR _local Dionex Templates Browser AMAR local DEMO IC Applications 2 4 2003 11 18 32 A En fDionex Templates CA Panels 1 6 2003 3 05 51 PM C IC Applications E Reports 2 4 2003 11 18 32 A CA Panels E Reports ICS 1000 H E AUDIT fil manual Figure 3 4 Chromeleon Main Window and Browser Doc 031879 01 3 03 3 Operation and Maintenance ER System In the Browser expand the Dionex Templates Panels Dionex ICUCS 1000 System Panels folder Several ICS 1000 System Control Panels PAN files are provided corresponding to various system configurations There are two styles of panels Traditional panels provide controls on a single window with minimal graphics e System panels provide a more graphical interface than the traditional style and include more controls You can choose either style of panel depending on your personal preference Open a panel for your system configuration by double clicking its name in the list For example if your system includes an ICS 1000 and an AS50 autosampler double click either ICS 1000 Traditional System AS50 pan or ICS 1000 System ASS0 pan The Control Panel opens unconnected see Figure 3 5 To connect to the timebase open the
114. n the Chromeleon Control Panel Write down the short term pressure fluctuations they should be less than 0 13 MPa 20 psi ICS 1000 installation is complete For routine operation refer to Chapter 3 Doc 031879 01 3 03 B 39 ICS 1000 lon Chromatography System B 17 Connecting an AS50 Autosampler Optional B 17 1 AS50 Configuration Requirements To use an AS50 autosampler with the ICS 1000 the AS50 must meet the following requirements e An injection valve cannot be installed in the AS50 e The AS50 must have Moduleware version 1 11 or later installed e Control of the ICS 1000 injection valve must be enabled in the AS50 The following AS50 models are configured at the factory to meet the above requirements e AS50 without injection valve P N 061309 e AS50 without injection valve with sample preparation P N 061310 e AS50 without injection valve with sample preparation and sample tray cooling P N 061311 e AS50 without injection valve with sample tray cooling P N 061312 Notes e To identify the version of Moduleware currently installed in the ASSO go to the ASSO POWER UP screen press Menu 8 and 1 If a Moduleware update is required contact Dionex e In order to use an AS50 that has an injection valve installed the valve must be disconnected from the AS50 electronics Contact Dionex for assistance The AS50 electronics components cannot be serviced by the user e Ifthe ASSO is currently running wit
115. nd the AS50 drip tray NOTE For PEEK waste lines sharply bend the waste line tubing about 5 mm from the end to ensure it stays in place in the opening in the drip tray When bending the tubing be sure not to restrict the inner diameter 7 Ifyou have not already done so add the AS50 to the Chromeleon timebase see Section B 8 B 42 Doc 031879 01 3 03 Connecting an AS50 Autosampler Optional B 17 3 Enable AS50 Control of the Injection Valve Follow the steps below if you are connecting an AS50 that was not configured at the factory for ICS 1000 support Injection valve control is already enabled in pre configured AS50 models see the list in Section B 17 1 1 On the ASSO front panel press Menu and 0 to go to the TIME FUNCTION OUT screen see Figure B 41 In the LOAD INECT VALVE TTL 1 field select ENABLED ENABLED DISABLED Figure B 41 AS50 Time Function Out Screen 2 Turn the AS50 power off and then back on All AS50 injection valve commands whether issued from the AS50 front panel or from Chromeleon will now control the ICS 1000 injection valve Doc 031879 01 3 03 B 43 ICS 1000 lon Chromatography System B 18 Connecting an AS40 Automated Sampler Optional 1 CAUTION Place the AS40 to the left of the ICS 1000 on the workbench Open the front door of the ICS 1000 and thread the outlet line from the AS40 through the left side slot at the front of the ICS 1000 Connect t
116. ne Container Figure B 48 Piston Seal Wash Flow Schematic B 50 Doc 031879 01 3 03 Manually Connecting to a Control Panel B 22 Manually Connecting to a Control Panel This section describes how to manually connect the ICS 1000 to a Control Panel if you do not use the application templates described in Section B 12 1 Inthe Browser expand the Dionex Templates Panels Dionex_IC ICS 1000 folder Several System Control Panels corresponding to various system configurations are provided 2 Open the panel for your system configuration by double clicking its name in the list For example if your system includes an ICS 1000 and an AS50 autosampler double click either ICS 1000_System_AS50 pan or ICS 1000 Traditional System ASS0 pan NOTE The two types of panels system and traditional system are similar in function but have different looks You can select either style depending on your personal preference When the Control Panel opens the controls on the panel are not enabled see Figure B 49 EX Pump and Detector Sampl j Audit Trai Datasource 1 Elapsed Time Istem Retentic PE Sequence 1 Run Time ystem PgmEn Sample 1 System 1 Program 1 Startup Shutdown m Pump_ECD DeviceType Pump Pump ECD DeviceType Dete cto r j T Connected T Connected Connected Signal A Signal Valui Sup
117. ng Replacing Check Valves 1 Close the eluent valve from the ICS 1000 Control Panel in Chromeleon 2 Turnoffthe main power switch to ensure that you do not unintentionally start the ICS 1000 3 To prevent contamination of pump parts put on a pair of rubber gloves before disassembling the pump head 4 Disconnect the tube fittings from the inlet and outlet check valve assemblies on the primary pump head see Figure 5 4 5 Usea 1 2 inch wrench to loosen both check valve assemblies Remove the check valve assemblies from the pump head Outlet Check Valve Primary Pump Head Secondary Pump Head Acorn Nuts Inlet Check Valve Figure 5 4 Pump Heads NOTE The inlet check valve assembly housing has a 1 4 28 port The outlet check valve assembly housing has a 10 32 port Doc 031879 01 3 03 5 11 ICS 1000 lon Chromatography System 6 Ifyou are installing new cartridges P N 045994 in the existing check valve Double hole Single hole 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 Outlet Check NOTE The pump will not operate Valve properly unless the cartridge is installed in the housing in the correct orientation Liquid flows through the check valve in the large single hole and out the small double holes 7 Install the inlet check valve
118. njecting Samples After loading the sample in the sample loop switch the injection valve to the Inject position using one of the following methods e Manually Click the Inject button on the Chromeleon Control Panel see Figure 3 6 e Automatically Include the Inject command in a Chromeleon program See the examples in Section 3 10 5 3 10 5 Example Chromeleon Commands for Loading and Injecting Samples The following examples show commands for loading and injecting samples using an AS50 or AS40 autosampler Example AS50 Program Commands 0 000 Pump ECD Autozero Zero the baseline Load Switch the valve to Load Wait CycleTimeState Wait for cycle time if any Inject Switch the valve to Inject Wait InjectState Wait for injection to complete ECD 1 AcqOn Start data acquisition 14 000 ECD 1 AcqOff Stop data acquisition Example AS40 Program Commands 2 300 Pump ECD Relay 1 Closed Duration 138 00 Note 1 0 000 Pump ECD Autozero Note 2 ECD_1 AcqOn Note 3 Pump InjectValve InjectPosition Duration 30 00 Note 4 30 00 ECD 1 AcqOff Note 5 Doc 031879 01 3 03 3 17 ICS 1000 lon Chromatography System AS40 Program Command Notes 1 Ce go le D Close the ICS 1000 RELAY OUT 1 which is connected to the AS40 LOAD relay This signals the AS40 to load the sample Zero the baseline Start data acquisition Switch the valve to Inject Stop data acquisition 3 11 Process Samples Samples
119. no air bubbles are exiting the pump waste line 5 Press Pump Off 6 Close the waste valve Do not overtighten The pump is now ready for operation NOTE Ifthe two standard priming procedures described above are unsuccessful prime the pump with isopropyl alcohol See Section 5 15 for instructions B 38 Doc 031879 01 3 03 Equilibrating the System B 15 Equilibrating the System 1 After priming the pump turn on the pump and set the flow to the operating rate Flush the system for about 5 minutes to equilibrate Monitor the system pressure from the Control Panel to make sure it is at the expected pressure for the installed column refer to the column manual for details and is stable If the pressure is less than the expected amount gas may be trapped in the system Release the gas by removing the pump fitting on the injection valve The fitting is labeled P 2 Allow the air to escape and then reconnect the fitting Check that liquid is flowing out of the suppressor REGEN OUT waste line and that the pressure is stable Monitor the baseline conductivity In general it should be 30 uS for a system set up for anion analyses and 2 uS for a system set up for cation analyses Equilibration time varies and it can take some time to reach these expected values B 16 Verifying Operational Status After the system has equilibrated verify the actual pump pressure and stability by monitoring the pump pressure reading o
120. ns B 9 Plumbing B 25 Power connection B 11 Priming B 36 B 38 Separator column B 20 Software license B 5 B 6 Stand alone operation setup C 7 C 8 Starting the ICS B 12 Suppressor B 21 TTL and relay connections C 1 C 2 Unpacking B 2 USB connections B 9 B 10 Waste lines B 23 Injecting samples 3 14 Installation troubleshooting B 53 Via autosampler 3 16 Inverted edge TTL input control C 4 Via syringe 3 15 Inverted pulse TTL input control C 5 Via vacuum syringe 3 16 Ion chromatography Injection port 2 1 Overview 1 1 Injecting via syringe 3 15 Ion exchange 1 3 Injection valve 2 5 2 24 Isocratic delivery system 1 2 Controlling with an AS50 B 43 C 9 Isopropyl alcohol 5 29 Index 4 Doc 031879 01 3 03 Index K Key code Chromeleon B 6 L Leak sensor 2 5 Leak sensor wet alarm 4 4 Replacement 5 28 Leaks Cell 4 10 Fittings 4 9 Injection valve 4 10 Liquid 4 9 Pressure transducer 4 10 Pump check valve 4 9 Pump head 4 10 Pump head waste valve 4 10 Pump piston seal 4 10 Suppressor 4 10 LED A 2 License Chromeleon B 5 B 6 License server Chromeleon B 6 Linearity requirements A 3 Liquid leaks 4 9 See also Leaks Load inject valve alarm 4 5 Loading samples 3 14 Loop See Sample loop Low pressure limit A 2 M Main power receptacle 2 8 Maintenance 3 21 Daily 3 21 Ongoing 3 21 Weekly 3 21 Yearly 3 22 Manual sample p
121. ntended as a starting point only You can add additional samples to the sequence change injection parameters and edit the pgm and qnt files Refer to the Chromeleon online Help for details NOTE After completing the installation see Section 3 11 for how to process the samples and standards in the sequence 19 Double click the pan file to open the Control Panel for your system see the example in Figure B 33 IE ICS 1000 System ICS 1000 AMAR CS 1000 Pump Sampl Datasource 16 07 29 User AMar from AMAR E psi has connected to timebase ICS 1000 Sequence 16 07 28 User AMar from AMAR Sample has acquired control over timebase ICS 1000 Settings Program CS 1000 Injector Elapsed Program Time ICS 1000 System Total Program Time Connected Startup Shutdown Show Plot Load PUT Inject 40 0 irom Pas _Injector Settings Settings CS 1000 Detector uaua 0 108 uS Suppressor Off sc O oma Detector Settings 0 00 0 50 1 00 1 50 2 00 Figure B 33 ICS 1000 System Control Panel Example B 34 Doc 031879 01 3 03 Setting the Eluent Level NOTE If the Connected check box is not selected click the box to connect the ICS 1000 to the Control Panel B 12 1 Verifying Chromeleon Communication Verify that Chrome
122. off the pump motor The pump is now ready for operation Doc 031879 01 3 03 5 29 ICS 1000 lon Chromatography System 5 16 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 1000 DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du ICS 1000 DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des ICS 1000 ACHTUNG 2 The fuse holder is part of the main power receptacle see Figure 5 20 on the ICS 1000 rear panel To remove the fuse holder squeeze the tab on the top of the holder to release it and pull the holder straight out of its compartment 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 Main Power Receptacle Fuses 2 LE oi Fuse Holder Fuse Holder Side View Figure 5 20 Main Power Fuse Holder 5 30 Doc 031879 01 3 03 A 1 Electrical Main Power Fuses A 2 Physical Dimensions without reservoir Weight Decibel Level A Specifications 85 to 265 Vac 47 to 63 Hz The ICS 1000 power supply is au
123. om the new eluent valve through the mounting plate Attach the mounting plate to the new valve using the screws removed in Step 8 Figure 5 17 Removing the Valve Mounting Plate Connect the cable from the new valve to the ICS 1000 cable Feed the cables back inside the ICS 1000 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 Turn on the power to the ICS 1000 Prime the pump see Section B 14 Doc 031879 01 3 03 5 27 ICS 1000 lon Chromatography System 5 14 Replacing the Leak Sensor 1 Turn off the power to the ICS 1000 2 Open the ICS 1000 front door 3 Loosen the screw on the front of the leak sensor see Figure 5 18 Note The screw remains attached to the sensor Loosen Leak Sensor 4 Remove the leak sensor from the component panel and pull the cable out of the opening in the panel 5 The cable attached to the leak sensor connects to a cable inside the ICS 1000 Continue pulling the cable until the connectors for the two cables are outside of the panel see Figure 5 19 6 Disconnect the two cables Figure 5 19 Leak Sensor Cable 7 Connect the cable from the new leak sensor to the ICS 1000 cable 8 Feed the cables back inside the ICS 1000 Align the leak sensor with the component panel opening and fingertighten the screw 9 Make sure the leak sensor does not tou
124. omatography System 10 Press the suppressor onto the tabs and then slide it down to lock it in place Pull slightly on the center of the suppressor to verify that it is securely fastened Figure B 20 shows an SRS suppressor installed on the component panel Remove the union connecting ELUENT IN and ELUENT OUT and connect these lines to the corresponding ports on the suppressor Figure B 20 Suppressor Installed SRS Shown Remove the fitting plug from REGEN IN and connect it to the REGEN IN port on the suppressor Connect the TO SRS AES REGEN OUT line to the REGEN OUT port on the suppressor Replace the cover on the column heater if installed making sure the GUARD IN line is aligned with the slot on the side of the heater cover Go on to Section B 10 B 22 Doc 031879 01 3 03 Connecting the Waste Lines B 10 Connecting the Waste Lines The ICS 1000 has the following waste lines e PUMP WASTE carries prime waste from the pump e TO WASTE OUT carries sample overflow from the injection valve e WASTE GAS SEPARATOR carries system waste from the suppressor Untape the coiled waste lines from the rear panel Place the ends of the PUMP WASTE and TO WASTE OUT lines into a waste container Direct the WASTE GAS SEPARATOR line from the top of the ICS 1000 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
125. on rinse seal gently insert the shaft of the piston through the small hole in the center of the guide see photo below c Pullthe seal off the end ofthe piston shaft and remove the piston from the guide 3 Hold the new piston rinse seal P N 048722 with the grooved side facing up 4 Using your fingertip gently press the piston rinse seal into the guide until the edge of the seal is below the surface of the guide The piston rinse seal is made of soft plastic Do not press on the seal with anything hard or sharp including your fingernail If the seal is nicked or gouged it will not seal properly and may result in leaks 5 Place the new O ring P N 059283 into the groove in the guide 6 Remove the O ring from the groove in the flat side of the spacer and replace it with the new O ring P N 014895 Doc 031879 01 3 03 5 15 ICS 1000 lon Chromatography System 8 In one hand hold the guide with the O ring and piston rinse seal facing up this prevents the O ring from falling out In the other hand hold the spacer with the cavity facing down Gently press the guide into the cavity in the spacer until it is fully seated Removing the Piston Seal from the Head 1 6 Fill the head cavity with deionized water by injecting the liquid through either the piston opening or the inlet check valve Reinsert the piston approximately 1 8 inch into the seal If this is the primary pump head install a 10 32 fit
126. op P N 042857 is installed on the valve at the factory See Section 2 4 4 for details about valve operation Separator and Guard Columns Both the separator and guard columns are packed with resin and perform the separation of the sample ions The main function of the guard column is to trap contaminants and remove particulates that might damage the separator column Column Heater Optional Not Pictured The column heater controls the temperature of the separator and guard columns The temperature can be set to between 30 C and 60 C and it must be set at least 5 C above the ambient temperature See Section 2 4 5 for details about the column heater Doc 031879 01 3 03 2 5 ICS 1000 lon Chromatography System Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions thereby increasing detection sensitivity Either an AES Atlas Electrolytic Suppressor SRS Self Regenerating Suppressor or MMS MicroMembrane Suppressor can be used with the ICS 1000 See Section 2 4 6 for details DS6 Heated Conductivity Cell The flow through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell A heat exchanger inside the cell regulates the temperature which can be set to between 30 C and 55 C For optimum performance set the temperature to at least 7 C above the ambient temperature See Section 2 4 7 for details about the c
127. ort to the ICS 1000 injection valve is calibrated for use with the ICS 1000 To ensure injection precision do not shorten by cutting or lengthen this line or replace it with a different uncalibrated line Route AS50 needle seal line to ICS 1000 injection valve Insert the waste line from the ICS 1000 injection valve here Figure B 38 AS50 Drip Tray Doc 031879 01 3 03 B 41 ICS 1000 lon Chromatography System 4 Connect the needle seal line from the AS50 to port AS50 S 5 on the injection valve Needle Seal Li see Figure B 39 S The green waste line that is connected to port W 6 on the injection valve see Figure B 39 is connected with a union to a Teflon waste line see Figure B 40 and routed through the tubing chase to the ICS 1000 rear panel Waste 5 Disconnect the green waste line labeled AS50 TRAY from the union and route the line to the drip tray in the autosampler compartment AS50 Waste Line disconnect from union You can either leave the disconnected Teflon waste line and union in the tubing chase or pull the line out from the front Figure B 40 Injection Valve Waste Line Union 6 Pushthe end of the green AS50 TRAY line into the small round opening on the right side of the ASSO tray see Figure B 38 Make sure the injection valve waste line is not elevated above the injection valve at any point between the valve a
128. osampler see Section B 17 of this manual To connect an AS40 see Section B 18 Also see the AS50 Autosampler Operator 5 Manual Document No 031169 or the 4S40 Automated Sampler Operator s Manual Document No 034970 The manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 E 2 How dol print Click the Print toolbar button in Chromeleon see Section 2 3 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 6 for pump flow rate troubleshooting If a contaminated column is suspected clean the column as instructed in the column manual The column manual is included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 E 4 How dol adjust retention times Retention times are calculated during calibration The Use Recently Detected Retention Time parameter in the Chromeleon QNT Editor General tab can be used to compensate for some types of retention time drifts for example evaporation of volatile components in pre mixed solvents or an aging column Refer to the Chromeleon Help or user s guide for details Doc 031879 01 3 03 E 1 ICS 1000 lon Chromatography System E 5 E 6 E 7 E 8 E 9 E 10 E 11 When should remake standards Standards are used only for calibration and should always be made fres
129. p Type Cell Temp Connected Autozero Ready Data Rate a Show Plot Hold Mode 10 0 i olume d from Pos Position Stop Mode Pressure ressure Value Flow Rate Off On Prime Inject Valve Inject Load Eluent Flow Valve Closed Open h 1 00 1 50 2 00 2 50 3 00 3 50 4 00 4 50 5 00 Figure B 49 ICS 1000 Traditional System Control Panel Unconnected Doc 031879 01 3 03 B 51 ICS 1000 lon Chromatography System 3 To connect the Control Panel to the ICS 1000 open the Control menu and click the name of the ICS 1000 timebase at the bottom of the menu The Control Panel is now connected to the ICS 1000 and the controls are enabled see Figure B 50 F ICS 1000 Pump and Detector ICS 1000 AMAR Audit Trail Datasource Elapsed Time 15 02 01 User AMar from AMAR has acquired control over timebase ICS 1000 15 08 15 EluentValve Open Sequence Run Time 15 08 19 EluentValve Closed s m 15 08 21 EluentValve Open ample 8 15 08 23 EluentValve Closed e EAE ICS 1000 Pump ICS 1000 Dete ctor mmm Eluent Bottle jv Connected Iv Connected Connected 0 09009 uS None E 35 0 C 0 001 COE agg avec CL Toa T Shut e E Hold Mod 10 0 ode
130. pecifications listed in Appendix A Provide a sturdy workbench for the ICS 1000 of a height that ensures convenient access to the interior Allow at least 15 cm 6 in behind the ICS 1000 for power connections and ventilation For optimal performance install the ICS 1000 in a draft free location out of the path of air conditioning and heating vents Optional Provide a clean gas source regulated to between 0 55 and 0 83 MPa 80 and 120 psi for pressurization of the eluent reservoir Use ASTM filtered Type I 18 megohm deionized water when preparing eluent and regenerant Doc 031879 01 3 03 B 1 ICS 1000 lon Chromatography System B 2 Unpacking the ICS 1000 System 1 After removing the ICS 1000 from the shipping box and removing the top layer of foam remove the next layer of foam see Figure B 1 Figure B 1 ICS 1000 After Removing Shipping Box and First Layer of Foam 2 Setthe eluent bottle on top of the ICS 1000 see Figure B 2 CE Figure B 2 ICS 1000 with Eluent Bottle B 2 Doc 031879 01 3 03 Unpacking the ICS 1000 System 3 CAUTION MISE EN GARDE VORSICHT Remove the next layer of foam and remove the Ship Kit box see Figure B 3 Figure B 3 ICS 1000 with Ship Kit The bottom foam layer has two cutouts on either side of the ICS 1000 module use these as hand holds when lifting the module see Figure B 3 Lift the ICS 1000 out of the bottom layer of foam and set it on a
131. place the column heater see Section 5 11 COLUMN HEATER SHORT CIRCUIT This error occurs when there is a short circuit on the thermistor input used to measure the column heater temperature This error indicates a faulty column heater To troubleshoot e Replace the column heater see Section 5 11 Doc 031879 01 3 03 4 3 ICS 1000 lon Chromatography System DEGAS CALIBRATION FAILED This error occurs when the degas vacuum does not reach the expected level during calibration To troubleshoot 1 Retry the calibration 2 Ifcalibration still fails the vacuum degas assembly may need to be replaced Contact Dionex for assistance HARDWARE NOT PRESENT This error indicates an error in the ICS 1000 electronics To troubleshoot e Contact Dionex for assistance The ICS 1000 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 4 If liquid accumulates in the tray the sensor signals the problem and the Leak sensor wet error message appears To troubleshoot 1 Locate the source of the leak by visually inspecting the tubing fittings and components on the component panel 2 Tighten fittings or replace tubing and fittings as required Refer to Section 4 2 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray thoroughly to prevent th
132. pump flow is also stopped Flow Rate Sets the pump flow rate in mL min Pressure The sliders select the upper and lower pressure limits The Pressure field displays the current pressure On Off Prime Turn the pump on and off or start the pump priming function 2 16 Doc 031879 01 3 03 2 Features Inject Valve Displays the current position of the inject valve The Inject and Load buttons select the position Inject Load rEluent Flow Valve Closed Open Column Heater Optional ICS 1000 Column Heater so c Inject Valve Eluent Flow Valve Displays the current position of the eluent flow valve The Closed and Open buttons select the position Set Temp Sets the temperature of the column heater Detector ICS 1000 Detector F Connected JOHN EXCITE J None 03 E soc s Aerem Ready 5 0 Hz Stetina 0 mA 4 ELS Mode Show Plot from Pos 10 0 E ECD 1 0 112 5 0 min 1 0 0 00 0 50 1 00 1 50 2 00 2 50 3 00 3 50 4 00 4 50 5 00 Connected Connects the ICS 1000 to the Chromeleon Control Panel enabling communication between the PC and the module Clearing the Connected check box disconnects the ICS 1000 from the PC Autozero Sets the conductivity to zero Ready Indicates if the detector is ready to begin data acquisition Doc 031879 01 3 03 2 17 ICS 1000 lon Chromatography System Signal Displays the offset
133. quirements The manual is on the Dionex Reference Library CD ROM P N 053891 Excessive System Backpressure Restriction in the system plumbing Check all liquid lines for crimping or blockage Make sure the ferrule fittings are not overtightened onto tubing Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for details The manual is on the Dionex Reference Library CD ROM P N 053891 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 Doc 031879 01 3 03 4 15 ICS 1000 lon Chromatography System Clogged column bed supports Refer to the instructions in the column manual for troubleshooting guidance Column manuals are included on the Dionex Reference Library CD ROM P N 053891 located in the ICS 1000 Ship Kit P N 057905 Contaminated columns Clean the columns as instructed in the column manual Plugged injection valve passages Rebuild the injection valve see Section 5 4 4 8 Peak Ghosting Ghosting is the appearance of extraneous peaks in a chromatogram These may be late eluting peaks from a previous injection or
134. r setting up Chromeleon For details about any of these steps refer to the Chromeleon user s guide or online Help B 8 1 Assigning the ICS 1000 to a Timebase 1 Ifthe Chromeleon Server is not running the icon on the taskbar is crossed out in red ax start the Server by right clicking the icon and selecting Start Server When the server starts the icon changes to gray ss 2 Open the Server Configuration program select Start gt Programs gt Chromeleon gt Server Configuration 3 The Unassigned USB Devices dialog box appears see Figure B 10 Unassigned Dionex IC USB Devices Detected x The software has detected USB devices which are not assigned to a Timebase You may add the devices to an existing Timebase create a new Timebase for these devices or simply press the Cancel button to postpone assigning the module Server Name AMAR r Timebase m Unassigned USB Devices 1CS 1000 200011 Assigned Devices Dionex ASI 100 Autosampler Dionex P580 Pump Dionex LI VD3405 PDA lt lt massi Has Mioaule New Delete Jo Launch Sener Gontiquration on GK Cancel Figure B 10 ICS 1000 Unassigned to Timebase Doc 031879 01 3 03 B 13 ICS 1000 lon Chromatography System 4 Click the New button 5 The Timebase box displays a default name the Server Configuration name You can use the provided name or type a new one for example ICS 1000 6 Press
135. rapped in the system Release the gas by removing the pump fitting on the injection valve port labeled P 2 Allow the air to escape and then reconnect the fitting e Ifthe pressure fluctuates by more than about 0 13 MPa 20 psi prime the pump See Section 4 3 for additional troubleshooting information e Ifthe pressure is too high there may be a restriction in the system plumbing See Section 4 7 for troubleshooting information Verify that the baseline conductivity is at the expected reading for your application and is stable In general it should be 30 LS for a system set up for anion analyses and lt 2 uS for a system set up for cation analyses See Section 4 12 for troubleshooting information if the conductivity is too high See Section 4 13 if the baseline is drifting or has excessive noise large fluctuations in readings Verify that the cell heater is at the set point and is stable The temperature is at equilibrium when the Set Temperature and Current Temperature readings on the Control Panel are the same Verify that the column heater temperature if installed is at the set point and stable The temperature is at equilibrium when the Set Temperature and Current Temperature readings on the Control Panel are the same The system is now ready for sample processing Doc 031879 01 3 03 3 11 ICS 1000 lon Chromatography System 3 9 Prepare Samples 3 9 1 3 9 2 NOTE Sample preparation can be performed wh
136. re 5 6 Priming Valve Knob P N 055709 Outlet Check A Valve Assembly P N 045721 O Ring P N 055752 Piston Seal p P N 055870 f Spacer with Drain P N 057913 lt Primary Pump Head N VE P N 055711 Piston Rinse Seal a S A Ew P N 048722 N Qo RA O Ring IS J P N 014895 J O Ring Inlet Check Ne PIN 059283 __ valve Assembly gt Seal Guide P N 045722 Piston P N 058032 PIN 052840 Figure 5 5 Primary Pump Head Waste Valve Knob P N 055710 F YJZ A O Ring P N 055752 Piston Seal x P N 055870 ee NY Spacer with Drain Secondary PIN 057913 J Pump Head j Piston Rinse Seal AAN Vy PIN 048722 CAT eA O Ring Seal Guide eee P N 058032 X O Ring 74 P N 059283 Piston P N 052840 Figure 5 6 Secondary Pump Head 5 14 Doc 031879 01 3 03 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 Hold the guide with the flat side facing up b To dislodge the pist
137. reservoir enter the volume of liquid in the reservoir on the Chromeleon Control Panel see Figure 3 6 The ICS 1000 determines the eluent usage by monitoring the flow rate and the length of time the pump is on and updates the Eluent Level field as the eluent is used up A warning first appears if the level falls below 200 mL Warnings are repeated at 100 mL and 0 mL In order for the eluent level displayed on the Control Panel to be accurate the level must be entered by the user when the reservoir is filled The ICS 1000 does not automatically detect when the reservoir is filled nor when it is empty Enter the volume of Note The Eluent Bottle liquid in the reservoir 200 amp field and slider gauge ICS 1000 Pump Eluent Bottle are updated as the 74 iie un liquid is used up se 0 3 4 6 Figure 3 7 Setting the Eluent Level 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 1000 3 8 Doc 031879 01 3 03 3 Operation and Maintenance 3 5 Check All Connections 1 Make sure the reservoir is filled and the tubing connecting the reservoir to the ICS 1000 tubing is securely connected Make sure the USB cable from the computer is connected to the USB receptacle on the ICS 1000 rear panel 3 6 Prime the Pump If you changed elu
138. ressor over power 4 8 Suppressor stopped for zero flow rate 4 8 F Facility requirements B 1 Filter end line Bacterial contamination 3 21 4 12 Dirty or clogged 3 21 4 12 Installation 3 7 Fittings Leaking 4 9 Replacing 5 9 Requirements 5 9 Doc 031879 01 3 03 Index 3 ICS 1000 lon Chromatography System Flow rate 2 5 A 2 Calibration 5 6 Troubleshooting 4 14 Flow schematic 2 9 FROM PC USB connections B 9 Front panel 2 1 Specifications A 2 Fuses Replacement procedure 5 30 Requirements A 1 G Gas separator waste tube B 23 Gas source Connection B 47 Installation B 47 Pressure requirement B 47 Ghosting 4 16 Guard column 2 5 B 19 Installation B 20 H Hardware not present error 4 4 Heater Column 2 26 High pressure alarm 4 6 High pressure limit A 2 Humidity limits A 1 I Leaking 4 10 Plumbing connections 2 24 Rebuilding 5 10 Specifications A 3 Troubleshooting 4 5 Installation B 1 B 53 Adding devices to a timebase B 16 Analog output connection C 9 AS40 autosampler B 44 ASS50 Autosampler B 40 Assigning devices to a timebase B 15 Assigning USB devices B 14 Chromeleon B 5 B 13 Columns B 19 Computer B 4 Eluent reservoir B 25 B 48 Equilibrating the system B 39 Gas separator waste tube B 23 Gas source B 47 Guard column B 20 Key code B 8 Operating system requirements B 5 Operational status verification B 39 PC connectio
139. rily in sequence BE 800 psi Sequence SEQ MAMAR Io 000manual Sample 2 on server version 6 50 SP2 Build Pump Settings 957 Alpha started serial number 853 Program LoadPosition Load Inject Injector Settings jICS 1000 Detector 0 022 uS Suppressor Off L oma Detector Settings Elapsed Program Time Total Program Time ICS 1000 System iv Connected Startup Shutdown Show Plot from Pos Figure 2 9 ICS 1000 System Control Panel Graphical 2 14 Doc 031879 01 3 03 2 Features System Controls Overview This section provides brief descriptions of the various controls available on the ICS 1000 System Control Panels NOTE The examples are from the traditional style of panel Datasource Elapsed Time Sequence Run Time Sample em Pod Startup Shutdown Datasource Displays the database in which the chromatographic data for the sample is saved Sequence Displays the sequence in which this sample is included Sample Displays the name of the sample that is running Program Displays the name of the program that is running Elapsed Time Displays the time that has elapsed since the sample analysis began Run Time Displays the total run time System Startup Starts the pump and suppressor The flow rate and suppressor current settings that were in effect at system shutdown see below are restored
140. rly maintenance 3 22 Atlas Electrolytic Suppressor 2 6 See also Suppressor Audit Trail 2 16 Automated control 2 11 Autosampler Sample injection 3 16 See also AS40 Automated Sampler See also ASS0 Autosampler Autozero 2 17 3 11 3 18 Index B Background conductivity High 4 18 Offsetting 3 11 Backpressure 2 23 Restriction in plumbing 5 7 Troubleshooting 4 15 Baseline Drift 4 19 Equilibration B 39 Noise 2 10 4 19 Stability 2 27 Batch processing 3 2 Starting 3 20 See also Sample processing Blockages Liquid lines 4 6 5 7 Bottle See Reservoir Browser 2 12 3 5 B 51 C Cables AS40 Relay Control B 44 Power cord 5 30 USB B 9 Calibration 5 1 Conductivity cell 5 4 Flow rate 5 6 Vacuum degas assembly 5 7 Cation separations 3 11 Cell See Conductivity cell Cell calibration 5 4 Cell drive A 3 Doc 031879 01 3 03 Index 1 ICS 1000 lon Chromatography System Check valves Cleaning procedure 5 11 5 12 Replacement procedure 5 11 5 12 Chromatogram 1 3 Chromeleon 2 11 Adding devices to a timebase B 16 Alarm conditions 4 3 Browser 2 12 3 5 Control Panel 2 11 3 18 Creating a sequence 3 19 Degas options 4 20 Direct control 2 11 Error messages 4 3 Installation B 5 B 13 Interface 2 11 License installation B 5 B 6 Menu 2 11 3 18 Programs 2 11 2 15 3 16 3 19 Starting 3 4 B 26 System properties dialog box B 16 Timebase 3 5 Toolbar
141. rocedures Lists problems and presents step by step procedures for how to isolate and eliminate the cause of each problem Provides step by step instructions for routine service and parts replacement procedures that the user can perform Lists the ICS 1000 specifications and installation site requirements Describes how to install the ICS 1000 Describes the ICS 1000 TTL and relay control features Lists spare parts for the ICS 1000 Provides answers to frequently asked questions about ICS 1000 operation Defines terms commonly used in ion analysis Doc 031879 01 3 03 ICS 1000 lon Chromatography System 1 3 1 gt DANGER gt WARNING gt CAUTION IMPORTANT gt DANGER gt AVERTISSEMENT gt MISE EN GARDE Safety Messages and Notes This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the ICS 1000 when properly followed Safety messages appear in bold type and are accompanied by icons as shown below Indicates an imminently hazardous situation which if not avoided will result in death or serious injury Indicates a potentially hazardous situation which if not avoided could result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury Also used to identify a situation or practice that may seriously damage the instrument but will not caus
142. rocessing 3 2 MicroMembrane Suppressor 2 6 See also Suppressor N Nitrite in samples 3 12 Normal edge TTL input control C 4 Normal pulse TTL input control C 4 O Offsetting background conductivity 3 11 Operating features 2 1 Operating pressure A 1 Operating ranges Cell heater 2 6 Column heater 2 5 Flow rate 2 5 Operating system requirements B 5 Operating temperature A 1 Operation Equilibration time 3 11 Overview 3 1 Priming 3 9 5 29 B 38 Reservoir setup 3 6 Sample preparation 3 12 Sample processing 3 2 Setting operating conditions 3 10 Starting Chromeleon 3 4 System power up 3 3 Operational status verification 3 11 Option not installed error 4 5 Oven See Column heater Overview 1 4 P Panels Chromeleon Control Panel 2 11 3 18 Chromeleon Wellness Panel 5 1 Component panel 2 4 Parameters Chromeleon operating commands 2 11 3 19 B 34 Doc 031879 01 3 03 Index 5 ICS 1000 lon Chromatography System PC See Computer Peak ghosting 4 16 Peak height Reproducibility 2 27 Troubleshooting 4 17 Peaks Extraneous ghosting 4 16 PEEK Conductivity cell body 2 27 Physical specifications Decibel level A 1 Dimensions A 1 Weight A 1 Piston seals Replacement procedure 5 13 5 14 5 16 5 17 Pistons Replacement procedure 5 17 Plotting detector output 2 18 Plumbing Columns and suppressor B 25 Injection valve 5 10 Replacing tubing and fittings 5 9 Troubleshoo
143. romeleon control the AS50 must be added to the ICS 1000 timebase see Section B 8 For front panel control the AS50 and ICS 1000 can be set up for 3 14 Doc 031879 01 3 03 3 Operation and Maintenance stand alone operation This requires a TTL cable connection between the AS50 and the ICS 1000 See Section C 3 for stand alone setup instructions 3 10 1 Loading Samples with a Syringe 1 Make sure the injection port on the ICS 1000 front door see Figure 2 1 is connected to the sample port S 5 on the injection valve see Figure 3 9 SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP TO INJ Orange VALVE c Black TO INJ VALVE W Green Figure 3 9 Injection Valve Connections 2 Fill the 1 cc syringe P N 016388 provided in the ICS 1000 Ship Kit P N 057905 with a calibration standard or sample 3 Insert the syringe into the injection port on the ICS 1000 front door 4 Verify that the injection valve is in the Load position 5 Overfill the sample loop with several sample loop volumes Excess sample will exit through the injection valve waste line 6 Leave the syringe in the port 7 Switch the injection valve to the Inject position see Section 3 10 4 Doc 031879 01 3 03 3 15 ICS 1000 lon Chromatography System 3 10 2 Loading Samples with a Vacuum Syringe 3 10 3 1 Disconnect the waste line from port W 6 of the injection
144. s 2 11 3 18 Verifying communication B 35 Wellness Panel 5 1 Chromeleon Server Starting 3 4 B 13 Chromeleon Server Configuration program Starting B 13 Timebase B 15 Column heater 2 5 2 26 Replacement procedure 5 23 Specifications A 4 Column heater alarms Column heater exceeds safe temperature 4 3 Column heater open circuit 4 3 Column heater short circuit 4 3 Columns 2 5 Cleaning E 3 Contaminated 4 17 Damage from IPA 5 29 Installing B 19 Storing E 2 Commands Chromeleon 2 11 3 19 B 34 Component panel 2 4 Computer Connections B 9 Operating system requirements B 5 Unpacking B 4 Conductivity Causes of high conductivity E 3 Temperature effect 2 27 Conductivity cell 2 6 2 27 Calibrating 5 4 Calibration constant 5 21 High cell output 4 18 Leaking 4 10 No response 4 18 Replacement procedure 5 20 Specifications A 3 Volume 2 27 Conductivity cell specifications Active volume A 3 Cell body A 3 Electrodes A 3 Maximum pressure A 3 Contacting Dionex 5 1 Contamination Column 4 16 4 17 Eluents 4 16 Sample 4 17 Standard 4 16 Control Panel 2 11 2 13 3 18 System Panel 2 13 Wellness Panel 2 13 D Daily maintenance 3 21 Data Backing up E 2 Deleting E 2 Saving 3 19 Data acquisition 3 18 Data analysis description 1 3 Index 2 Doc 031879 01 3 03 Index Data rise time B 46 Decibel level A 1 Degas tubing assembly See Vacuum degas assembly Degas calibr
145. s source regulated to between 0 55 and 0 83 MPa 80 and 120 psi 3 Push the other end of the tubing onto the inlet of the air regulator see Figure B 46 4 Remove the eluent reservoir cap 5 Connect the gas line from the eluent reservoir cap to the gas line on the air regulator outlet 6 Slip the air regulator accessory bracket over the neck of the eluent reservoir see Figure B 46 Eluent Gas Line Lj Air Regulator Accessory Bracket i k a h ON Gas Inlet Line 3 mm 1 8 in ID Connec as source LA Figure B 46 ICS 1000 Pressurized Eluent Reservoir Connections Optional Doc 031879 01 3 03 B 47 ICS 1000 lon Chromatography System B 20 2 Pressurizing the Eluent Reservoir Optional NOTE Do not pressurize the ICS 1000 until after the reservoir is plumbed 1 Pull out the air regulator knob and turn it fully counterclockwise to ensure there is no pressure to the reservoir when the gas source is turned on 2 Turnon the gas source 3 Pull out the air regulator knob and turn it clockwise to pressurize the eluent reservoir 4 Adjustthe pressure to between 30 and 40 kPa 5 and 6 psi Push the regulator knob back in Do not pressurize the eluent reservoir above 70 kPa 10 psi CAUTION Ne mettez jamais les r servoirs d luants sous une pression sup rieure 0 07 MPa 10 Ib po MISE EN GARDE Setzen Sie den Eluentbehalter auf keinen Fall einem Druck ber 0 07 MPa
146. sampler For autosampler injections the injection port tubing is disconnected from the ICS 1000 injection valve and replaced by the autosampler outlet tubing Other setup requirements depend upon the model of autosampler Setup for an AS40 Autosampler A relay or TTL connection is required for Chromeleon to control sample loading See Section B 18 for AS40 autosampler installation instructions Setup for an AS50 Autosampler To use an AS50 autosampler with the ICS 1000 the AS50 must meet the following requirements e An injection valve cannot be installed in the AS50 e The AS50 must have Moduleware version 1 11 or later installed e Control of the ICS 1000 injection valve must be enabled in the AS50 The following AS50 models are configured at the factory to meet the above requirements e AS50 without injection valve P N 061309 e AS50 without injection valve with sample preparation P N 061310 e AS50 without injection valve with sample preparation and sample tray cooling P N 061311 e AS50 without injection valve with sample tray cooling P N 061312 See Section B 17 for AS50 autosampler installation instructions After the ASSO is configured for use with the ICS 1000 all ASSO modes of injection full loop partial loop and partial loop limited sample are supported In addition all AS50 injection valve commands whether issued from the AS50 front panel or from Chromeleon will control the ICS 1000 injection valve For Ch
147. ssigned devices B 13 V Vacuum degas assembly 2 19 Calibration 5 7 Components 2 19 Fails to run 4 20 Priming B 37 Specifications A 3 Troubleshooting 4 11 Valve See Eluent valve See Injection valve W Warranty voiding 5 1 Waste lines Blocked 4 9 Connection B 23 Connection to AS50 B 42 Waste valve 2 22 Opening 2 22 5 13 O ring replacement procedure 5 18 Water samples 3 12 Weekly maintenance 3 21 Weight A 1 Wellness Panel 2 13 5 1 Y Yearly maintenance 3 22 Doc 031879 01 3 03 Index 9 ICS 1000 lon Chromatography System Index 10 Doc 031879 01 3 03
148. t the Waste Gas Separator line to the waste tube see Figure B 22 CAUTION NE FERMEZ PAS LE CONTENEUR DE GAZ R SIDUEL L Le ICS 1000 travaille avec un proces d lectrolyse qui produit des petites quantit s de gaz d oxyg ne ou d hydrog ne Afin de garantir que le gaz ne soit pas enferm dans un conteneur ferm et puisse s y concentrer connectez un tube noir gaz r siduel diam tre int rieur 1 3 cm n de commande 045460 un conteneur ouvert non ferm Connectez le conteneur r siduel au tube r siduel gaz s parateur d sign Waste Gas Separator MISE EN GARDE B 24 Doc 031879 01 3 03 Setting Up the Eluent Reservoir VERSCHLIESSEN SIE DEN ABFALLBEHALTER NICHT Der ICS 1000 verwendet einen Elektrolyseprozess wodurch kleine Mengen an Sauerstoff und Wasserstoff entstehen Fuhren Sie einen schwarzen Gasabscheiderschlauch ID 1 3 cm Bestell Nr 045460 in einen VORSICHT offenen unverschlossenen Abfallbehalter damit sich das Gas nicht in einem geschlossenen Behalter sammelt und aufkonzentriert Verbinden Sie die mit Waste Gas Separator bezeichnete Leitung mit dem Abfallschlauch B 11 Setting Up the Eluent Reservoir 1 Rinse the eluent reservoir 2 Prepare the eluent as instructed in the manual for the column being installed The column manual is included on the Dionex Reference Library CD ROM P N 053891 located in the Ship Kit 3 Fill the reservoir with the prepared eluent 4
149. tch on the ICS 1000 rear panel see Figure 3 3 to turn on the system power Table 3 2 shows the ICS 1000 conditions at power up Also turn on the power to the computer and the autosampler if Mul T Ir asd B Figure 3 3 ICS 1000 Rear Panel Feature Power Up Condition Pump Off Injection valve Load position Cell Reading current value Suppressor Off Cell heater Set to the last value used The default when the Column oven temperature Optional ICS 1000 is turned on for the first time is 35 C Set to the last value used The default when the ICS 1000 is turned on for the first time is 30 C Table 3 2 ICS 1000 Power Up Conditions When you start the suppressor the value used last is restored Doc 031879 01 3 03 3 3 ICS 1000 lon Chromatography System 3 3 Start Chromeleon 1 NOTE See Section B 8 for how to set up Chromeleon if you are beginning operation of an ICS 1000 that has not been configured in a timebase If the Chromeleon Server is not running the icon on the taskbar is crossed out in red a start the Server by right clicking the icon and selecting Start Server When the server starts the icon changes to gray Sh Start Chromeleon by selecting Start gt Programs gt Chromeleon gt Chromeleon The Chromeleon main window and the Browser will open Your screen display should resemble Figure 3 4 If the Browser does not open select Browser from the File menu to open it Chromeleo
150. ted to the parallel PC interface or USB port The dongle stores the serial number of a Chromeleon computer NOTE If the software license is managed via a License Server a dongle is not required 1 Plug the dongle into the appropriate port on the computer either the parallel or USB port depending on the type of dongle Tighten the connector screws on a parallel port dongle 2 Ifit is not already running start the Chromeleon Server Monitor select Start gt Programs gt Chromeleon gt Server Monitor The Server Monitor window opens Doc 031879 01 3 03 Installing the Chromeleon Software License 3 Che ck the server status If Chromeleon Server is running idle is displayed the license Key Code was entered before shipping the computer and you can omit the remaining steps in this section Click Close and go on to Section B 5 If Chromeleon Server is running idle Evaluation Mode is displayed see Figure B 4 the license Key Code has not yet been entered If this is the case go on to Step 4 Chromeleon Server Monitor FI F3 Status Close act Chromeleon Server is running idle Evaluation Mode Help Start i Quit Monitor Config Serial No 648 Figure B 4 Server Evaluation Mode 4 Open Chromeleon select Start gt Programs gt Chromeleon gt Chromeleon Doc 031879 01 3 03 B 7 ICS 1000 lon Chromatography System 5 Select File gt Preferences to open the
151. terclockwise until it is loose and then pull the knob straight out of the cavity in the pump head Priming Valve Waste Valve Figure 5 7 Waste and Priming Valves 4 Ifthe O ring is removed with the valve knob in Step 2 pull the O ring off the end of the knob see Figure 5 8 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 IMPORTANT Scratches in the cavity will cause leaks around the base of the knob while the pump is being primed Doc 031879 01 3 03 5 Service Valve Knob O Ring P N 055752 Figure 5 8 Waste Valve or Priming Valve O Ring Replacement 5 Slide a new O ring P N 055752 over the end of the valve 6 Toreinstall the valve containing the new O ring turn the knob clockwise and then tighten fingertight NOTE It is normal to encounter resistance after several rotations of the knob the O ring is being pushed into the cavity of the pump head 7 Turn on the main power switch 8 Open the eluent valve 9 Prime the pump see Section B 14 Doc 031879 01 3 03 5 19 ICS 1000 lon Chromatography System 5 9 Replacing the Conductivity Cell 1 Turn off the ICS 1000 power 2 Open the front door and disconnect the tubing from the CELL IN and CELL OUT fittings see Figure 5 9 View A Loosen the two screws on the cell
152. the Enter key 7 Inthe Unassigned USB Devices box select the ICS 1000 and then click the Assign button The ICS 1000 is now assigned to the timebase see Figure B 11 If you are installing more than one ICS 1000 you can verify the serial numbers for each by checking the label on the component panel 8 Repeat Step 7 if you are adding additional USB devices to this timebase Unassigned Dionex IC USB Devices Detected Assign gt gt Cx Unassian Rest i Gaule Launch Server Configuretionon OK pK emen Figure B 11 ICS 1000 Assigned to a Timebase 9 Click OK to close the dialog box The Server Configuration program window appears B 14 Doc 031879 01 3 03 Setting Up Chromeleon 10 Click the icon next to the server name to expand the folder The timebase you created is displayed see Figure B 12 Server Configuration Chromeleon Server Configuration File Edit View Server Help oe aR amp amar M Sharable Devices H E DEMO 243 1 Figure B 12 Server Configuration with ICS 1000 Timebase ER O 4 3 v 11 To verify that the ICS 1000 is correctly connected to the timebase double click its name under the timebase Click Yes if the following message appears Communication to the device will be stopped Do you want to continue Doc 031879 01 3 03 ICS 1000 lon Chromatography System 12 The ICS 1000 System
153. the manual provided by the hub vendor for complete installation instructions The USB standard limits the USB cable length to 5 meters 16 ft Each IMPORTANT USB device can be separated from the PC by no more than five hubs Thus each USB device can be located no more than 30 meters 32 yds from the PC B 10 Doc 031879 01 3 03 Connecting the Power Cord B 6 Connecting the Power Cord Connect the power cord IEC 320 C13 ordered separately from the main power receptacle on the rear panel to a grounded power source The ICS 1000 power supply is auto sensing so no adjustment is required to select the line voltage SHOCK HAZARD To avoid electrical shock use a grounded receptacle Do not operate the ICS 1000 or connect it to AC power mains without an earthed ground connection gt WARNING The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the ICS 1000 and is easily accessible gt CAUTION Operation at AC input levels outside of the specified operating voltage range may damage the ICS 1000 gt CAUTION DANGER D ELECTROCUTION Pour viter toute lectrocution il faut utiliser une prise de courant avec prise de terre Ne l utilisez pas et ne le branchez pas au secteur C A sans utiliser de branchement mis la AVERTISSEMENT terre gt Le cordon d alimentation principal est utilis comme dispositif principal de d branchement Veillez
154. 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 14 shows the injection valve connections The injection valve is plumbed at the factory with all tubing and fittings for connection to the pump injection port column and waste A 25 uL PEEK sample loop P N 042857 is installed between ports L 1 and L 4 Dionex offers 2 24 Doc 031879 01 3 03 2 Features sample loops in various sizes If necessary the pre installed 25 uL loop can be replaced with a loop that has a different sample injection volume SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP Orange Black TO INJECT Green VALVE P Figure 2 14 Injection Valve Plumbing Doc 031879 01 3 03 2 25 ICS 1000 lon Chromatography System 2 4 5 Column Heater Optional l Figure 2 15 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 and it must be set at least 5 C above the ambient temperature Temperature is monitored via a thermistor mounted in the heater block Setting the temperature to 0 C turns off the column heater If the temperature exceeds 65 C the column heater is shut off and the error message Column heater exceeds safe temperature is displayed
155. the two eluent and the two regenerant lines from the suppressor To remove the suppressor from the component mounting panel slide it up to detach it from the mounting tabs on the panel and then pull it toward you Continue pulling the suppressor out until the yellow connector on the cable inside the ICS 1000 is outside the panel see Figure 5 11 Disconnect the suppressor cable twist the ring on the yellow connector and pull the two connectors apart Yellow Connector Figure 5 11 Removing the Suppressor Connect the cable from the new suppressor to the ICS 1000 cable align the pins on the two connectors and push them together Orient the suppressor with the REGEN OUT fitting on top and the cables to the right Push the cables into the opening in the component panel 5 22 Doc 031879 01 3 03 5 Service 11 12 13 14 Align the top of the suppressor with the guide line printed on the component panel see Figure 5 12 and align the slots on the rear of the suppressor with the tabs on the panel Press the suppressor onto the tabs and then slide it down until it locks into place Pull slightly on the center ofthe suppressor to verify that it is securely fastened Note Some suppressors require more force to secure them onto the tabs Connect the two eluent and two regenerant lines to the new suppressor Close the ICS 1000 front door 1 Suppressor Mounting Tabs
156. they may 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 Insufficient time between sample injections Wait until the previous sample has been completely eluted before making another injection Insufficient flush between samples Flush the sample loop with at least 10 loop volumes of deionized water or sample between sample injections Incorrect or contaminated standards Remake standards Incorrect or contaminated eluent Remake the eluent according to the instructions in the column manual Column manuals are included on the Dionex Reference Library CD ROM P N 053891 Install or replace the end line filter on the end of the deionized water line see Section 3 4 3 4 16 Doc 031879 01 3 03 4 Troubleshooting Malfunctioning injection valve 1 Rebuild the injection valve see Section 5 4 2 Ifthe valve leak persists contact Dionex for assistance 4 9 Nonreproducible Peak Height or Retention Time Column overloading Dilute the sample see Section 3 9 Liquid leaks Locate and eliminate the leaks see Section 4 2 Incomplete or imprecise filling of the sample loop 1 Fill the sample loop until excess sample exits the waste line 2 Inspect the 1 cc syringe P N 016388 and replace if damaged Pump not primed properly Prime the pump see Section B 12 4 10 Abnormal R
157. ting 5 7 Power Turning on 3 3 B 12 Power cord 5 30 B 11 Power receptacle 2 8 B 11 Power requirements A 1 Power up conditions 3 3 Pressure Limit 4 7 Pump operating specifications A 2 System 4 6 4 7 Pressure ripple A 2 Pressure slope calibration error 4 5 Pressure transducer 2 5 2 23 Leaking 4 10 System backpressure 2 23 Pressurizing Eluent reservoir B 48 Priming 3 9 5 29 B 36 B 38 Pump is out of prime 4 12 With a syringe B 36 With isopropyl alcohol 5 29 With the Prime button B 38 Priming valve Opening 2 22 O ring replacement procedure 5 18 Printing E 1 Processing samples 3 2 3 18 3 19 Automatically batch 3 2 3 19 Manually 3 2 3 18 Product warranty 5 1 Program time 2 15 Programs Chromeleon 2 11 2 15 3 16 3 19 Run time 2 15 Pulse damper 2 10 2 23 Pump 2 21 Flow rate 2 5 Leaks 4 10 Operating pressure A 2 Over pressure alarm 4 6 Primary pump head 2 21 Priming 3 9 B 36 Priming problems 4 11 Secondary pump head 2 22 Troubleshooting 4 13 Under pressure alarm 4 7 Pump check valve leaking 4 9 Pump components 2 21 Pump degas See Vacuum degas assembly Pump head waste valve Leaking 4 10 O ring replacement procedure 5 18 Pump heads 5 11 Pump motor lost control alarm 4 5 Pump pressure hardware error 4 6 Pump priming valve O ring replacement procedure 5 18 Pump specifications Flow rate A 2 Operating pressure A 2 Type A 2 Index 6 Doc
158. ting plug P N 042772 on the outlet check valve Tighten the plug 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 Push the piston into the head This should hydraulically unseat the seal from the head Remove the piston and pull off the seal NOTE If the piston seal is not removed make sure the 10 32 fitting plug s are tight and add more water Make sure the head contains no air bubbles and then repeat Steps 2 and 5 Remove the 10 32 fitting plug s Installing the New Piston Seal 1 Open the priming valve knob primary pump head or waste valve knob secondary pump head by turning the knob one quarter to one half turn counterclockwise Push the piston through the spacer and then through the new seal Insert the piston and seal into the pump head until the seal makes contact with the bottom of the counterbore NOTE If necessary lubricate the seal with a small amount of isopropyl alcohol to facilitate insertion To seat the seal push down on the spacer until it is flush with the head A clicking sound indicates that the seal is correctly seated 4 Close the priming valve knob or waste valve knob Doc 031879 01 3 03 5 Service 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
159. tituting non Dionex parts may impair ICS 1000 performance thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information 5 1 Diagnostic and Calibration Procedures Diagnostic and calibration procedures are performed from the Chromeleon Wellness Panel see Figure 5 1 For an overview of the Wellness Panel features see Section 5 1 1 For instructions on performing calibration and diagnostic procedures see the following sections e Calibrating the Conductivity Cell Section 5 1 2 Calibrating the Flow Rate Section 5 1 3 Calibrating the Vacuum Degas Assembly Section 5 1 4 Doc 031879 01 3 03 5 1 ICS 1000 lon 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 Open the Chromeleon Browser and expand the Dionex Templates folder Expand the Panels folder and then the Wellness folder In the right pane of the Browser window double click ICS 1000 1500 2000 Wellness user pan The Wellness Panel appears Open the Control menu and click the name of the ICS 1000 timebase at the bottom of the menu This connects the Wellness Panel to the ICS 1000 and enables the controls on the panel g wellness Panel ICS 1000 AMAR E B x System Statu
160. to sensing and requires no voltage adjustment Two 3 15 amp fast blow IEC 127 fuses P N 954745 Height 56 1 cm 22 1 in Width 22 4 cm 8 8 in Depth 53 3 cm 21 0 in 30 kg 66 Ib lt 52 db at A WEIGHTING setting A 3 Environmental Operating Temperature Humidity Operating Pressure 4 C to 40 C 40 F to 104 F 5 to 95 relative humidity noncondensing 35 MPa 5000 psi maximum liquid path tubing valve columns etc Doc 031879 01 3 03 ICS 1000 lon Chromatography System A 4 Front Panel Power LED On when power is present off when no power is present Inject Valve Indicate the position of the inject valve LEDs Alarm LED Indicates an alarm state Status LEDs Indicate instrument status A 5 Pump Type Dual piston in series variable speed 100 uL per revolution Flow Rate Settable range 0 00 to 5 00 mL min in 0 01 increments Optimal Operational Range 0 4 to 2 0 mL min Flow Accuracy lt 1 of set value within the optimal operational range Flow Precision lt 0 2 Operating 35 MPa 5000 psi maximum Pressure High Pressure 0 7 to 34 4 MPa 100 to 5000 psi Limit Low Pressure 0 0 to 33 7 MPa 0 to 4900 psi Limit Delay Volume 800 uL Pressure Ripple lt 1 at 13 8 MPa 2000 psi and 1 0 mL min A 2 Doc 031879 01 3 03 A Specifications A 6 Detector Range Temperature Compensation Cell Drive Linearity 0 to 3200 uS digital output
161. to the front of the ICS 1000 Doc 031879 01 3 03 ICS 1000 lon Chromatography System 2 1 3 Component Panel Figure 2 4 shows the user accessible components installed on the component panel behind the ICS 1000 front door Eluent Valve Leak Sensor Pump Heads Pressure Transducer Injection Valve Columns Connector for optional column heater 60 COCC8 6 Suppressor DS6 Conductivity Cell Mounting brackets for a second suppressor D Tubing Chase 2 Figure 2 4 ICS 1000 Component Panel 2 4 Doc 031879 01 3 03 2 Features Eluent Valve The eluent valve controls the flow from the eluent reservoir It opens automatically when the pump is running and closes when the pump is off Leak Sensor The leak sensor is installed in the drip tray at the bottom of the component panel If liquid accumulates in the tray an error message is reported in Chromeleon and the Alarm LED flashes Pump Heads The ICS 1000 includes a serial isocratic dual head pump The flow rate can be set to 0 00 and to between 0 05 and 5 0 mL min However for optimum performance set the flow rate to between 0 4 and 2 0 mL min Setting the flow rate to 0 00 turns off the pump See Section 2 4 3 for details about the pump Pressure Transducer The pressure transducer measures the system backpressure Injection Valve The injection valve is a six port electrically activated valve A 25 uL sample lo
162. tography System 2 4 4 Injection Valve 2 24 2 4 5 Column Heater Optional 2 26 2 4 6 Suppressor 2 27 2 4 7 DS6 Heated Conductivity Cell 2 27 3 Operation and Maintenance 3 1 3 2 3 3 3 4 3 5 3 6 3 7 3 8 3 9 Operation Overview aiaa t a eS sapere eeu eee inde 3 1 Power Up the System 3 3 Sab CBEGIEIeOIE en tential non gta aat adc p VCI do 3 4 Set Up the Eluent Reservoir 3 6 3 4 1 Prepare the Eluent 3 6 3 42 Degas the Eluent 3 6 SAS o Filterthe E ueh ss s a asad eo AL gna Pula COPA RS 3 7 344 PAR Reservo Sucks oe ea Sone UU Sore RAs ORCI AL 3 8 34 3 Set te El ent Leyel bas aq adco quete S aute Mme 3 8 3 4 6 Connect the ReServolt res sese apes Sot pde Ua ete ES 3 8 Cheek All Connections ressens o Ra ac vac eR Ic epi 3 9 Prime the Pump 3 9 Set System Operating Conditions 3 10 Equilibrate the System and Verify Operational Status 3 11 Prepare Samples ainsi niet tV ae y entem 3 12 3 9 1 Collecting and Storing Samples 3 12 3 92 Pretreating Samples 3 12 3 93 Diluting Samples 3 13 Doc 0
163. uggest how to optimize instrument performance etc Doc 031879 01 3 03 ICS 1000 lon Chromatography System 1 3 2 Safety Labels The ICS 1000 meets EN 61010 1 1993 safety CAN CSA C22 2 No 1010 1 92 safety UL 3101 1 10 93 safety EN 50082 1 1992 susceptibility EN 55011 1991 emissions The TUV GS C US Mark safety labels and the CE Mark label on the ICS 1000 attest to compliance with these standards The symbols below appear on the ICS 1000 or on ICS 1000 labels A Alternating current D Protective conductor terminal earth ground Power supply is on Power supply is off Doc 031879 01 3 03 2 Features This chapter describes key ICS 1000 features and introduces the Chromeleon user interface 2 4 Operating Features 2 1 1 Front Panel Figure 2 1 illustrates the front panel of the ICS 1000 Status LEDs Power LED Injection Port Figure 2 1 ICS 1000 Front Panel Injection Port The sample to be analyzed can be injected manually into the injection port using a syringe For automated sample injection the ICS 1000 must be connected to an autosampler For more information about sample injection see Section 3 10 LEDs The status LEDs see Figure 2 2 indicate the status of various system functions See Table 2 1for a description of each LEDs function The power LED indicates whether the ICS 1000 power is on Doc 031879 01 3 03 2 1 ICS 1000
164. ugh the separator column the sample ions are separated In the ICS 1000 the mode of separation is called ion exchange This is based on the premise that different sample ions migrate through the IC column at different rates depending upon their interactions with the ion exchange sites 4 Suppression e After the eluent and sample ions leave the column they flow through a suppressor that selectively enhances detection of the sample ions while suppressing the conductivity of the eluent 5 Detection e A conductivity cell measures the electrical conductance of the sample ions as they emerge from the suppressor and produces a signal based on a chemical or physical property of the analyte 6 Data Analysis e The conductivity cell transmits the signal to a data collection system e The data collection system for the ICS 1000 this is Chromeleon identifies the ions based on retention time and quantifies each analyte by integrating the peak area or peak height The data is quantitated by comparing the sample peaks in a chromatogram to those produced from a standard solution The results are displayed as a chromatogram and the concentrations of ionic analytes can be automatically determined and tabulated Doc 031879 01 3 03 1 3 ICS 1000 lon Chromatography System 1 2 Overview of the ICS 1000 The ICS 1000 is an integrated ion chromatography system containing a pump injection valve column heater and conductivity detector
165. workbench Inspect the ICS 1000 for any shipping damage Two or more persons should lift the ICS 1000 which weighs 30 kg 66 Ib Lift the ICS 1000 only from each side of the cabinet bottom Lifting from the front door will damage the door hinges Au moins deux personnes peuvent soulever le ICS 1000 il p se 30 kg 66 Ib Ne soulevez le ICS 1000 que par chaque c t du fond de l armoire Son soul vement par la porte du panneau avant endommagera les charni res de la porte Der ICS 1000 wiegt ber 20 kg Daher sollte das Ger t nur von zwei oder mehr Personen angehoben werden Greifen Sie dazu an beiden Seiten unter das Ger t Heben Sie den Autosampler nicht an der Vordert r an da dadurch die T rangeln besch digt werden k nnten Doc 031879 01 3 03 B 3 ICS 1000 lon Chromatography System B 2 1 Unpacking the Computer North America only 4 NOTE These instructions assume that Chromeleon software and the software license were installed on the computer before shipping Remove the central processing unit CPU keyboard mouse and all documentation from the computer box and place these items on a workbench Remove the monitor from its box and place it on the workbench Follow the instructions in the computer installation guide to hook up the monitor mouse keyboard and CPU Go on to Section B 4 Installing the Chromeleon Software License B 2 2 Unpacking the Computer outside North America 1 R
166. x d 2 DAMPER e Ui 08 dT T 3 N 2 oO IN Or s L OUT i PY PRESS JQ A XDUCER OX VALVE Lu D 1 F lt OUT N ee ee 9 PUMP PUMP HEAD HEAD N G WASTE IN IN OUT Figure 5 2 ICS 1000 Flow Schematic NOTE The numbers on the flow schematic indicate the order in which liquid flows through the system components 5 8 Doc 031879 01 3 03 5 Service 5 3 Replacing Tubing and Fittings The ICS 1000 is plumbed with the tubing and tubing assemblies listed below Tubing Size and Type Color 0 125 mm 0 005 in ID PEEK Red P N 044221 0 25 mm 0 010 in ID PEEK Black P N 042690 0 50 mm 0 020 in ID PEEK Orange P N 042855 0 75 mm 0 030 in ID PEEK Green P N 044777 1 58 mm 0 062 in ID Teflon amp Clear P N 014157 25 uL sample loop Orange P N 042857 Used For Connection from pump pulse damper to pressure transducer Connections between other system components Connection from injection port to injection valve Connection from injection valve to waste Connection from pump to degas or eluent reservoir pump waste Connection between ports L 1 and L 4 on the injection valve e 10 32 fittings P N 043275 and ferrules P N 043276 are used for most tubing connections For tightening requirements refer to nstallation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Dionex Reference Library CD ROM P N 053891 e j 8
167. y System 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 It is then pushed through the pressure transducer which measures the system pressure From there it is pushed through a pulse damper which smooths minor pressure variations from the pump to minimize baseline noise The eluent then flows into the injection valve G After sample is loaded into the sample loop and the injection valve is toggled to the Inject position eluent passes through the sample loop If the optional column heater is installed the eluent sample mixture is pumped through the heat exchanger which heats the mixture to the column heater temperature The mixture then goes to the guard and separator columns and through the suppressor From the suppressor the mixture flows through the cell where the analytes are detected A digital signal is sent to Chromeleon software Analog output can be collected simultaneously Finally the mixture flows out of the cell and is recycled back into the suppressor where it is used as the water source for the regenerant chamber Flow is then routed to waste P 2 10 Doc 031879 01 3 03 2 Features 2 3 The Chromeleon Interface NOTE This section provides a brief overview of the Chromeleon interface For details refer to the Chromeleon Help or user s manual Chromeleon software is used for remot
168. y issuing direct control commands from the Chromeleon control panel or by including the commands in a control program Figure C 4 shows an example relay program command for controlling an AS40 autosampler 812A Production Test Chromatogram Commands E d Is m Production Test Chromatogram ppr essor arren 3 2 300 0 000 15 000 Flow 1 50 Pump ECD Relay 1 Closed Duration 138 00 For AS40 injection Relay 1 turned on to start Relay 1 turned off after the AS40 Load cycle and 138 seconds Pump ECD Autozero ECD l Acqon Pump InjectValve InjectPosition Duration 30 00 load the sample loop ECD l Acqoff Figure C 4 Example Program for AS40 Control Doc 031879 01 3 03 C TTL and Relay Control C 3 Example Setup for Stand Alone Operation This section describes an example setup for stand alone operation operation without Chromeleon software with an AS50 autosampler and a third party analog to 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 Verify the AS50 Configuration Refer to Section B 17 1 to verify that the AS50 meets the configuration requirements for use with the ICS 1000 Connect the AS50 Autosampler Follow the instructions in Section B 17 2 to connect the AS50 autosampler to the IC
169. y software produces a chromatogram a plot of the detector output vs time The chromatography software converts each peak in the chromatogram to a sample concentration and produces a printout of the results Doc 031879 01 3 03 1 1 ICS 1000 lon Chromatography System A typical IC analysis consists of 6 stages see Figure 1 1 1 Eluent Delivery Eluent Separator Column 3 Separation Pump Guard Column Injection Valve Sample 2 Sample Injection 6 Data Analysis Conductivity 5 Detection Cell Suppressor 4 Suppression Sample Loop Figure 1 1 lon Analysis Process 1 Eluent Delivery Eluent a liquid that helps to separate the sample ions carries the sample through the ion chromatography system The ICS 1000 is an isocratic delivery system This means that the eluent composition and concentration remain constant throughout the run 2 Sample Injection The liquid sample is loaded into a sample loop either manually or automatically if an automated sampler is installed When triggered the ICS 1000 injects the sample into the eluent stream 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 Doc 031879 01 3 03 1 Introduction 3 Separation e As the eluent and sample are pumped thro

ICS-1000 Ion Chromatography System Operator`s Manual

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