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Dionex ICS-1600 Ion Chromatography System Operator`s Manual

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1. Datasource 11 06 27 AM Pump ECD Please verify the solvent and waste level values Sequence 11 06 28 AM Manually acquired samples will be stored Sample temporarily in sequence SEQ ACMADLER localSystem 2Wmnanual Program 11 06 28 AM Chromeleon server version 6 80 SR6a Build Elapsed Program Time CS 1600 Syste Total Program Time Connected _ Startup Shutdown Show Plot 20 0 ul from Pos 1 3 00 Figure 3 4 Dionex ICS 1600 Control Panel on the Chromeleon Panel Tabset Doc 065290 03 10 12 43 Dionex ICS 1600 lon Chromatography System 3 4 Set Up the Eluent Reservoir 3 4 1 3 4 2 NOTE If you plan to operate the system in the RFIC ER mode disregard the instructions here Follow the instructions provided with your RFIC ER Installation Kit to set up the RFIC ER eluent reservoir 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 Dionex ICS 1600 To ensure optimal pump performance observe the following precautions 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 The optional vacuum degas assembly provides prog
2. C N INFORMATION V MODULE SETUP Na JO RU RR EIUS INPUT OUTPUT N d f DIAGNOSTIC j I These pages can be opened from the menu or the Home page Pump Calibration FLOW RATE la x DEGAS Detector Calibration MV CONDUCTIVITY CELL vs ELECTRIC CONDUCTIVITY CELL COLUMN HEATER CAL VALUES Me Figure B 6 Overview of Dionex ICS 1600 Touch Screen Pages Doc 065290 03 10 12 Dionex ICS 1600 lon Chromatography System B 4 Home Page s Pump Orsi Limit 1000 4000 Edit Field Flow Rate Command UTE selected _ Pine Eluent Level Total 146 99 pS Status Field Autozero Cell Heater Load Elapsed Time Type None MMS OFF Command Button unselected 0 00 L Remote Mode PLOT STATUS c HOME Figure B 7 Dionex ICS 1600 Touch Screen Home en Page B 4 1 Home Page Pump Controls Orsi Limit 1000 4000 Flow Rate mL min Eluent Level L Pump Pressure Display The HOME page indicates the current pressure reading from the pressure transducer The pressure unit can be set to psi the factory default MPa or bar see Section B 7 1 The minimum and maximum pressure limits are displayed below the current pressure reading If the pressure reading goes outside these limits the pump is stopped and an error message appears in the
3. 99 5 5 Replacing an Auxiliary Valve Pod 0000 c eee eee 100 5 6 Cleaning and Replacing the Pump Check Valves 103 5 7 Replacing a Pump Piston Seal and Piston Rinse Seal 105 5 8 Replacing a Pump Piston 0 0 eee eee eee ee 109 5 9 Replacing the Waste Valve or Priming Valve O Ring 110 Doc 065290 03 10 12 Contents 5 10 Replacing the Conductivity Cell 0 0 00 ee eee eee 112 5 11 Replacing the Suppressor 0 0 0 cee eee ee eee ee 115 5 12 Replacing the Column Heater sese 116 5 13 Replacing the Column Heater Heat Exchanger 119 5 14 Replacing the Eluent Valve eeleleeeeee 120 5 15 Replacing the Leak Sensor 0 0 0 eee eee eee 122 5 16 Priming the Pump 0 0 cee cece I 123 5 16 1 Priming the Eluent Lines with a Syringe 123 5 16 2 Priming with the Prime Button 125 5 17 Priming the Pump with Isopropyl Alcohol 4 126 5 18 Changing Main Power Fuses 0 000 cece eee eee eee 127 A Specifications 129 AJ Electrical iresenbreeessceeseskEekeE SPP d pes 129 A 2 Physical ore iorra po S r p ER pe Were ne e Gauge anaes EE E des 129 AS Environmental sc 2622s rue bU eV Pers 130 AA brontPanel 5 mercede et eR ae ear tread 130 A 5 Analytical Pump and Fluidics 0 0 0c eee eee eee 130 A 6 Eluent
4. Figure 5 7 Dionex ICS 1600 Flow Schematic Standard Configuration 96 Doc 065290 03 10 12 5 Service E ep ELUENT ERD OUT OUT OUT O IN PUMP d IN 1 DEGAS COND e optional CELL PULSE DAMPER UJ U 9 IN ER2 e ON tis es gt C EHE i SUPPRESSOR SAMPLE z s 2 a o o brd tc W o VALVE 3 PUMP PUMP ij HEAD HEAD IN WASTE WASTE Figure 5 8 Dionex ICS 1600 Flow Schematic RFIC ER Mode Doc 065290 03 10 12 97 Dionex ICS 1600 lon Chromatography System 5 3 Replacing Tubing and Fittings The Dionex ICS 1600 is plumbed with the tubing and tubing assemblies listed below Tubing Size and Type Color Used For 0 125 mm 0 005 in ID PEEK Red Connection from pump pulse damper P N 044221 to pressure transducer 0 25 mm 0 010 in ID PEEK Black Connections between other system P N 042690 components 0 50 mm 0 020 in ID PEEK Orange Connection from injection port to P N 042855 injection valve 0 75 mm 0 030 in ID PEEK Green Connection from injection valve to P N 044777 waste 1 58 mm 0 062 in ID PTFE Clear Connection from pump to degas or P N 014157 eluent reservoir pump waste 25 uL sample loop Orange Connection between ports L 1 and P N 042857 L 4 on the injection valve e The ER Tubing Kit P N 070061 contains the four pieces of tubing required for connections from the RFIC ER columns to the c
5. IN WASTE 4 PRESS XDUCER z 5 l Q o c E c amp i oO WASTE OUT mE Figure 2 12 Dionex ICS 1600 Flow Schematic RFIC ER Mode Doc 065290 03 10 12 25 Dionex ICS 1600 lon Chromatography System 2 3 2 3 1 Chromeleon and Chromeleon Xpress The Dionex ICS 1600 is controlled by a PC configured with Chromeleon Chromatography Management System or Chromeleon Xpress Chromeleon Chromatography Management System provides complete instrument control data acquisition and data management Chromeleon Xpress provides real time control and monitoring of instruments but does not include data management capabilities The Panel Tabset The Chromeleon and Chromeleon Xpress panel tabset provides a centralized location for controlling system functions A panel tabset for a Dionex ICS 1600 system typically includes the following Control panels e A Dionex ICS 1600 Control panel see Figure 2 13 provides access to Dionex ICS 1600 functions The label on the tab for this panel is the name of the timebase in which the Dionex ICS 1600 is configured Ft A Tim Pump Settings Settings Injecto Load E _Injector Settings Settings 7 Column Heater Temperature 35 0 C _ Heater Settings _ Heater Settings U 0 025 uS Suppressor Off oma Detector Setti
6. option to select it with pump SUPPRESSOR M 2 1 2 Top Cover Figure 2 7 illustrates the top cover of the Dionex ICS 1600 PW uli Eluent TE Reservoir Figure 2 7 Dionex ICS 1600 Top View Figure 2 6 Suppressor Page Selecting an Option Reservoir Storage The Dionex ICS 1600 top cover has room for up to three 2 L plastic reservoirs P N 044129 or one 4 L plastic reservoir P N 039164 Tubing Chase The tubing chase under the top cover routes tubing to the front of the Dionex ICS 1600 Doc 065290 03 10 12 15 Dionex ICS 1600 lon Chromatography System 2 1 3 Component Panel Figure 2 8 shows the user accessible components installed on the component panel behind the Dionex ICS 1600 front door Pressure Transducer Leak Sensor Pump Heads Injection Valve Auxiliary Valve Optional DS6 Conductivity Cell Suppressor Column Heater and Columns Eluent Valve Mounting Brackets for Second Suppressor Screen Adjustment Knob under display eee cceoeococooceo Tubing Chase 2 Figure 2 8 Dionex ICS 1600 Component Panel 16 Doc 065290 03 10 12 2 Features Pressure Transducer The pressure transducer measures the system backpressure Leak Sensor The leak sensor is installed in the drip tray at the bottom of the component panel If liquid accumulates in the tray an error message is logged in the Chromel
7. Contaminated or degraded sample Take appropriate precautions when preparing and storing samples to prevent contamination and degradation see Section 3 9 Contaminated column 1 Clean the column as instructed in the column manual Column manuals are included on the Thermo Scientific Reference Library DVD P N 053891 2 If cleaning is unsuccessful replace the column 4 12 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 Doc 065290 03 10 12 79 Dionex ICS 1600 lon Chromatography System 4 13 installed and the screws tightened an electronics connector on the cell plugs into a receptacle inside the Dionex ICS 1600 No flow from pump This condition has several possible causes see Section 4 5 and Section 4 6 for details Cell electronics malfunctioning Use the Chromeleon Wellness Panel diagnostics to test the electronics see Section 5 1 and the Chromeleon Help for instructions If the variance reading is outside the tolerance range less than 1 uS the electronics are malfunctioning Contact Thermo Fisher Scientific for assistance The Dionex ICS 1600 electronics cannot be serviced by the user High 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
8. Column heater heat exchanger 0 125 mm 0 005 in ID tubing for use with 2 mm columns Column heater cover assembly Microbore tubing kit Relay TTL 12 position connector plug Twisted pair of wires RFIC ER Kits RFIC ER Anion Startup Kit ICS 1100 ICS 1600 RFIC ER Anion Consumables Kit ICS 1100 ICS 1600 RFIC ER Cation Startup Kit ICS 1100 ICS 1600 RFIC ER Cation Consumables Kit ICS 1100 ICS 1600 ER Tubing Kit Miscellaneous IEC 127 fast blow fuses rated 3 15 amps USB cable 5 m 16 ft External USB hub 178 Doc 065290 03 10 12 D Reordering Information Part Number ltem Preventive Maintenance Kits 057954 Dionex ICS 1600 Preventive Maintenance Kit 060581 Dionex AS Preventive Maintenance Kit 055647 Dionex AS DV Preventive Maintenance Kit Doc 065290 03 10 12 179 Dionex ICS 1600 lon Chromatography System 180 Doc 065290 03 10 12 E 1 E 2 E 3 E 4 E 5 E FAQ How do I hook up an autosampler For instructions on how to connect the Dionex ICS 1600 to an autosampler refer to the Dionex ICS 1600 installation instructions Also refer to the autosampler operator s manuals which are included on the Thermo Scientific Reference Library DVD P N 053891 How do I print Click the Print toolbar button in Chromeleon 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 7 for pump flo
9. Removed Doc 065290 03 10 12 119 Dionex ICS 1600 lon Chromatography System 9 10 11 Remove the plastic backing from the new heat exchanger P N 059979 with 0 25 mm 0 010 in ID tubing P N 060943 with 0 125 mm 0 005 in ID tubing and press the heat exchanger onto the heater Replace the screws removed in Step 8 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 14 Replacing the Eluent Valve l 2 3 Turn off the power to the Dionex ICS 1600 Open the Dionex ICS 1600 front door To prevent an eluent leak during the valve replacement procedure disconnect the eluent line from the reservoir cap or plug the line on the left side of the valve with a coupler P N 039056 and a plug P N 037268 after you disconnect the liquid line from the valve in Step 4 Disconnect the two liquid lines connected to the eluent valve see Figure 5 25 Unscrew and remove the two screws that attach the Disconnect valve to the component panel see Figure 5 25 Save the screws TS Figure 5 25 Eluent Valve 120 Doc 065290 03 10 12 5 Service 6 Pullthe valve straight out from the component panel and begin pulling the attached cable out of the opening in the panel 7 The cable is connected to a matching cable inside the Dionex ICS 1
10. f Toensure that the new values are recorded in the Dionex ICS 1600 memory do not turn off the Dionex ICS 1600 power for at least 1 minute after downloading Doc 065290 03 10 12 113 Dionex ICS 1600 lon Chromatography System To calibrate the cell on the Dionex ICS 1600 touch screen DIAGNOSTIC page a Go to the DIAGNOSTIC page and touch Electric Conductivity Cell b On the ELECTRIC CONDUCTIVITY CALIBRATION page see Figure 5 19 touch Run Offset Cal ELECTRIC CONDUCTIVITY CALIBRATION Total Conductivity 0 000 pS Cell Constant Wait until this calibration is done before doing slope cal Run Slope Cal WARNING THIS WILL ERASE THE PRIOR SLOPE CALIBRATION AND STORE A NEW VALUE Fine Offset 0 00000000 Slope 0 02483527 X 1075 Medium Offset 0 00000000 Slope 0 39736432 X 1075 Coarse Offset 0 00000000 Slope 1 66264525 X 1075 o b pe M Figure 5 19 Electric Conductivity Calibration Page c When the offset calibration is complete touch Run Slope Cal d Touch the Cell Constant field and enter the value printed on the front of the cell e To ensure that the new calibration values are recorded in the Dionex ICS 1600 memory do not turn off the Dionex ICS 1600 power for at least 1 minute f Record the new calibration values in the Chromeleon Wellness database To do this open the Wellness Panel see Section 5 1 1 and click Upload under Update Wellness Database 114 Doc 065290 03 10 12 5 Servi
11. which smooths minor pressure variations from the pump to minimize baseline noise The eluent then flows through the ERI column Q and into the injection valve After sample is loaded into the sample loop G 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 9 and through the suppressor QD From the suppressor the mixture flows through the cell E 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 through the ER2 column B and is then recycled back into the suppressor From the suppressor flow moves to the ER3a and ER3b columns which remove contaminants from the eluent The ERC 10 B monitors the eluent for gas and shuts down the pump if the gas exceeds a pre defined limit The output from the ERC 10 is recycled back to the eluent bottle 24 Doc 065290 03 10 12 2 Features o T ELUENT ER3b S r OUT I AN HEAT EXCHANGER SAMPLE og gt v m D IN N a O pump 1 IN 9 DEGAS COND 9 e optional CELL E Q 5 2 PULSE 8 E R amon ER1 Le VALVE 3 PUMP PUMP t HEAD HEAD
12. A Specifications A 13 Suppressors Chemical Suppression Displacement Chemical Regeneration Electrolytic Suppression Current Control Range Salt Converter Dionex AMMS ICE Carbonic Acid Removal for Anions Non Suppressed Suppressor Wear Parts Suppression Capacity 2 mm and 4 mm anion and cation membrane suppression bed types 2 mm and 4 mm anion and cation membrane suppression bed types e Self Regenerating 2 mm and 4 mm anion and cation both membrane and MonoDisk suppression bed types available e Self Regenerating with External Water Mode 2 mm and 4 mm anion and cation both membrane and MonoDisk suppression bed types available SRS 4 mm 0 to 300 mA in 1 mA increments SRS 2 mm 0 to 100 mA in 1 mA increments AES 0 to 150 mA in 1 mA increments CMD 0 to 500 mA in 1 mA increments SRN 0 to 500 mA in 1 mA increments 2 mm and 4 mm versions available 2 mm and 4 mm versions available ASRS 300 with CRD 200 for hydroxide eluents ASRS 300 with CRD 300 for carbonate eluents Supported None peristaltic pump and inline filters not required Anion SRS 300 4 mm 200 peq min Cation SRS 300 4 mm 110 ueq min Anion SRS 300 2 mm 50 ueq min Cation SRS 300 2 mm 37 5 ueq min Anion MMS 300 4 mm 150 peq min Cation MMS 300 4 mm 150 ueq min Anion MMS 300 2 mm 37 5 ueq min Cation MMS 300 2 mm 37 5 ueq min Anion AES 25 ueq min Cation AES 25 ueq min Doc 065290 03 1
13. 065290 03 10 12 123 Dionex ICS 1600 lon Chromatography System Secondary Pump Head M Waste Valve close gt Primary Pump Head 10 mL Syringe by Priming Valve P N 079803 open Figure 5 30 Priming the Eluent Lines 3 Open the priming valve by turning it one quarter to one half turn counterclockwise 4 On the Dionex ICS 1600 Control panel in Chromeleon click the Pump Settings button The Pump Settings window opens see Figure 3 6 5 Under Eluent Flow Valve click the Open button 6 Draw the syringe back to begin pulling eluent through the flow path 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 7 After priming the lines thoroughly close the priming valve Do not overtighten 124 Doc 065290 03 10 12 5 Service 5 16 2 Priming with the Prime Button NOTE Perform this procedure after priming the eluent lines see Section 5 16 1 1 Check that the priming valve on the primary pump head is closed see Figure 5 31 Secondary Pump Head Waste Valve ae open N 4X LAG Primary un Pump Head Priming Valve close Figure 5 31 Priming the Pump 2 Open the waste valve on the secondary pump head by turning the knob one quarter to one half turn counterclockwise see Figure 5 31 Opening the
14. 55 56 Data acquisition 55 Data analysis description 3 Data rise time 157 158 Decibel level 129 Default panel tabset 27 Degas tubing assembly See Vacuum degas assembly Degas calibration failed alarm 64 Degassing eluents 28 44 Detection description 3 Detector controls on Home page 146 See also Conductivity cell Detector page 157 Setting analog out options 159 Setting the data rise time 158 Detector specifications Auto offset 132 Calibration 132 Cell drive 132 Control and data evaluation 132 Linearity 132 Range 132 Resolution 132 Temperature compensation 132 Diagnostic pages 162 Diagnostics 85 Dimensions 129 Dionex 42 Direct software control 27 Drip tray 17 DS6 Heated Conductivity Cell See Conductivity cell Duty cycle 29 155 E Elapsed time 146 148 Electrical specifications Fuses 129 Main power 129 Eluent Aqueous 59 74 Degassing 28 Delivery process 2 Filtering 45 Preparing 44 When to remake 182 Eluent bottle See Eluent reservoir Eluent level 45 145 Eluent reservoir Connecting 47 Monitoring liquid level in 45 145 Storage on top cover 15 Eluent valve 18 155 Replacing 120 End line filter See Filter end line Environmental specifications 130 Equilibration time 49 Doc 065290 03 10 12 Index 3 Dionex ICS 1600 lon Chromatography System ER Controller ERC 10 19 37 Error messages 63 70 Audit Trail description 61 Column heater exceed
15. 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 48 Doc 065290 03 10 12 3 Operation and Maintenance 3 8 Set or verify system operating parameters from either the Chromeleon Control panel or from the touch screen HOME page 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 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 PY NF Verify that the column heater is set to the correct value Automatically Turning on the Suppressor You can set up the Dionex ICS 1600 to turn on the suppressor automatically when the pump is turned on To do this select the Automatically turn on with pump option from the SUPPRESSOR page The suppressor is always turned off automatically when the pump is turned off Equilibrate the System and Verify Operational Status NOTE You can monitor system functions conductivity pressure cell temperature etc from the Chromeleon Control panel or from the touch screen HOME page 1 Allow the sy
16. see Section 2 4 4 The ELAPSED TIME field displays the amount of time since the last injection B 4 4 Home Page Detector Controls Detector Conductivity Readings 157 67 uS The offset conductivity is displayed in large numbers above Total 1258 14 pS the total conductivity The offset conductivity is the total l conductivity minus the current offset To determine the offset allow the system to equilibrate after startup At equilibration the conductivity reading is the background conductivity the eluent conductivity before sample injection Touch Autozero to zero the conductivity and offset this background reading from the total reading NOTE You can reverse the conductivity display to show the total conductivity in large type with the offset conductivity below it in small type Select this option on the MODULE SETUP page see Section B 11 Cell Heater Controls Cell Heater The temperature of the cell can be set to between 30 C and o C 55 C but must be at least 7 C above the ambient Off temperature To set the temperature touch the Cell Heater field and enter the desired temperature on the number pad 146 Doc 065290 03 10 12 B Touch Screen Operation To turn off the cell heater set the temperature to 0 The display to the right of the temperature setting indicates the heater status cell temperature is at equilibrium T cell temperature is rising 4 cell temperature is falling Off cell heater i
17. 065290 03 10 12 109 Dionex ICS 1600 lon Chromatography System 5 9 Replacing the Waste Valve or Priming Valve O Ring A damaged O ring causes leakage around the base of the waste valve or priming valve knob 1 Close the eluent valve from the Dionex ICS 1600 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page 2 Turn off the main power switch to ensure that you do not unintentionally start the Dionex ICS 1600 3 To remove the waste valve or priming valve from the pump head see Figure 5 15 turn the knob counterclockwise until it is loose and then pull the knob straight out of the cavity in the pump head Priming Valve Figure 5 15 Waste and Priming Valves 110 Doc 065290 03 10 12 5 Service 4 Ifthe O ring is removed with the valve knob in Step 3 pull the O ring off the end of the knob see Figure 5 16 If the O ring is not removed with the valve knob insert a thin object for example the bent end of a paper clip into the cavity in the pump head and carefully pull out the O ring Do not scratch the cavity Scratches in the cavity will cause leaks around the base of the knob IMPORTANT while the pump is being primed Valve Knob O Ring P N 055752 Figure 5 16 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
18. 104 Doc 065290 03 10 12 5 Service 5 7 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 Direct the flow to waste by opening the waste valve on the secondary pump head see Figure 5 15 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 Dionex ICS 1600 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page To prevent contamination of pump parts put on a pair of rubber gloves before disassembling the pump head Removing the Head and Piston 1 Turn off the main power switch to ensure that you do not unintentionally start the Dionex ICS 1600 2 Disconnect all tubing connections to the pump head 3 Locate the open end wrench P N 014605 provided in the Dionex ICS 1600 Ship Kit P N 067110 Use the wrench to remove the two acorn nuts see Figure 5 12 from the pump head 4 Slowly pull the head and allow it to separate from the housing Carefully disengage the head from the piston by pulling the head straight off and away from its mounting studs Lateral motion while disengaging the pump head from the piston may break
19. Control panel in Chromeleon or on the touch screen HOME page Turn off the Dionex ICS 1600 power briefly and then restart 4 Ifthe problem persists repeat Step 2 If the problem persists contact Thermo Fisher Scientific for assistance Doc 065290 03 10 12 65 Dionex ICS 1600 lon Chromatography System OPTION NOT INSTALLED This error occurs if a command is issued to control an option that is not installed To troubleshoot Check the Chromeleon Server Configuration program to verify that the option is enabled 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 Contact Thermo Fisher Scientific for assistance PUMP MOTOR LOST CONTROL This error indicates a problem in the pump controller electronics To troubleshoot Contact Thermo Fisher Scientific for assistance The Dionex ICS 1600 electronics components cannot be serviced by the user PUMP PRESSURE HARDWARE ERROR This error indicates a problem in the pump controller electronics To troubleshoot Contact Thermo Fisher Scientific for assistance The Dionex ICS 1600 electronics components cannot be serviced by the user 66 Doc 065290 03 10 12 4 Troubleshooting o PUMP OVER PRESSURE If the system pressure exceeds the set limit for at least 0 5 second this error message appears and the pump stops Pressure limits can be set in th
20. Dionex AS DV Autosampler is installed replace the tip and tubing The Dionex AS DV Preventive Maintenance Kit P N 055647 contains all of the components required to replace the sampling tip and the tubing between the tip and the injection valve Instructions are included with the kit 60 Doc 065290 03 10 12 4 1 4 Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the Dionex ICS 1600 Turn to the section of this chapter that best describes the operating problem or symptom that has been observed Each section lists possible causes of the problem or symptom in order of probability A systematic troubleshooting approach is the most effective way to determine the root cause If you are unable to resolve a problem by following the instructions here contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office Please have this chapter at hand when talking with Technical Support personnel Error Messages The Moduleware the instrument control firmware installed in each Dionex ICS 1600 module periodically checks the status of certain parameters If a problem is detected it is displayed on the touch screen Error messages are also reported to Chromeleon and logged in the Audit Trail Each error message is preceded by an icon that identifies the seriousness of the unde
21. HEATER CAL VALUES page see Figure 5 23 enter the Calibrated Offset and Calibrated Slope values recorded in Step 4 COLUMN HEATER CAL VALUES Calibrated Offset 0 000000 Calibrated Slope 0 000000 o d PTM Figure 5 23 Column Heater Cal Values Page 118 Doc 065290 03 10 12 5 Service c To ensure the calibration values are recorded in the Dionex ICS 1600 memory do not turn off the Dionex ICS 1600 power for at least 1 minute after entering the values d Record the calibration values in the Chromeleon Wellness database To do this open the Wellness Panel see Section 5 1 1 and click Upload under Update Wellness Database 5 13 Replacing the Column Heater Heat Exchanger 1 Turn off the Dionex ICS 1600 power Open the front door of the Dionex ICS 1600 Unscrew the two thumbscrews on the column 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 24 and remove the plate Disconnect the heat exchanger inlet line from port C on the injection valve 6 Heat Exchanger Screws 3 Thumbscrew4 Figure 5 24 Dionex ICS 1600 Column Heater Cover Disconnect the heat exchanger outlet line from the guard column inlet 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
22. ICS 1600 injection valve or the auxiliary valve if installed must be specified as the injection valve and must be linked to the Dionex AS in the Chromeleon timebase e An injection valve should not be installed in the Dionex AS See the Dionex ICS 1600 installation instructions for Dionex AS connection instructions NOTE The Dionex ICS 1600 and the Dionex AS can be set up for stand alone front panel operation This requires a TTL cable connection between the Dionex ICS 1600 and the Dionex AS See Section C 3 for stand alone setup instructions 52 Doc 065290 03 10 12 3 Operation and Maintenance Setup for a Dionex AS DV Autosampler To use a Dionex AS DV Autosampler with the Dionex ICS 1600 the following requirements must be met e The Dionex ICS 1600 injection valve must be linked to the Dionex AS DV in the Chromeleon timebase Setup for a Dionex AS HV Autosampler For setup information for the Dionex AS HV Autosampler see the Dionex AS HV Autosampler Operator s Manual Document No 065125 The manual is provided on the Thermo Scientific Reference Library DVD P N 053891 3 10 1 Loading Samples with a Syringe 1 Make sure the injection port on the Dionex ICS 1600 front door see Figure 2 1 is connected to 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 IN Orange ri VALVE C ITO rig Green TO INJ
23. Plumbing connections 33 Rebuilding 99 Specifications 133 Troubleshooting 65 Input Output page 162 174 Installation Analog output connection 175 Priming 123 125 Index 4 Doc 065290 03 10 12 Index Stand alone operation setup 172 173 TTL and relay connections 165 166 Installed options 160 Inverted edge TTL input control 170 Inverted peaks 158 Inverted pulse TTL input control 170 Ion chromatography overview 1 Ion exchange 3 Isocratic delivery system 2 Isopropyl alcohol 126 127 L LCD screen 11 12 139 Specifications 130 See also Touch screen Leak sensor 17 Leak sensor wet alarm 65 Replacement 122 Leaks Auxiliary valve 72 Cell 72 Fittings 71 Injection valve 72 Liquid 71 Pressure transducer 72 Pump check valve 71 Pump head 71 Pump head waste valve 72 Pump piston seal 71 Suppressor 72 LED 130 Linearity requirements 132 Liquid leaks 71 See also Leaks Load inject valve alarm 65 Loading samples 52 Local Mode 147 Locked Remote mode 142 Loop See Sample loop M Main power receptacle 21 Maintenance 58 Daily 58 Ongoing 58 Weekly 59 Yearly 59 Manual sample processing 40 MicroMembrane Suppressor 18 See also Suppressor Module Setup page 161 Moduleware 61 160 MPa 154 N Nitrite in samples 51 Noise baseline 158 Normal edge TTL input control 169 Normal pulse TTL input control 170 O Offset conductivity 161 Offset per
24. Power Power Switch Press the power switch on the Dionex ICS 1600 rear panel see Figure 3 3 to turn on the system power Table 3 1 shows the Dionex ICS 1600 conditions at power up B Also turn on the power to the computer and the autosampler if used Figure 3 3 Dionex ICS 1600 Rear Panel Feature Pump Power Up Condition Off Injection valve Load position Cell Reading current value Suppressor Off Cell heater Set to the last value used The default when the Dionex ICS 1600 is turned on for the first time is 35 C Column oven temperature Set to the last value used The default when the Dionex ICS 1600 is turned on for the first time is 30 C When you start the suppressor the value used last is restored Table 3 1 Dionex ICS 1600 Power Up Conditions Doc 065290 03 10 12 41 Dionex ICS 1600 lon Chromatography System 3 3 Connecting to Chromeleon NOTE If you are beginning operation of a Dionex ICS 1600 that has not been configured in a timebase refer to the Dionex ICS 1600 installation instructions for Chromeleon setup instructions 1 Turn on the PC 2 Start the Chromeleon Server if it is not already running a Check the Chromeleon Server Monitor icon on the Windows taskbar e When the server is running the icon is gray Sa e When the Server is not running the icon is crossed out in red ak To start the server right click the ico
25. Rate Calibration Press for instructions Instructions Reset Flow Rate Cal Reset Cal Degas Calibration _ Press for instructions Degas Calibration Log Calibration Value Degas Pressure Current Cal Date Last Calibration Date Instructions Log 196610 3 7 2009 Set Flow Rate to 1 00 1 00 mL min Current Pump Pressure 800 psi 5 00 minute timer 5 00 min Enter new Flow Rate Cal 50g f Store Calibration Value Calibrate Log Calibration Value Log Current Calibration Date 3 7 2009 Last Calibration Date 3 7 2009 Electric Conductivity Cell Calibration Press for instructions Conductivity Cell Offset Cal Conductivity Cell Slope Cal Current Calibration Date Last Calibration Date Instructions Offset Cal Slope Cal 3 7 2009 3 7 2009 onductivity Cell Temperature Calibration Press for instructions Instructions Set Cell Temp to 35 C Cell 35 C Set Flow Rate to 1 00 1 00 mL min Total Conductivity 0 053 ps Cond Cell Calibration Calibrate Log Calibration Value Log Current Calibration Date 37 2009 Last Calibration Date 37 2009 ummy Cell Test Press for instructions Instructions Q Dummy Cell zm o Log Dummy Cell Value Log Figure 5 1 Chromeleon Wellness Panel 86 Doc 065290 03 10 12 5 Service Use the Wellness Panel to perform the following functions Ca
26. Regeneration 0 0 cee eee ee ee 132 A 7 Detector Electronics O A O A eee 132 A 8 Conductivity Cell with Heat Exchanger 0 133 ALO Injection Valve ie ahead eee eae eee pen 133 A 10 Auxiliary Valve Optional 0 0 eee eee eee eee 134 A 11 Vacuum Degas Assembly Optional 005 134 Doc 065290 03 10 12 V Dionex ICS 1600 lon Chromatography System A12 Column Heater i o seins nier endete edente eu be ae 134 A TI SUppressots ocre eunt tno dae EE eee Eee ensi 135 A TA Autosamplet rosene noseia Boh ce cele oe prb Hae dee bus 136 A5 System Software coe epe wave beh pe pepe UMES ER ERUNT Ra 136 Touch Screen Operation 139 B 1 Using the Touch Screen 0 0 0 eee eee eee 139 B 2 Using the Touch Screen with Chromeleon 142 B 3 Overview of Dionex ICS 1600 Touch Screen Pages 143 Bid Home Page 22 ie Re Ie eda caer dione 144 B 4 1 Home Page Pump Controls selle 144 B 4 2 Home Page Column Heater 004 145 B 4 3 Home Page Injection Valve Controls 146 B 4 4 Home Page Detector Controls 005 146 B 4 5 Other Home Page Controls 0 020002 eee eee 147 Bid Plot Pace ws nel E Poa BAA he Ee ot a a ots 148 BiG Status Page oeste Led te ottenere 149 B 6 1 Viewing Other Status Parameters 0 151 B 6 2
27. Reservoir egeo As Watt ade 45 3 45 Setthe Bluent Level 2 eL Eu 45 3 4 6 Connect the Reservoir 0 cece ene 47 3 5 Check All Connections 0 0 eens 47 3 6 Prime the Pump 3 cavex a pe x ERE wee Ree NER A qa ea 47 Doc 065290 03 10 12 Contents 3 7 Set System Operating Conditions 0 0 eee eee eee 48 3 8 Equilibrate the System and Verify Operational Status 49 3 9 Prepare Samples ie osse dene Autonet dante deua Bla tg 50 3 9 1 Collecting and Storing Samples 50 3 9 2 Pretreating Samples 0 0 0 cece eee eee 51 3 9 3 Diluting Samples 0 0 eee ee eee 51 3 10 Loading and Injecting Samples 0 0 0 eee 52 3 10 1 Loading Samples with a Syringe 00 53 3 10 2 Loading Samples with a Vacuum Syringe 54 3 10 3 Loading Samples with an Autosampler 54 3 10 4 Injecting Samples ossis cso cri nean e eee eee eee 55 3 11 Processing Samples osc 8 260 RE De pE RE NT 55 3 11 1 Manual Sample Processing 000 0005 55 3 11 2 Automatic Batch Sample Processing 56 3 12 Mamtenance ose caver accede aloes m nates se yek eas oa 58 4 Troubleshooting 0 0 61 4 1 Error Messages leeeee III 61 4 2 Troubleshooting Error Messages llle 63 4 3 JEiquid Leaks vss tea SV LENS REV 71 4 4 P
28. Scientific Reference Library DVD 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 4 Clogged column bed supports Refer to the instructions in the column manual for troubleshooting guidance Column manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Contaminated columns Clean the columns as instructed in the column manual or replace the guard column Doc 065290 03 10 12 77 Dionex ICS 1600 lon Chromatography System Plugged injection valve or auxiliary valve passages Rebuild the valve see Section 5 4 4 9 Peak Ghosting Ghosting is the appearance of extraneous peaks in a chromatogram These may be late eluting peaks from a previous injection They may also be the result of a contaminated standard or eluent or a malfunctioning injection valve These peaks may co elute with peaks of interest resulting in nonreproducible peak heights areas Insufficient time between sample injections Wait until the previous sample has been completely eluted before making another injection Insufficient flush bet
29. Upload under Update Wellness Database 94 Doc 065290 03 10 12 5 Service 5 2 Isolating a Restriction in the Liquid Lines A restriction in the liquid plumbing will cause excessive system backpressure 1 2 Begin pumping eluent through the system including the columns Follow the flow schematics in Figure 5 7 or Figure 5 8 and work backward through the system beginning at the suppressor Regen Out port One at a time loosen each fitting and observe the pressure The connection at which the pressure drops abnormally indicates the point of restriction NOTE The numbers on the flow schematics 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 If the 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 065290 03 10 12 95 Dionex ICS 1600 lon Chromatography System WASTE o ELUENT OUT OUT 2 e IN o 11 IN 9 oas COND a Q optional CELL ce z 2 5 T 8 d l amp PULSE o DAMPER S o o e rd i SSA UIE Eam a s L 7 w c awa VALVE WASTE 3 PUMP PUMP jj HEAD HEAD IN WASTE 4 PRESS XDUCER OUT
30. and determines chromatographic properties Equivalent Conductivity 1 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 065290 03 10 12 187 Dionex ICS 1600 lon Chromatography System Packing The material that fills a chromatographic column usually a resin or silica based material Pellicular Resin A resin with a solid nonporous core coated with a thin layer of more porous material The exchange sites of pellicular ion exchange resins are located only on the surface layer of the bead These resins have a low ion exchange capacity Pre Co
31. and pump casting Use the open end wrench P N 014605 provided in the Dionex ICS 1600 Ship Kit P N 067110 to tighten the two acorn nuts that attach the pump head to the pump housing see Figure 5 12 Tighten the nuts evenly 12 in Ib torque If the leak persists replace the piston seal see Section 5 7 Liquid leaks from the seal wash port Replace the piston seal see Section 5 7 74 Doc 065290 03 10 12 4 Troubleshooting Scratched pump piston Check the pump pistons for scratches and replace if necessary see Section 5 8 4 5 Pump Does Not Start No power front Power LED indicator is not lit Check that the power cord is plugged in Check the main power fuses and replace if needed see Section 5 18 No communication between Dionex ICS 1600 and Chromeleon Verify that the USB cable is connected correctly For connection and setup information refer to the Dionex ICS 1600 installation instructions Pump is turned off Turn on the pump from either the Chromeleon Control panel or the Dionex ICS 1600 touch screen HOME page Flow rate is set to 0 Set the flow rate from either the Chromeleon Control panel or the Dionex ICS 1600 touch screen HOME page 4 6 No Flow 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 Doc 065290 03 10 12 75 Dionex ICS 160
32. efficiency can be determined by the following N 5 54 t W 19 Where t the peak retention time in seconds Wip 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 5 to t4 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 186 Doc 065290 03 10 12 F Glossary of relatively clean sample This allows large volumes of sample to be injected lowering concentration detection limits Conductivity A measure of the ease with which electrical current flows through a liquid contained between two opposite charged electrodes Conductivity is a characteristic of ions in solution Units are siemens Counterion Ions carrying a charge opposite that of the sample ions e g Na may be the counterion of a CT analyte These ions preserve electrical neutrality in solution Crosslink Divinylbenzene content in a polystyrene divinylbenzene PS DVB resin this contributes to the mechanical strength of the resin
33. 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 5 17 Doc 065290 03 10 12 111 Dionex ICS 1600 lon Chromatography System 5 10 Replacing the Conductivity Cell 1 Turn off the Dionex ICS 1600 power 2 Open the front door and disconnect the tubing from the CELL IN and CELL OUT fittings see Figure 5 17 View A Loosen the two screws on the cell front cover The screws remain attached see Figure 5 17 View B Unscrew SCIENTIFIC DS6 HEATED CONDUCTIVITY CELL SERIALNO Cid CELL CONSTANT L 1 Disconnect View A Figure 5 17 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 Dionex ICS 1600 see Figure 5 18 Figure 5 18 Removing the Cell Assembly 112 Doc 065290 03 10 12 5 Service 5 Slide the new cell assembly straight into the opening in the component panel until it stops and the cell cover is flush against the component panel The cell s electronic connector automatically plugs into a connector inside the Dio
34. output line from the injection valve 6 Disconnect the line from the suppressor ELUENT OUT port to the cell inlet and connect the pump output line directly to the cell inlet 7 Disconnect the line from the suppressor REGEN IN port to the cell outlet Direct the cell outlet line to a waste container 8 Verify that the backpressure is at least 7 MPa 1000 psi 9 If you are using the touch screens to perform the calibration open the CONDUCTIVITY CELL page see Figure 5 4 CONDUCTIVITY CELL Push this button to set cell heater to 35 C n Total Conductivity 0000 pS 35 C Cell Constant 0 000000 Pump imM KCI through the cell at 1 mL min Push this button to set 1 mL min flow rate 1 mL min Calibrate WARNING THIS WILL ERASE THE PRIOR CELL CALIBRATION AND STORE A NEW VALUE o b ge Figure 5 4 Conductivity Cell Page 10 On the Wellness Panel under Conductivity Cell Calibration click Cell 35 C or touch 35 C on the Dionex ICS 1600 touch screen Allow the cell to reach this temperature and then wait an additional 5 90 Doc 065290 03 10 12 5 Service 11 12 13 14 15 16 17 minutes to let it stabilize When the temperature has stabilized is displayed to the right of the temperature reading on the CONDUCTIVITY CELL page Select 1 00 mL min to begin pumping 1 00 mM KCI through the cell at 1 0 mL min Wait until the total conductivity reading stabilizes in abo
35. outputs conductivity data as a 0 to 1 V signal to an integrator or recording device For connection and setup information refer to the Dionex ICS 1600 installation instructions USB Connectors A USB receptacle is provided to allow connection to the Chromeleon computer Two USB ports are provided for connecting to other USB 20 Doc 065290 03 10 12 2 Features devices For connection instructions refer to the Dionex ICS 1600 installation instructions TTL and Relay Connector The TTL and Relay connector strip provides two TTL outputs two relay outputs and four TTL inputs The outputs can be used to control functions in other TTL or relay controllable devices 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 Chases The upper tubing chase routes tubing from the RFIC ER compartment to the Dionex ICS 1600 rear panel The lower chase routes tubing from the rear panel to the component panel Tubing Clips The tubing clips hold tubing routed from the top cover in place Power Switch The power switch provides on off control of power to the Dionex ICS 1600 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 Dionex ICS 1
36. pos 1356 n 41 82 e Pump On Off ES 2 1 TTL GND 7 black Start Continue Schedule pos 11 12 12 Start Acquisition Analog Data Transfer ANALOG IN 4 RELAY OUT Third Party Analog to Digital Converter and Controller System Function Connection Inject AS TTL Out 1 to ICS 1600 TTL In 1 Autozero AS TTL Out 2 to ICS 1600 TTL In 2 Pump On Off AS RLY Out 2 to ICS 1600 TTL In 3 Start Data Acquisition AS RLY Out 1 to Third party DAC RLY In Start Continue Schedule Third party ADC RLY OUT to AS TTL In 2 ICS 1600 TTL Inputs AS TTL Inputs TTL IN 1 Inject TTL IN 1 unassigned TTL IN 2 Autozero TTL IN 2 Start Continue Schedule TTL IN 3 Pump On Off TTL IN 3 Tray Temp On Off TTL IN 4 Mark TTL IN 4 Therm Compart On Off Figure C 6 Example Connections for Stand Alone Operation Doc 065290 03 10 12 173 Dionex ICS 1600 lon Chromatography System Assign Dionex ICS 1600 Input Functions Go to the Dionex ICS 1600 INPUT OUTPUT touch screen page and verify that the Inject function is assigned to TTL input 1 that Autozero is assigned to TTL input 2 and that the TTL Input Control Type is Normal Edge see Figure C 7 INPUT OUTPUIT nputs TTL 4 Leadilnject TTL 3 Pump On fg TTL Input Control Type Outputs o dy ay Figure C 7 Input Output Page Enable Dionex AS Control of the Injection Valve 1 On the Dionex AS front pan
37. 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 065290 03 10 12 185 Dionex ICS 1600 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 Channeling 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
38. sex onte ee Bes wee YS 181 E 3 Why are the retention times moving 0 0 00008 181 E 4 How do I adjust retention times 0 0 00 e eee eee 181 E 5 When should I remake standards 0 000000 ee 181 Doc 065290 03 10 12 vii Dionex ICS 1600 lon Chromatography System F Glossary E 6 When should I remake eluents E 7 How do I start Chromeleon E 8 How dol delete data 00505 E 9 How do I back up data 00 00 00 E 10 How do I shut off the system E 11 How do I store columns 00 E 12 How do I know when a column is dirty E 13 How do I clean a column E 14 Why is the conductivity high E 15 How do I configure and operate the auxiliary valve Index PET 182 TEE 182 ETET 182 Priesti pioak 182 E E 182 TEETE 182 DERT ERENER 183 E 183 viii Doc 065290 03 10 12 1 Introduction 1 1 Introduction to lon Chromatography IC The Thermo Scientific Dionex ICS 1600 Ion Chromatography System Dionex ICS 1600 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
39. steps for routine operation of the Dionex ICS 1600 Power up the system C Start Chromeleon Set up the reservoir or RFIC ER system Check all connections C Prime the pump Set operating conditions Equilibrate the N system C Prepare samples Verify operating status Process samples Figure 3 1 Operation Flow Chart Doc 065290 03 10 12 39 Dionex ICS 1600 lon Chromatography System Sample Processing Overview Samples can be run manually one at a time or they can be grouped and run automatically in batches Figure 3 2 shows the typical steps for manual and batch sample processing Manual Sample Manual Sample Batch Sample Processing Processing Processing Using the Front Panel Using Chromeleon Using Chromeleon Load the sample Load the sample Create a sequence Sequence Wizard Start data C Autozero acquisition Add the sequence to the batch Inject the sample C Autozero 4 4 J C Start the batch Optional Inject the sample Record data from the analog output Stop data A third party recording acquisition device must be connected to the analog output Optional Save the manual sequence data Figure 3 2 Sample Processing Overview 40 Doc 065290 03 10 12 3 Operation and Maintenance 3 2 Turning On the System
40. the desired numerical value for the field and then touch the ENTER button Flow Rate in mL min range 0 00 0 05 to 5 00 Touch CANCEL to cancel the entry and return Touch a to the previous number to page enter the value Touch ENTER to confirm the entry and return to the previous page Figure 2 3 Number Keypad Doc 065290 03 10 12 13 Dionex ICS 1600 lon Chromatography System e Touching the page name for example HOME v in the bottom right corner opens a menu of pages see Figure 2 4 HOME PLOT STATUS Touch a page name to display PUMP the page SUPPRESSOR DETECTOR INFORMATION MODULE SETUP INPUT OUTPUT Figure 2 4 Dionex ICS 1600 Touch Screen Menu of Pages e Touching a page name on the menu of pages displays the selected page For example touching SUPPRESSOR displays the SUPPRESSOR page see Figure 2 5 See Appendix B for details about each touch screen page SUPPRESSOR Type None MMS kd Touch to select a Current e mA different option Automatically turn on with pump Touch to return to the Home page gt fA SUPPRESSOR Figure 2 5 Suppressor Page 14 Doc 065290 03 10 12 2 Features e Touching thy returns you to the HOME page e Touching opens a list of options see Figure 2 6 SUPPRESSOR None MMS Current X Automatically turn on M N o ty Touch an
41. the conductivity to zero Turn the pump on and off also turns the suppressor on and off e 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 Locate the twisted pair of wires P N 043598 and the 12 position connector plug Position 1 P N 923687 see Locking Figure C 2 in the Dionex Screws ICS 1600 Ship Kit P N 067110 Position 12 2 Follow these basic steps to connect the TTL or relays Figure C 2 12 Position Connector Plug a Foreachrelay or TTL to be used connect an active wire red and a ground wire black to the 12 position connector plug at the appropriate pin locations Refer to Figure C 1 or the label on the Dionex ICS 1600 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 IMPORTANT Stray strands of wire to short to the adjoining position on the connector 166 Doc 065290 03 10 12 C TTL and Relay C
42. the eluent usage by monitoring the flow rate and the length of time the pump is on The Dionex ICS 1600 updates the Eluent Level field as the eluent is depleted 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 screen to be accurate the level must be entered by the user when the reservoir is filled The Dionex ICS 1600 does not automatically detect when the reservoir is filled nor when it is empty B 4 2 Home Page Column Heater Column Heater The temperature of the column heater can be controlled to o C or between 30 and 60 C For optimal performance set the column heater to at least 5 C above the ambient temperature To set the temperature touch the Column Heater field and enter the desired temperature on the number pad To turn the Doc 065290 03 10 12 145 Dionex ICS 1600 lon Chromatography System column heater off set the temperature to 0 The display to the right of the temperature setting indicates the heater status column temperature is at equilibrium ji column temperature is rising i column temperature is falling Off column heater is off B 4 3 Home Page Injection Valve Controls Valve Elapsed Time OQ OQninutes The Inject and Load buttons select the position of the injection valve A dark background and white text on a button indicates the current valve position For details about the valve positions
43. the flow rate Refer to the suppressor manual for the recommended current setting for your application The suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 156 Doc 065290 03 10 12 B Touch Screen Operation NOTE When Chromeleon is used to control the Dionex ICS 1600 the Program Wizard automatically calculates the current required for the application e To manually control the suppressor power touch the Off and On buttons e To automatically control the suppressor power simultaneously with the pump flow select Automatically turn on with pump NOTE The suppressor always turns off when the pump is off regardless of whether the Automatically turn on with pump option is selected B 9 Detector Page Use the DETECTOR page to set the data rise time and to select parameters for adjusting the analog output To open this page select DETECTOR from the menu of pages DETECTOR Data Rise Time sec Conductivity Polarity Analog Qut Output Normal Offset Polarity Range d See Figure B 17 Detector Page Doc 065290 03 10 12 157 Dionex ICS 1600 lon Chromatography System B 9 1 B 9 2 Setting the Data Rise Time The data rise time determines the amount of filtering performed on the conductivity data The rise time is a measure of how quickly the detector responds to a change in signal and is defined as the time it takes the ou
44. valve directs the eluent flow path to waste and eliminates backpressure 3 Inthe Pump Settings window see Figure 3 6 click the Prime button Confirm that the waste valve is open by clicking OK when the reminder message appears The pump will begin pumping at about 3 mL min 4 Continue priming the Dionex ICS 1600 until no air bubbles are exiting the pump waste line 5 Inthe Pump Settings window click Pump Off 6 Close the waste valve Do not overtighten the valve Doc 065290 03 10 12 125 Dionex ICS 1600 lon Chromatography System 5 17 Priming the Pump with Isopropyl Alcohol 1 NOTE Prime the pump heads with isopropyl alcohol only if the two standard priming procedures described in Section 5 16 are unsuccessful Connect a 10 mL syringe P N 079803 filled with Secondary isopropyl alcohol IPA to Pump Head the port in the primary pump head see Waste Valve _ Figure 5 32 open Open the waste valve on the secondary pump head see Figure 5 32 by turning the knob one quarter to one half turn hcm Syringe Priming Valve counterclockwise P N 079803 open Primary Pump Head Figure 5 32 Priming the Pump Heads with IPA In the Pump Settings window see Figure 3 6 click Pump On Open the priming valve on the primary pump head by turning it one quarter to one half turn counterclockwise Use the syringe to slowly push alcohol through the pump NOTE Be careful not to push any air tra
45. 0 12 135 Dionex ICS 1600 lon Chromatography System Void Volume SRS 300 4 mm 50 uL SRS 300 2 mm 15 uL MMS 300 4 mm 50 uL MMS 300 2 mm 15 uL AMMS ICE 300 4 mm 50 uL AMMS ICE 300 2 mm 15 uL Anion AES 35 uL Cation AES 35 uL A 14 Autosampler Automation Using Autosampler Sequential Simultaneous Injection Automated Dilution Online Sample Degassing Online Filtration Automation Flexibility Dionex AS Dionex AS AP Dionex AS DV or Dionex AS HV Autosampler or third party autosampler May be available depends on autosampler capabilities Available with a Dionex AS Autosampler e Dilution Factor 1 1 to 1 1000 e Dilution Time 15 seconds with sample overlap Optional CRD 200 300 required Available with a Dionex AS DV Autosampler or an inline filter High using Chromeleon software and post run features A 15 System Software Software Automated Procedure Wizards System Wellness and Predictive Performance Chromeleon Chromatography Management System or Chromeleon Xpress validated for use with Windows Vista or Windows XP Standard feature Standard feature 136 Doc 065290 03 10 12 A Specifications Data Trending Plots Virtual Column Simulator Application Templates Automation Support for Third Party Vendors 3D Software for PDA MS and ED Customizable System Control Panels System Status Virtual Channels Power Fai
46. 0 lon Chromatography System Waste Valve Priming Valve Figure 4 2 Waste and Priming Valves Flow rate is set to 0 Set the flow rate from the Dionex ICS 1600 Control panel in Chromeleon or from the touch screen HOME page Eluent valve is closed Open the eluent valve from the Dionex ICS 1600 Control panel in Chromeleon or from the touch screen PUMP page Pump not primed Prime the pump see Section 5 17 e Broken pump piston Replace the piston see Section 5 8 4 7 Erratic Flow Pressure Reading e Pump needs priming Prime the pump see Section 5 17 76 Doc 065290 03 10 12 4 Troubleshooting Damaged piston seal Replace the piston seal see Section 5 7 Dirty pump check valve Clean or replace the check valve see Section 5 6 Leaking liquid lines or fittings Check the liquid lines and fittings for small leaks Tighten or if necessary replace the liquid line connection see Section 5 3 Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is included on the Thermo Scientific Reference Library DVD P N 053891 4 8 Excessive System Backpressure Restriction in the system plumbing Check all liquid lines for crimping or blockage Make sure the ferrule fittings are not overtightened onto tubing Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for details The manual is included on the Thermo
47. 042857 is installed on the valve at the factory 32 Doc 065290 03 10 12 2 Features The valve has two operating positions Load and Inject see Figure 2 17 LOAD POSITION INJECT POSITION Sample In s Sample In To Column To Column Sample re em 5 To Waste From Pump To Waste From Pump Figure 2 17 Injection Valve Flow Schematics Eluent flows through either the Load or Inject path depending on the valve position e Inthe 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 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 18 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 Thermo Fisher Scientific offers sample loops in various sizes If necessary the pre
48. 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 IMPORTANTI Relay loads in excess of 200 mA or with included power supplies over 60 V may damage the relay drivers on the CPU The TTL outputs are normally at 5 volts Setting a TTL output to 0 volts turns on the action in the connected device The TTL and relay output states can be controlled from Chromeleon either by issuing direct control commands from the Chromeleon Control panel or by including the commands in a control program To control the TTL and relay output states from the touch screen select INPUT OUTPUT from the menu of pages The INPUT OUTPUT page appears see Figure C 4 e To set a relay touch the relay field and select the desired state Open or Closed For example if Relay 1 is connected to the Load input on the autosampler touch the Relay 1 field and select Closed to start the load cycle e To seta TTL outputs touch the TTL field and select the desired state 5 Volts or 0 Volts Doc 065290 03 10 12 171 Dionex ICS 1600 lon Chromatography System C 3 Example Setup for Stand Alone Operation This section describes an example setup for stand alone operation operation without Chromeleon software with a Dionex AS Autosampler and a third party analog to digital converter and controller If your configuration includes different devices use the following steps as guid
49. 3 Dionex ICS 1600 Server Configuration Properties TTL Inputs 168 Doc 065290 03 10 12 C TTL and Relay Control To select TTL input functions and the control type from the touch screen go to the INPUT OUTPUT touch screen page see Figure C 4 INPUIT OUTPUT Select a lLoad inject TIL 3 Function Normal Edge M4 Select a Control Type A pong Figure C 4 Input Output Page Selecting TTL Functions TTL Input Control Types The Dionex ICS 1600 TTL inputs respond to four types Normal Pulse of signals to accommodate different controlling devices Inverted Edge The default control type Normal Edge is compatible Inverted Pulse with the output signals provided by Dionex modules Normal Edge If the device connected to the Dionex ICS 1600 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 Action Off or No Effect operation the negative falling edge of a signal turns on the NORMAL function For example for the EDGE i Load Inject function the Action On negative edge switches the injection valve position to Load Doc 065290 03 10 12 169 Dionex ICS 1600 lon Chromatography System The action of the positive rising edge depends on the function For the Load Inject function the rising
50. 4 Unscrew the black locking ring on the front of the valve see Figure 5 10 and remove the ring 5 Grasp the front of the valve pod and pull firmly to remove it from the Dionex ICS 1600 Black Locking Ring Figure 5 10 Unscrew the Valve Locking Ring 6 Check that the new pod 6 port P N 061947 10 port P N 061948 has the correct number of ports for the valve being serviced 7 Align the slots in the new pod with the runner in the valve holder on the Dionex ICS 1600 see Figure 5 11 Valve pods are keyed to fit only one way one slot is narrower than the other Verify that the slots are aligned with their matching runners 8 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 5 11 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Splines Figure 5 11 Valve Pod and Pod Holder Doc 065290 03 10 12 101 Dionex ICS 1600 lon Chromatography System 9 Push the pod into the holder until it clicks into place Replace the black locking ring 10 Reconnect all liquid lines to the valve 11 Turn on the pump flow Check for leaks from the valve Tighten fittings as required see Section 5 1 1 12 Close the door 102 Doc 065290 03 10 12 5 Service 5 6 Cleaning and Replacing the Pump Check Valves A dirty check valve causes erratic flow rates and pressures In ad
51. 4 Right Side Panel Figure 2 9 illustrates the RFIC ER compartment on the right side of the Dionex ICS 1600 Figure 2 9 RFIC ER Compartment Cover Removed The compartment houses the ER Controller ERC 10 and various columns required for operation in the RFIC ER mode The ERC 10 electronics monitor the volume of electrolysis gases such as hydrogen and oxygen in the eluent stream If the predefined safety limit is exceeded the ERC 10 shuts down the pump to prevent the buildup of gases in the eluent bottle If you plan to operate in the RFIC ER mode you must order one of these kits e RFIC ER Anion Startup Kit ICS 1100 ICS 1600 P N 069570 e RFIC ER Cation Startup Kit ICS 1100 ICS 1600 P N 069569 Each Startup Kit includes one Installation Kit and one Consumables Kit Together these kits contain additional items purification columns a special eluent bottle etc required for RFIC ER operation For more information refer to the manual shipped with the Installation Kit Doc 065290 03 10 12 19 Dionex ICS 1600 lon Chromatography System 2 1 5 Rear Panel Figure 2 10 illustrates the Dionex ICS 1600 rear panel Tubing Clips Power Switch Upper Chase Analog Output Connector Waste Lines 3 USB Connectors TTL and Relay Main Power Connector Strip Receptacle Lower Chase Figure 2 10 Dionex ICS 1600 Rear Panel Analog Output Connector The analog output connector
52. 5 4 Leaking detector cell 1 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 2 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 Thermo Fisher Scientific for assistance 72 Doc 065290 03 10 12 4 Troubleshooting 4 4 Pump Difficult to Prime or Loses Prime Excessive pressure fluctuations more than 3 difference from one pressure reading to the next indicate that the pump is out of prime Empty eluent reservoir and or no eluent connected Fill the reservoir Make sure all connections are secure Eluent improperly or insufficiently degassed If the Dionex ICS 1600 does not contain a vacuum degas assembly degas the eluent manually see Section 3 4 4 If the Dionex ICS 1600 contains a vacuum degas assembly check the degas settings 1 Open the Chromeleon Server Configuration program Right click the Dionex ICS 1600 device in the timebase and select Properties 2 Select the Options tab see Figure 4 1 Dionex ICS 1600 IC System Solvents State Devices Inject Valve Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General ptions Signals Head Type amp Limits M Degas C Always Off C Always On C Cycle Monito
53. 51 to 3200 uS cm Rise times from 0 to 10 s user selectable Fixed at 1 7 per 1 C at cell temperature Ambient 7 C 30 to 55 C 0 01 C A 8 Conductivity Cell with Heat Exchanger Cell Body Cell Electrodes Cell Volume Maximum Cell Operating Pressure Heat Exchanger Operating Temperature A 9 Injection Valve Chemically inert polymeric material Passivated 316 stainless steel compatible with MSA lt l uL 10 MPa 1500 psi Inert tortuous path for low axial dispersion 30 to 55 C 86 to 130 F must be at least 7 C above the ambient temperature Injection Valve 6 port 2 position Rheodyne valve with PEEK wetted components electrically activated Doc 065290 03 10 12 133 Dionex ICS 1600 lon Chromatography System A 10 Auxiliary Valve Optional Auxiliary Valve 6 port or 10 port 2 position Rheodyne valve with PEEK wetted components electrically activated A 11 Vacuum Degas Assembly Optional Channel Single channel degas channel with degas membranes Pump Dual stage diaphragm vacuum pump Materials Wetted materials PEEK PTFE A 12 Column Heater Operating 30 to 60 C 86 to 140 F minimum 5 C above ambient Temperature temperature Settable range is equal to working range Temperature 0 5 C at sensor Stability Temperature 0 5 C at sensor at 40 C Accuracy Maximum 250 mm analytical column with 50 mm guard column Column Lengths 134 Doc 065290 03 10 12
54. 600 Continue pulling until the JT connectors for the two cables are Eluent Valve outside the panel see Figure 5 26 Disconnect the cables 8 Remove the mounting plate on the old valve by unscrewing and removing the two screws Save the screws 9 Thread the cable from the new eluent valve through the mounting plate Remove Screws 10 Attach the mounting plate to the new valve using the screws removed in Step 8 Figure 5 27 Removing the Eluent Valve Mounting Plate 11 Connect the cable from the new valve P N 057945 to the Dionex ICS 1600 cable Feed the cables back inside the Dionex ICS 1600 Doc 065290 03 10 12 121 Dionex ICS 1600 lon Chromatography System 12 13 14 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 Dionex ICS 1600 Prime the pump see Section 5 17 5 15 Replacing the Leak Sensor 1 Turn off the power to the Dionex ICS 1600 Open the Dionex ICS 1600 front door Loosen the screw on the front of W the leak sensor see Figure 5 28 Note The screw remains attached to the sensor Figure 5 28 Leak Sensor Remove the leak sensor from the component panel and pull the cable out of the opening in the panel The cable attached to the leak sensor is connected to a matching cable inside the Dionex ICS 1600 Continu
55. 600 and is easily accessible CAUTION TP r gt 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 MISE EN GARDE Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist VORSICHT Doc 065290 03 10 12 21 Dionex ICS 1600 lon Chromatography System 2 2 Flow Schematics The following figures illustrate the liquid flow path through a Dionex ICS 1600 when using suppression in autorecycle mode Two configurations are shown Figure 2 11 illustrates the liquid flow path through components when performing conventional ion chromatography Figure 2 12 illustrates the liquid flow path when operating in the RFIC ER mode Flow Description for Standard Configuration Eluent from the eluent reservoir flows first through the pump degas assembly if it is installed and then through the eluent valve to the pump The eluent is then pushed through the pressure transducer which measures the system pressure From there the eluent is pushed through a pulse damper which smooths minor pressure variations from the pump to minimize baseline noise The eluent then flows into the injection valve Q After sample is loaded into the sample loop and the injection valve is toggled to th
56. An end line filter P N 045987 is provided in the Dionex ICS 1600 Ship Kit P N 067110 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 3 4 4 Fill the Reservoir Fill the reservoir with the prepared eluent 3 4 5 Set the Eluent Level After filling the reservoir enter the volume of liquid in the reservoir in one of the following locations e On the HOME page in the Eluent Level field see Figure 3 5 e In the Eluent Bottle field in the Pump Settings window accessed from the Dionex ICS 1600 Control panel on the Chromeleon panel tabset see Figure 3 4 The Dionex ICS 1600 determines the eluent usage by monitoring the flow rate and the length of time the pump is on and updates the Eluent Bottle Doc 065290 03 10 12 45 Dionex ICS 1600 lon Chromatography System volume as the eluent is depleted A warning appears if the level falls below 200 mL Warnings are repeated at 100 mL and 0 mL In order for the level displayed in the Eluent Bottle box and gauge to important be accurate you must enter the level when the reservoir is filled The Dionex ICS 1600 does not automatically detect when the reservoir is filled nor when it is empty Enter the volume of Eluent Level Note The Eluent Level liquid in
57. 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 chromatography 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 065290 03 10 12 1 Dionex ICS 1600 lon Chromatography System A typical IC analysis consists of six stages see Figure 1 1 1 Eluent Delivery 6 Data Analysis Conductivity 15 Detection Suppressor 4 Suppression Eluent Separator Column 3 Separation Pump Guard Column Injection Valve Sample 2 Sample Injection 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 Dionex ICS 1600 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 Dionex ICS 1600 injects the sample into the eluent stream The
58. Chromeleon Audit Trail and on the touch screen See Section 4 2 for troubleshooting information See Section B 7 1 for how to set the pressure limits 144 Doc 065290 03 10 12 B Touch Screen Operation Flow Rate The flow rate can be set to 0 00 which turns off the pump and to between 0 05 and 5 00 mL min The recommended operating flow rate is between 0 40 and 2 00 mL min Refer to the column manual for the flow rate to use with your column and application Column manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Pump On Off Control Touching the On button immediately starts the pump flow at the rate displayed in the Flow Rate field Touching Off stops the flow Prime The Prime button is reserved for use during the pump head priming procedure Touching the Prime button displays a confirmation page that reminds you to open the waste valve Open the valve and then touch the OK button to begin priming Or to exit the page without priming touch the Cancel button To stop priming touch the Off button During priming the flow rate is approximately 3 mL min See Section B 13 for detailed priming instructions Eluent Level Use this field to monitor the amount of liquid in the eluent reservoir When you fill the reservoir enter the amount of liquid in the reservoir For example if the reservoir contains 200 mL and you add 1 liter enter 1 2 liters Thereafter the Dionex ICS 1600 determines
59. Dionex ICS 1600 lon Chromatography System Operator s Manual Document No 065290 Revision 03 October 2012 2012 by Thermo Fisher Scientific Inc All rights reserved AES AMMS ICE ASRS Chromeleon Dionex IonPac OnGuard and SRS are registered trademarks of Thermo Fisher Scientific Inc in the United States Microsoft Windows Windows 2000 and Windows XP are registered trademarks of Microsoft Corporation in the United States and other countries Adobe Acrobat and Adobe Reader are registered trademarks of Adobe Systems Incorporated in the United States and other countries Reagent Free and RFIC are trademarks of Thermo Fisher Scientific Inc PEEK is a trademark of Victrex PLC All other trademarks are the property of Thermo Fisher Scientific Inc and its subsidiaries Thermo Fisher Scientific Inc provides this document to its customers with a product purchase to use in the product operation This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific Inc The contents of this document are subject to change without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scientific Inc makes no representations that this document is comple
60. Doc 065290 03 10 12 71 Dionex ICS 1600 lon Chromatography System Leaking pressure transducer 1 Make sure the liquid line connections into the pressure transducer are tight Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is included on the Thermo Scientific Reference Library DVD P N 053891 Replace any damaged fittings 2 Ifthe pressure transducer continues to leak contact Thermo Fisher Scientific for assistance The pressure transducer cannot be serviced by the user 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 If the leak persists replace the waste valve O ring see Section 5 9 Leaking suppressor Refer to the suppressor manual for troubleshooting procedures Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Leaking injection valve or auxiliary valve 1 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 included on the Thermo Scientific Reference Library DVD P N 053891 Replace any damaged fittings 2 Liquid leaks from behind the valve stator may indicate a scratched rotor seal Rebuild the valve see Section
61. Setup button A drop down list replaces the label for each field and the Setup button changes to Apply see Figure B 11 1234 ei To 6 s Total 1258 14 LS wee MOS hours Faw Ra M00 mL min pari 25 c Euppressor E200 mA Eluent a Figure B 11 Status Page Setup Doc 065290 03 10 12 151 Dionex ICS 1600 lon Chromatography System 2 Touch the down arrow next to the field you want to change A list of the available status parameters appears see Figure B 12 1234 To 6 TE Total 1258 14 15 toa Euer MO hours 100 mL min 29 C 200 mA Figure B 12 Status Page Parameter List 3 Touch the parameter you want to display 4 When finished touch the Apply button B 6 2 Status Parameter Details Status Parameter Description Eluent time The number of hours the eluent supply will last if the pump runs continuously at the current flow rate Flow rate The actual flow rate currently output by the pump Suppressor The actual current applied to the suppressor Elapsed time The number of hours since the last injection Cell temp The temperature of the cell heater C followed by a status symbol T or J Column temp The temperature of the column heater C followed by a status symbol is or 4 152 Doc 065290 03 10 12 B Touch Screen Operation B 7 Pump Page Use the PUMP page to set parameters related to pump operati
62. Status Parameter Details 0 0 0 0 00s ee eee 152 B Pump Pages vos he we RE Melde Me 153 B 7 1 Setting Pump Pressure Limits and Selecting the Pressure Unit Lh eats epe eI nU Ree tee E RU 153 B 7 2 Setting Degas Operating Parameters Optional 154 B 7 3 Controlling the Eluent Valve 0 0 0004 155 vi Doc 065290 03 10 12 Contents B 8 Suppressor Page 0 0 eee eee eee eee 156 B 9 Detector Page 1 usos ble dads Een b tuis ee les ie A 157 B 9 1 Setting the Data Rise Time 0 02 05 158 B 9 2 Selecting the Conductivity Polarity ss 158 B 9 3 Setting Analog Out Options 0005 159 B 10 Information Page sssseeeeee III 160 B 11 Module Setup Page 0 aa ea a a eee 161 B 12 Input Output Page 0 ce eee 162 B 13 Diagnostic and Calibration Pages 0 0 00 e eee eee 162 C TTL and Relay Control 165 C TTL and Relay Connections 0 0 00 eee eee eee 165 C 1 1 Selecting TTL Input Functions and Control Types 168 C 2 Controlling TTL and Relay Outputs 000 171 C 3 Example Setup for Stand Alone Operation 172 D Reordering Information 177 cq Doro TNT re ene ae ee eee eee 181 E 1 How do I hook up an autosampler 00 0 0 en 181 E2 How dol print 23 en no en
63. The results are displayed as a chromatogram and the concentrations of ionic analytes can be automatically determined and tabulated Doc 065290 03 10 12 3 Dionex ICS 1600 lon Chromatography System 1 2 Overview of the Dionex ICS 1600 The Dionex ICS 1600 is an integrated ion chromatography system containing a pump injection valve column heater and conductivity detector Other system components including a guard column separator column and suppressor vary depending on the analyses to be performed The Dionex ICS 1600 can optionally be configured with a vacuum degas assembly for online eluent degassing An optional second high pressure valve 6 port or 10 port can be installed for sample preparation applications The Dionex ICS 1600 contains a built in ER Controller and pre plumbed tubing for operation in the RFIC ER Reagent Free Ion Chromatography with Eluent Regeneration mode RFIC ER technology uses the suppressor to regenerate returning eluent allowing a single batch of eluent to be used for up to four weeks Dionex ICS 1600 operation can be controlled in one of two ways e Remotely with a personal computer running Microsoft Windows Vista or Windows XP and Chromeleon software version 6 80 SR6a or later Chromeleon also provides data acquisition and data processing functions e Locally with the front panel LCD touch screen The touch screen is used for instrument control only It does not provide data acq
64. UP page lets you select options for the touch screen display and conductivity readings To open this page select SETUP from the menu of pages MODULE SETUP Backlight Duration Always On kd Screen Timeout Never kd change to Home Ad screen Make conductivity the primary display value o ESTA Figure B 19 Module Setup Page Module Setup Options e Backlight Duration Select 2 hour time out to turn off the backlight after 2 hours if the touch screen is not used during that time Select Always On to have the backlight remain on continuously e Screen Time out If the touch screen is not used during the selected time out the display will change to show the screen selected from the list For example if you select 5 min and BUSY the display will change to the BUSY page see Figure B 10 5 minutes after the last time the Change touch screen was used Select Never to always fo cerca display the page that was used last options e Conductivity Display Select either Offset the Tme out options default setting or Total as the primary conductivity display value The selected value is shown in large bold type on the HOME and STATUS screens with the other value in smaller type Doc 065290 03 10 12 161 Dionex ICS 1600 lon Chromatography System B 12 Input Output Page The INPUT OUTPUT page provides control of the Dionex ICS 1600 TTL inputs and TTL and relay outputs To open this page select INPUT O
65. UTPUT from the menu of pages For details about relay and TTL control see Appendix C INPUT OQUTPUT Inputs TTL 4 Load inject TTL 3 Pump On fg m 2 m 4 Mark M TTL Input Control Type Outputs o d pee Figure B 20 Input Output Page B 13 Diagnostic and Calibration Pages Diagnostic and calibration functions can be performed either from the touch screen diagnostic and calibration pages or from the Chromeleon Wellness Panel To open a touch screen diagnostic or calibration page select DIAGNOSTIC from the menu of pages The DIAGNOSTIC page opens see Figure B 21 From there you can select the type of diagnostic or calibration to perform For detailed instructions on how to perform the various calibration and diagnostic procedures see Section 5 1 162 Doc 065290 03 10 12 B Touch Screen Operation DIAGNOSTIC Pump Calibration Flow Rate Detector Calibration Conductivity Cell Electric Conductivity Cell Column Heater Cal Values ccs Figure B 21 System Diagnostic Menu Page NOTE The Service button provides access to service functions that are performed only by Thermo Fisher Scientific personnel An access code is required to go to the service pages Doc 065290 03 10 12 163 Dionex ICS 1600 lon Chromatography System 164 Doc 065290 03 10 12 C TTL and Relay Control C 1 TTL and Relay Connections A 12 pin connector strip for TTL relay control is
66. VALVE P VALVE W damiani Green Black Figure 3 9 Injection Valve Connections 2 Fill the 1 cc syringe P N 016388 provided in the Dionex ICS 1600 Ship Kit P N 067110 with a calibration standard or sample 3 Insert the syringe into the injection port on the Dionex ICS 1600 front door see Figure 2 1 4 Verify that the injection valve is in the Load position Overfill the sample loop with several sample loop volumes Excess sample will exit through the injection valve waste line Doc 065290 03 10 12 53 Dionex ICS 1600 lon Chromatography System 6 Leave the syringe in the port 7 Switch the injection valve to the Inject position see Section 3 10 4 3 10 2 Loading Samples with a Vacuum Syringe 3 10 3 1 Disconnect the waste line from port W 6 of the injection valve see Figure 3 9 and attach a shorter line 25 to 30 cm 10 to 12 inches of PEEK or PTFE polytetrafluoroethylene 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 Dionex ICS 1600 Ship Kit P N 067110 into the injection port on the Dionex ICS 1600 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 aut
67. ading 33 Reordering 177 Sample processing 40 55 56 Batch 40 56 Manual 40 55 With Chromeleon 55 56 Samples Collecting and storing 50 Diluting 51 Filtering 51 Injecting 52 54 Loading 52 Pretreating 51 Saving data 55 56 Seal replacement 106 Second valve Troubleshooting 68 Second valve error 68 Selectivity Troubleshooting 79 Self Regenerating Suppressor 18 See also Suppressor Separation process 3 Separator column 18 Sequence Control panel 27 Sequence Wizard 58 Server Configuration program Starting 42 Service chase 15 18 Service procedures 104 Check valve cleaning 103 104 Check valve replacement 103 Conductivity cell replacement 112 Fuse replacement 127 Injection valve rebuilding 99 Isolation of liquid lines restriction 95 Leak sensor replacement 122 Piston replacement 109 Piston seal replacement 105 Priming valve O ring replacement 110 Rebuilding the auxiliary valve 99 Rebuilding the injection valve 99 Replacing tubing and fittings 98 Suppressor replacement 115 Tubing and fittings replacement 98 Waste valve O ring replacement 110 Signal to noise ratio 158 Software control 26 Modes of 27 Software specifications Application templates 136 Automated procedure wizards 136 Automation support for third party vendors 136 Customizable system control panels 136 Customized reporting 137 Daily Audit Trail 136 Multiple network control 137 Network failure prote
68. alibration value in the Audit Trail If you performed the calibration from the Dionex ICS 1600 touch screen record the new calibration values in the Chromeleon Wellness database To do this open the Wellness Panel see Section 5 1 1 and click Upload Doc 065290 03 10 12 93 Dionex ICS 1600 lon Chromatography System 5 1 5 Calibrating the Vacuum Degas Assembly When to Calibrate 1 After every 6 months of use Open the Dionex ICS 1600 Wellness Panel in Chromeleon see Section 5 1 1 or open the Dionex ICS 1600 touch screen PUMP DEGAS page see Figure 5 6 PUMP DEGAS Pump degas calibration takes 90 seconds Vacuum Degas Pressure reading 0 Degas Calibration value 0 o d pewem ug Figure 5 6 Pump Degas Page On the Wellness Panel under Degas Calibration select Calibrate or touch Calibrate on the Dionex ICS 1600 touch screen The degas pump runs for 90 seconds to allow a vacuum to be created After 90 seconds the vacuum degas pressure reading is recorded When the vacuum degas assembly is running in monitor mode this calibration value is used to determine when to turn on the degas pump If you are using the Wellness panel click Log to record the new calibration value in the Audit Trail If you performed the calibration from the Dionex ICS 1600 touch screen record the new calibration values in the Chromeleon Wellness database To do this open the Wellness Panel see Section 5 1 1 and click
69. alve 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 9 or auxiliary valve 6 Close the door 7 Turn on the pump Doc 065290 03 10 12 99 Dionex ICS 1600 lon Chromatography System SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP TO INJ Orange VALVE C P Black TO INJECT VALVE P Green TO INJ VALVE W Green Figure 5 9 Injection Valve Plumbing 5 5 Replacing an Auxiliary Valve Pod This procedure describes how to replace the mechanical part the pod of the optional auxiliary valve This procedure is an alternative to rebuilding the valve see Section 5 4 NOTE If the valve electronics require service contact Thermo Fisher Scientific Electronics related repair procedures must be performed by Thermo Fisher Scientific personnel IMPORTANT Substituting non Dionex Thermo Fisher Scientific parts may impair performance thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information 1 Turn off the pump flow from the Dionex ICS 1600 Control panel in Chromeleonor from the touch screen HOME page 2 Open the Dionex ICS 1600 front door 3 Disconnect each liquid line connected to the valve 100 Doc 065290 03 10 12 5 Service
70. ce 5 11 Replacing the Suppressor Refer to the suppressor manual for guidance about when to replace a suppressor Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 1 Refer to the suppressor quick start guide shipped with the suppressor for instructions on preparing the suppressor before initial use and for additional installation details Turn off the pump from the Dionex ICS 1600 Control panel in Chromeleon or from the touch screen HOME page Open the front door of the Dionex ICS 1600 Disconnect the two eluent and the two regenerant lines from the suppressor To remove the suppressor from the component 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 Dionex ICS 1600 is outside the panel see Figure 5 20 Disconnect the suppressor cable twist the ring on the yellow connector and pull the two connectors apart Yellow Connector E Figure 5 20 Removing the Suppressor Connect the cable from the new suppressor to the Dionex ICS 1600 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 Doc 065290 03 10 12 115 Dionex ICS 1600 lon Chromatography System 10 11 12 13 14 Push the cables
71. centage analog out 159 Offsetting background conductivity 49 146 Operating features 11 Operating humidity 130 Operating ranges Cell heater 17 146 Column heater 18 145 Flow rate 17 145 Operating temperature 130 Operation Equilibration time 49 Overview 39 Priming 47 125 126 Reservoir setup 44 Sample preparation 50 Sample processing 40 Setting operating conditions 48 Starting Chromeleon 42 Doc 065290 03 10 12 Index 5 Dionex ICS 1600 lon Chromatography System System power up 41 Operational status verification 49 Option not installed error 66 Options installed 160 Oven See Column heater Overview of system 4 P Panel tabset 26 How to display 27 Panels Chromeleon Control panel 55 Chromeleon Wellness panel 85 Component panel 16 Parameters Chromeleon operating commands 56 Peak ghosting 78 Peak height Effect of rise time on 158 Reproducibility 36 Troubleshooting 79 Peak shape 158 Peak width 158 Peaks Effect of rise time on 158 Extraneous ghosting 78 Inverted 158 Reversed 158 159 PEEK Conductivity cell body 36 PGM file See Programs Physical specifications Decibel level 129 Dimensions 129 Weight 129 Piston seals Replacement procedure 105 106 Pistons Replacement procedure 109 Plot offset 148 Plot page 147 148 Elapsed time 148 Plot offset 148 Range 148 Plotting detector output 148 Plumbing Injection valve 100 Replacing tubin
72. creen Operation Edit Field Command Button selected Command Button unselected Pump 0 psi Limit 1000 4000 Flow Rate Total 146 99 pS Autozero Cell Heater Status Field Elapsed Time Type None MMS Eluent Level L Perat Mode 2 pee Figure 2 2 Dionex ICS 1600 Touch Screen Home i Page NOTE To adjust the screen contrast open the front door and adjust the knurled knob under the screen see Figure 2 8 e Edit fields and command buttons have blue text on a shaded background Fields that display status information are not shaded e Edit fields have square corners while command buttons are rounded e To select a command button or edit a field touch and release the command button or edit field with your fingertip NOTE When you touch a button or edit field the action is taken when you lift your finger If you unintentionally touch a button or field you can cancel the action by sliding your finger away from the button or field before lifting e Touching a command button for example inject J executes the command immediately 12 Doc 065290 03 10 12 2 Features e Selecting a command button changes the button s appearance to white text on a dark backgound for example Flow Rate e Touching an edit field for example mL min opens a page with a number keypad see Figure 2 3 Use the keypad to enter
73. ction 137 Power failure protection 136 Sample Audit Trail 136 Sequential injection 136 Storage of calibration settings 137 System status virtual channels 136 System trigger commands and conditionals 136 System Wellness and Predictive Performance 136 Virtual column simulator 136 Specifications Autosampler 136 Column heater 134 Conductivity cell 133 Detector 132 Electrical 129 Environmental 130 Injection valve 133 Index 8 Doc 065290 03 10 12 Index LCD touch screen 130 Physical 129 Pump 130 Supressors 135 System software 136 Vacuum degas assembly 134 Stand alone operation 172 176 Analog output connection 175 AS setup 174 176 Example connections 173 TTL and relay connections 172 Standards When to remake 181 Status Control panel 27 Status page 147 149 Sulfite in samples 51 Suppression description 3 Suppressor Controlling the current to 156 Description 18 36 Leaking 72 Replacement procedure 115 Selecting the type 156 Suppressor alarms Suppressor not connected 69 Suppressor over current 69 Suppressor over power 70 Suppressor stopped for zero flow rate 70 Suppressor page 156 Supressor specifications Chemical suppression 135 Displacement chemical regeneration 135 Electrolytic suppression 135 Sequential suppression for anions 135 Suppression capacity 135 Suppressor wear parts 135 Void volume 135 Syringe injection 53 Vacuum 54 System Shutdown 182 Start
74. dL Secondary protective conductor terminal 8 Doc 065290 03 10 12 1 Introduction 5 BO Power supply is on Power supply is off Hot surface Indicates a potential hazard Refer to the operator s manual for an explanation of the hazard and how to proceed Doc 065290 03 10 12 Dionex ICS 1600 lon Chromatography System 10 Doc 065290 03 10 12 2 Features This chapter describes key Dionex ICS 1600 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 Dionex ICS 1600 a i ELUENT Touch Screen Power mm C3 LED ell e Injection O Port Figure 2 1 Dionex ICS 1600 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 Dionex ICS 1600 must be connected to an autosampler For more information about sample injection see Section 3 10 Touch Screen The LCD touch screen provides local control of most Dionex ICS 1600 functions You can control many of these functions directly on the touch screen s HOME page see Figure 2 2 From the HOME page you can also go to a series of pages that provide access to all other locally controlled Dionex ICS 1600 operating functions Doc 065290 03 10 12 11 Dionex ICS 1600 lon Chromatography System Summary of Touch S
75. dary pump head assembly Outlet check valve assembly 10 32 Inlet check valve assembly 1 4 28 Check valve cartridges Piston Piston seal Piston rinse seal O ring for waste valve or priming valve Eluent valve 10 mL 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 mL syringe for manual injections Injection Valve Rebuild Kit Auxiliary Valve Auxiliary Valve Kit 6 port valve Auxiliary Valve Kit 10 port valve Injection Valve Rebuild Kit for use with auxiliary valve also Doc 065290 03 10 12 177 Dionex ICS 1600 lon Chromatography System Part Number 061947 061948 056116 056118 064554 064556 064555 064557 057985 069564 059979 060943 079910 052324 923686 043598 069570 067791 069569 067792 070061 954745 060494 060392 Item Auxiliary valve pod assembly 6 port valve Auxiliary valve pod assembly 10 port valve Suppressors Cell and Column Heater Dionex AAES Anion Atlas Electrolytic Suppressor Dionex CAES Cation Atlas Electrolytic Suppressor Dionex ASRS 300 4 mm Anion Self Regenerating Suppressor Dionex CSRS 300 4 mm Cation Self Regenerating Suppressor Dionex ASRS 300 2 mm Anion Self Regenerating Suppressor Dionex CSRS 300 2 mm Cation Self Regenerating Suppressor Dionex DS6 heated conductivity cell Column heater assembly Column heater heat exchanger 0 25 mm 0 010 in ID tubing
76. degas assembly may need to be replaced Contact Thermo Fisher Scientific for assistance HARDWARE NOT PRESENT This error indicates a problem in the Dionex ICS 1600 electronics 64 Doc 065290 03 10 12 4 Troubleshooting To troubleshoot Contact Thermo Fisher Scientific for assistance The Dionex ICS 1600 electronics components cannot be serviced by the user LEAK SENSOR WET The leak sensor is installed in the drip tray at the bottom of the component panel see Figure 2 8 If liquid accumulates in the tray the sensor signals the problem and this error message appears To troubleshoot 1 Locate the source of the leak by visually inspecting the tubing fittings and components on the component panel Refer to Section 4 3 2 Tighten fittings or replace tubing and fittings as required Refer to Section 4 3 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray thoroughly to prevent the leak sensor from triggering additional error messages o LOAD INJECT VALVE ERROR If the injection valve fails to switch position within 1 second of being toggled the Dionex ICS 1600 Moduleware reports an error to Chromeleon and this error message appears To troubleshoot l Ifasequence is being executed terminate the sequence by selecting Batch Stop in Chromeleon 2 Try to toggle the valve from Load to Inject by clicking the Load and Inject buttons on the Dionex ICS 1600
77. dition it may cause the pump to lose prime and or be difficult to reprime If possible replace dirty check valves If new check valves are not available follow the instructions for cleaning Replacing Check Valves 1 Close the eluent valve from the Dionex ICS 1600 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page 2 Turn off the main power switch to ensure that you do not unintentionally start the Dionex ICS 1600 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 12 5 Use a 1 2 inch wrench to loosen both check valve assemblies Remove the check valve assemblies from the pump head _ Outlet Check Valve Primary Secondary Pump Head Pump Head Acorn Nuts Inlet Check Valve Figure 5 12 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 065290 03 10 12 103 Dionex ICS 1600 lon Chromatography System If you 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 Inlet Out
78. e Chromeleon Server Configuration or in the control program The limits can also be set on the touch screen PUMP page see Section B 7 1 To troubleshoot 1 Check for blockages in the liquid lines by working your way backward from the cell to the pump See Section 2 2 for the system flow schematics 2 Check that the flow rate is set to the correct value Check that the high pressure limit is set to the correct value 4 Restart the pump Doc 065290 03 10 12 67 Dionex ICS 1600 lon Chromatography System o PUMP STOPPED DUE TO LOST USB COMMUNICATION ERROR This error occurs if the Dionex ICS 1600 loses communication with Chromeleon To troubleshoot Verify that the USB cable is connected correctly from the Dionex ICS 1600 rear panel to the Chromeleon PC PUMP UNDER PRESSURE If the system pressure falls below the low pressure limit the pump stops and this error message appears Pressure limits can be set in the Chromeleon Server Configuration or in the control program The limits can also be set on the touch screen PUMP page see Section B 7 1 To troubleshoot 1 Make sure the eluent reservoir is full 2 Check for liquid leaks see Section 4 3 3 Check that the waste valve is closed 4 Prime the pump see Section 5 16 5 Restart the pump SECOND VALVE ERROR If the auxiliary valve fails to switch position within 1 second of being toggled the Dionex ICS 1600 Moduleware reports an error to Chromele
79. e pulling the cable until the connectors for the two cables are outside of the panel see Figure 5 29 Disconnect the two cables Figure 5 29 Leak Sensor Cable 122 Doc 065290 03 10 12 5 Service 7 Connect the cable from the new leak sensor P N 058053 to the Dionex ICS 1600 cable 8 Feed the cables back inside the Dionex ICS 1600 Align the leak sensor with the component panel opening and fingertighten the screw 9 Make sure the leak sensor does not touch the bottom of the drip tray 5 16 Priming the Pump 1 Verify that the eluent reservoir is filled the reservoir cap is installed and hand tightened and the liquid line from the Dionex ICS 1600 to the reservoir cap is connected 2 Verify that the waste lines are directed to a waste container 3 The priming procedure consists of two parts e Priming the eluent lines with a syringe see Section 5 16 1 Perform this procedure at initial installation after changing eluents or when eluent lines are empty e Priming the pump heads with the Prime button see Section 5 16 2 Perform this procedure after the eluent lines are primed 5 16 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 079803 to the priming valve port on the primary pump head see Figure 5 30 Doc
80. e Inject position eluent passes through the sample loop The eluent sample mixture is pumped through the heat exchanger G which heats the mixture to the column heater temperature The mixture then goes to the guard and separator columns and through the suppressor Q9 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 22 Doc 065290 03 10 12 2 Features r ELUENT OUT E i IN ra Q iN 2 1 DEGAS COND 3 e optional CELL E 3 ul o a lt oO 7 em Lu E 2 3 PUMP PUMP ij HEAD HEAD IN WASTE 4 OUT mc WASTE OUT z s 2 m o o S amp tc amp W o Figure 2 11 Dionex ICS 1600 Flow Schematic Standard Configuration Doc 065290 03 10 12 23 Dionex ICS 1600 lon Chromatography System Flow Description for RFIC ER Mode Eluent from the eluent reservoir flows first through the pump degas assembly if it is installed and then through the eluent valve to the pump The eluent is then pushed through the pressure transducer which measures the system pressure From there the eluent is pushed through a pulse damper
81. e 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 3 9 2 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 cartridges Refer to Installation and Troubleshooting Guide for OnGuard Cartridges Document No 032943 for instructions 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 to dilute the sample Whe
82. ed beaker To Calibrate 1 Open the Dionex ICS 1600 Wellness Panel in Chromeleon see Section 5 1 1 or open the Dionex ICS 1600 touch screen FLOW RATE page see Figure 5 5 FLOW RATE First push Reset Cal button Reset Cal Stabilize at 1 mL min at 2000psi 200psi for 20 min Push this button to set 1 mL min flow rate f mL min Collect water into tared beaker for exactly 5 minutes Enter weight of water 0 000000 g Wait 15 minutes before re checking o b Be Figure 5 5 Flow Hate Page Pressure 2016 psi 2 Verify that there is 14 1 4 MPa 2000 200 psi of backpressure 92 Doc 065290 03 10 12 5 Service 10 11 12 On the Chromeleon Wellness Panel under Pump Flow Rate Calibration select Reset Cal or touch Reset Cal on the touch screen Select 1 mL min to set the flow rate and begin pumping deionized water Allow the pump to stabilize for 20 minutes If you are using the Wellness Panel click 5 00 min to start the timer If you are using the touch screen start an external timer Immediately start collecting water into the tared beaker Collect the water for exactly 5 00 minutes Enter the weight of the water in grams If you are using the Wellness Panel click Calibrate to download the value to the Dionex ICS 1600 To recheck the value wait at least 15 minutes and then repeat the calibration If you are using the Wellness panel click Log to record the new c
83. edge switches the injection valve to the Inject position For the Pump On function the rising edge turns off the pump and suppressor For Autozero and Mark the rising edge has no effect Inverted Edge The inverted edge mode works identically to the normal edge mode except that the positive and negative edges are reversed in function 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 Action On TTL le INVERTED EDGE io y LL h Action Off or No Effect TTL Y a eae NORMAL PULSE gy Lll U 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 Inverted Pulse The inverted pulse mode operates identically to the normal pulse mode except that the positive and negative edges are reversed in function Action On Action Off TTL V INVERTED PULSE 49 y 170 Doc 065290 03 10 12 C TTL and Relay Control C 2 Controlling TTL and Relay Outputs The Dionex ICS 1600 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
84. eee 19 215 RearPanel 12 229 Per sas Dre an tenes 20 2 20 Flow Schematics seeeeeeeeee eh 22 2 3 Chromeleon and Chromeleon Xpress 000 esee 26 2 9 1 The Panel Tabset icici cocoa Rex 26 2 3 Software Control Modes 0 0 c eee eee eee 27 2 3 3 system Wellness ceresc ecse retean bee E p e p d 27 Doc 065290 03 10 12 i Dionex ICS 1600 lon Chromatography System 2 4 System Component Details 00 0 0 eee eee 28 2 4 1 Vacuum Degas Assembly Optional 28 24 2 Bluent Valve xi ofa esee tbe ER dre ea anes 30 2 4 3 PUMP os eec peser Dre PESE PW Ee EU Dens 30 2 4 4 Injection Valve ener esee ERREUR RES ERR 32 2 4 5 Auxiliary Valve Optional 0 000002 ee eee 34 244 0 Column Heater cna be etn Guten is wake othe arate 35 24 7 Suppressor i eree nra eee oe ere So eae ba hee Shed bee 36 2 4 8 DS6 Heated Conductivity Cell 0 0 0 00000000 36 24 9 JER Controller cete RR 37 3 Operation and Maintenance 39 3 1 Operation Overview 0 eee 39 3 2 Turning On the System Power 0 0 eee eee eee eee 41 3 3 Connecting to Chromeleon 0 0 eee eee 42 3 4 Set Up the Eluent Reservoir 0 0 ccc eee eee 44 3 4 1 Prepare the Eluent irre as one he 44 34 2 Degas the Eluent 0 0 0 eee ee 44 3 43 Filter the Eluent 0 0 cee ce eee 45 SAA Bill the
85. eine Verletzungsgefahr besteht Notes Informational messages also appear throughout this manual These are labeled NOTE and are in bold type NOTE NOTES call attention to certain information They alert you to an unexpected result of an action suggest how to optimize instrument performance etc Doc 065290 03 10 12 7 Dionex ICS 1600 lon Chromatography System 1 4 Safety and Regulatory Information The Dionex ICS 1600 was manufactured by Thermo Fisher Scientific at the following location 527 Lakeside Drive Sunnyvale CA 94088 3603 U S A The Dionex ICS 1600 is designed for IC ion chromatography applications and should not be used for any other purpose Operation of a Dionex ICS 1600 in a manner not specified by Thermo Fisher Scientific may result in personal injury If there is a question regarding appropriate usage contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office 1 4 4 Safety Labels The TUV T Mark and cTUVus Mark safety labels and the CE Mark label on the system indicate that it is in compliance with the following standards EMC Susceptibility and Emissions e EN 61326 1 2006 Safety e CAN CSA C22 2 61010 1 2004 UL 61010 1 2004 EN 61010 1 2001 The symbols below appear on the Dionex ICS 1600 or on labels affixed to the Dionex ICS 1600 n Alternating current D Primary protective conductor terminal
86. el press Menu and 0 to go to the TIME FUNCTION OUT screen In the LOAD INJECT VALVE TTL 1 field select ENABLED TIME FUNCTION OUT TTL STATE LOAD INJECT VALVE 1 ENABLED LOAD INJECT VALVE 2 DISABLED Help Prompt Figure C 8 Dionex AS Time Function Out Screen 2 Turn the Dionex AS power off and then back on You can now issue commands from the Dionex AS to switch the Dionex ICS 1600 injection valve position 174 Doc 065290 03 10 12 C TTL and Relay Control Connect the Analog Output 1 Locate the analog cable for the third party analog to digital converter and controller 2 Connect the analog input connector on the third party controller to the ANALOG OUTPUT connector on the Dionex ICS 1600 rear panel see Figure C 6 Configure the Dionex ICS 1600 Analog Output Go to the Dionex ICS 1600 DETECTOR touch screen page and select the settings shown in Figure C 9 DETECTOR Data Rise Time 1 00 sec Conductivity Polarity Analog Out Output Normal 96 Offset Polarity Range dy penses Mg Figure C 9 Detector Page Doc 065290 03 10 12 175 Dionex ICS 1600 lon Chromatography System Create a Dionex AS Method and Schedule Figure C 10 is an example of Dionex AS method timed events that can be used with the TTL Relay connections shown in Figure C 6 TIMED EVENTS METHOD 1 TIME VALVE CSV TTL1 TTL2 RLY1 RLY2 INIT LOAD 0 00 INJECT 1 0 50 0 Help Prompt Figure C 10 Example Di
87. elines and refer to your product documentation for specific connection details Connect the Dionex AS Autosampler Follow the instructions in the Dionex ICS 1600 installation instructions to connect the Dionex AS Autosampler to the Dionex ICS 1600 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 Figure C 5 in the Dionex ICS 1600 and Dionex AS Ship Kits Position 12 2 Attach the wires to the connector plug positions indicated in Figure C 6 Locking Screws 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 IMPORTANT Stray strands of wire to short to the adjoining position on the connector 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 172 Doc 065290 03 10 12 C TTL and Relay Control Dionex ICS 1600 Rear Panel Connections Dionex AS Rear Panel Connections ANALOG OUTPUT TTL 2 OUT TTL 1 IN TTL 1 OUT TTL2 Ne TENG RLY 2 OUT TTEA its RLY 1 qi TTL IN OUT 7 12 8 9 10 1 red pos black
88. eluent reservoir During routine operation the valve opens and closes automatically when the pump flow is turned on and off However during eluent line priming you can use the controls on the PUMP page to manually open the valve allowing liquid to flow through the lines when the pump is off See Section B 13 2 for eluent line priming instructions Doc 065290 03 10 12 155 Dionex ICS 1600 lon Chromatography System B 8 Suppressor Page Use the SUPPRESSOR page to specify the type of suppressor installed in the Dionex ICS 1600 turn the suppressor on and off and select the amount of current supplied to the suppressor To open this page touch the suppressor button on the HOME page or select SUPPRESSOR from the menu of pages SUPPRESSOR Type None MMS kd Current e mA X Automatically turn on with pump M NJ o d pese Figure B 16 Suppressor Page Suppressor Controls The suppressor type is typically selected at initial installation and does not need to be changed However if a different type of suppressor is installed later or if the suppressor is removed from the system touch the Type field and select the new suppressor type None MMS SRS or AES from the list To set the current touch the Current field and enter the desired setting in milliamperes on the number pad The appropriate suppressor current setting depends on several variables the suppressor type the column the eluent and
89. emperature coefficient which is determined experimentally Theoretical Plates N See Column Efficiency Void Volume V 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 065290 03 10 12 189 Dionex ICS 1600 lon Chromatography System 190 Doc 065290 03 10 12 Symbols Offset analog out 159 A Adjusting the contrast 12 139 Air particulate samples 51 Alarm conditions 63 70 See also Error messages Ambient temperature 81 Analog output 157 159 166 Offset 159 Configuring 159 175 Connections 175 Connector 20 Full scale 159 Range 159 Analog to digital controller 175 Anion separations 50 Application Wizard 57 AS Autosampler 52 Connections for stand alone operation 172 Enabling injection valve control 174 Maintenance yearly 59 Method for stand alone operation 176 Sample injection 54 Schedule for stand alone operation 176 Time Function Out screen 174 AS DV Autosampler 53 Maintenance yearly 60 Sample injection 54 AS HV Autosampler 53 Atlas Electrolytic Suppressor 18 See also Suppressor Audit Trail Error messages 61 Icons 61 Index Autosampler Loading samples with 54 See also AS Autosampler See also AS DV Autosampler Autosampler Control panel 27 Autosampler specificatio
90. eon Audit Trail and displayed on the LCD touch screen Pump Heads The Dionex ICS 1600 includes a dual piston serial pump The flow rate can be set to 0 00 mL min or to between 0 05 and 5 00 mL min However for optimum performance set the flow rate to between 0 40 and 2 00 mL min Setting the flow rate to 0 00 mL min turns off the pump See Section 2 4 3 for details about the pump Injection Valve The injection valve is a six port electrically activated Rheodyne valve A 25 uL sample loop P N 042857 is installed on the valve at the factory See Section 2 4 4 for details about valve operation Auxiliary Valve Optional The auxiliary valve is a two position electrically activated Rheodyne valve 6 Port Valve Kit P N 069472 10 Port Valve Kit P N 069473 See Section 2 4 4 for details about valve operation 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 and 55 C For optimum performance set the temperature to at least 7 C above the ambient temperature and 5 C above the column oven temperature See Section 2 4 8 for details about the cell Doc 065290 03 10 12 17 Dionex ICS 1600 lon Chromatography System Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions thereby inc
91. g Humidity Operating Pressure 35 MPa 5000 psi maximum liquid path tubing valve columns etc A 4 Front Panel Power LED On when power is present off when no power is present LCD Touch 14 VGA 320 x 240 pixels liquid crystal display with touch screen Screen which provides e Local control of Dionex ICS 1600 components pump detector suppressor injection valve column heater vacuum degas TTLs and relays e Display of conductivity data plot and operating status e Local control of calibration and diagnostic functions A 5 Analytical Pump and Fluidics Type Serial dual reciprocating pistons microprocessor controlled constant stroke variable speed Construction Chemically inert metal free PEEK pump heads and flow paths compatible with aqueous eluents of pH 0 to 14 and reversed phase solvents Operating 0 to 35 MPa 0 to 5000 psi Pressure Flow Rate 0 00 to 5 00 mL min in 0 01 mL min increments without changing Range pump heads Flow Precision 0 196 typical 130 Doc 065290 03 10 12 A Specifications Flow Accuracy Pressure Ripple Eluent On Off Valve Piston Seal Wash Pressure Alarm Limits Vacuum Degas Eluent Bottles Eluent Bottle Pressure Leak Detection lt 0 1 typical lt 1 at 13 8 MPa 2000 psi and 1 0 mL min Standard feature Dual pump head wash can be continuous when connected to rinse solution supply e Upper limit 0 to 35 MPa or 0 to 5000 psi in one unit MPa or
92. g and fittings 98 Troubleshooting 95 Polarity Selecting the conductivity polarity 158 Power Turning on 41 Power cord 127 Power receptacle 21 Power requirements 129 Power up conditions 41 Pressure Home page display 144 Limit 68 144 153 System 68 153 Unit selecting 153 Pressure transducer 17 32 Leaking 72 System backpressure 32 Prime button 145 Priming 47 123 125 126 Pump is out of prime 74 With a syringe 123 With isopropyl alcohol 126 With the Prime button 125 Priming valve Opening 30 O ring replacement procedure 110 Printing 181 Problems See Troubleshooting Processing samples 40 55 56 Automatically batch 40 56 57 Manually 40 55 Product warranty 85 99 100 Programmed software control 27 Programs Chromeleon 27 Controlling an autosampler 54 Index 6 Doc 065290 03 10 12 Index PSI 154 Pulse damper 22 24 32 Pump 30 Flow rate 17 145 Home page controls 144 Leaks 71 Over pressure alarm 67 Primary pump head 30 Priming 47 123 Priming problems 73 Secondary pump head 31 Selecting the pressure unit 153 Setting pressure limits 153 Stopped due to lost USB communication 68 Troubleshooting 75 Under pressure alarm 68 Pump check valve leaking 71 Pump degas See Vacuum degas assembly Pump head waste valve Leaking 72 O ring replacement procedure 110 Pump heads 103 Pump motor lost control alarm 66 Pump page 153 Changing the pressure u
93. gnetic 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 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 piston rinse seal gently insert the shaft of the piston through the small hole in the center of the guide see photo c Pullthe seal off the end of the 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 7 Inone 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 do
94. gs to and from the suppressor eluent ports Pump not properly primed Prime the pump see Section 5 17 Contaminated or incorrect eluent Remake the eluent using concentrated eluent and ASTM filtered Type I 18 megohm deionized water RFIC ER systems only Replace the RFIC ER columns if necessary An Audit Trail message will inform you when a column is approaching the end of its useful life span You can also check the life expectancy of the columns on the RFIC ER Wellness panel 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 Dionex ICS 1600 and the Dionex ICS 1600 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 Thermo Scientific Reference Library DVD P N 053891 Doc 065290 03 10 12 81 Dionex ICS 1600 lon Chromatography System e Cell above or below temperature Contact Thermo Fisher Scientific for assistance Damaged piston seal Replace the piston seal see Section 5 7 4 15 Vacuum Degas Assembly Does Not Run Degas option not enabled
95. he piston seal If unchecked these leaks can gradually contaminate the piston housing causing the pump to operate poorly If leaks occur replace the piston seals see Section 5 7 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 Every Six Months e Calibrate the cell see Section 5 1 3 e Calibrate the vacuum degas assembly see Section 5 1 5 e Replace the pump piston rinse seals and piston seals see Section 5 7 Yearly e Thermo Fisher Scientific recommends performing preventive maintenance annually as well as before scheduled Performance Qualification tests A Dionex ICS 1600 Preventive Maintenance Kit P N 057954 is available for this purpose e Rebuild the auxiliary valve if installed see Section 5 4 e Ifa Dionex AS Autosampler is installed perform the preventive maintenance procedure The Dionex AS Preventive Maintenance Kit P N 060581 is available for this purpose Doc 065290 03 10 12 59 Dionex ICS 1600 lon Chromatography System If a
96. ifferent from the temperature at which the cell was calibrated 36 Doc 065290 03 10 12 2 Features 2 4 9 DS6 Heated Conductivity Cell Components The cell front cover provides CELL IN and CELL OUT fittings for connecting the cell to the suppressor see Figure 2 8 The remaining cell components are mounted behind the component panel To replace the cell remove the screws on the cell front cover and pull the entire cell assembly out through the component panel See Section 5 10 for cell replacement instructions ER Controller The ER Controller ERC 10 is installed in the RFIC ER compartment at the factory During operation in the RFIC ER mode the ERC 10 electronics monitor the volume of electrolysis gases such as hydrogen and oxygen in the eluent stream If the predefined safety limit is exceeded the ERC 10 shuts down the Dionex ICS 1600 pump to prevent the buildup of gases in the eluent bottle Doc 065290 03 10 12 37 Dionex ICS 1600 lon Chromatography System 38 Doc 065290 03 10 12 3 Operation and Maintenance This chapter describes routine operating and maintenance procedures for the Dionex ICS 1600 The Dionex ICS 1600 is designed for IC ion chromatography applications and should not be used for any other purpose Operation of the Dionex ICS 1600 in a manner not specified by Thermo Fisher Scientific may result in personal injury 3 1 Operation Overview Figure 3 1 illustrates the basic
97. in Chromeleon 1 Open the Chromeleon Server Configuration program Right click the Dionex ICS 1600 device in the timebase and select Properties 2 Select the Options tab see Figure 4 3 Dionex ICS 1600 IC System Solvents State Devices Inject Valve Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General ptions Signals Head Type amp Limits M Degas Always Off C Always On C Cycle On 0 120 sec Off 0 5940 sec Monitor M Column Heater M Valve 2 RFIC ER Link to ERC Controller None Cancel Help Figure 4 3 Dionex ICS 1600 Server Configuration Properties Options 3 Verify that the Degas check box is selected 82 Doc 065290 03 10 12 4 Troubleshooting 4 Under Degas verify that the Always Off option is not selected If it is select one of the following settings instead e Cycle also select On 30 seconds and Off 10 minutes e Monitor 5 Ifthe Degas settings are correct but the degas assembly still does not run test the assembly by selecting the Always On option The pump should turn on immediately If it does not the vacuum degas assembly may need to be replaced Contact Thermo Fisher Scientific for assistance NOTE Degas options can also be selected from the touch screen PUMP page see Section B 7 Select the Degas Always On option only when testing the vacuum degas assembly Do not select the Always On option for routi
98. installed 25 uL loop can be replaced with a loop that has a different sample injection volume Doc 065290 03 10 12 33 Dionex ICS 1600 lon Chromatography System SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP TO INJ Orange VALVE C P Black TO INJECT _ Green VALVE P 2 4 5 Figure 2 18 Injection Valve Plumbing Auxiliary Valve Optional The auxiliary valve is a high pressure Rheodyne valve The electrically activated 2 position PEEK valve is offered in both 6 port and 10 port models 6 Port Valve Kit P N 069472 10 Port Valve Kit P N 069473 The auxiliary valve enables a variety of sample preparation activities including Online filtration Matrix elimination for example the removal of high backgrounds of chloride or organic material Concentrator based techniques Conditional injections large loop small loop applications where the data system monitors sample concentration and reinjects the sample using the smaller loop if the concentration is too high AutoNeutralization Matrix diversion prior to MS mass spectrometry detection For more information refer to Installing the ICS 1100 ICS 1600 ICS 2100 Auxiliary Valve Document No 065288 The manual is provided in the Auxiliary Valve Kit 34 Doc 065290 03 10 12 2 Features 2 4 6 Column Heater The column heater provides temperature control for the separator and gua
99. into the opening in the component panel Align the top of the suppressor with the guide line printed on the component panel see Figure 5 21 and align the slots on the rear of the suppressor 1 Suppressor with the tabs on the panel Mounting Tabs Press the suppressor onto the 2 Suppressor tabs and then slide it down until Cable Connector it locks into place Pull slightly 3 Guideline for on the center of the suppressor to AES verify that it is securely fastened 4 Guideline for Note Some suppressors require SRS more force to secure them onto the tabs Connect the two eluent and two regenerant lines to the new suppressor Close the Dionex ICS 1600 front door Figure 5 21 Suppressor Guidelines and Mounting Tabs on Component Panel 5 12 Replacing the Column Heater Turn off the Dionex ICS 1600 power Open the front door of the Dionex ICS 1600 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 c Unscrew the six thumbscrews on the top metal plate see Figure 5 22 and remove the plate 116 Doc 065290 03 10 12 5 Service Thumbscrews 6 Figure 5 22 Dionex ICS 1600 Column Heater Cover Hemoved d Remove the columns from the column heater e Pullthe column heater straight toward you to remove it from the component panel 4 Before instal
100. ions e Calibrating the Conductivity Cell Section 5 1 3 e Calibrating the Flow Rate Section 5 1 4 Calibrating the Vacuum Degas Assembly Section 5 1 5 Doc 065290 03 10 12 85 Dionex ICS 1600 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 Thermo Fisher Scientific Service Representatives To Open the Wellness Panel 1 In the Chromeleon Browser expand the Dionex Templates Panels Wellness folder 2 Double click ICS 1100 1600 2100 Wellness user pan The Wellness Panel opens see Figure 5 1 If the controls on the Wellness panel are disabled select Control Connect to timebase and then select the Dionex ICS 1600 timebase 1CS 1600 System Statu ER ICS 1600 Wellness Panel System 2 CMADLER1 ICS 1600 System Status Audit Trai iv Connected EJ Calibration Diagnostic Pump Calibration Details Details On Off kee D11 06 27 AM Pump_ECD Please verify the solvent and waste level values 11 06 28 AM Manually acquired samples will be stored temporarily in sequence SEQ CMADLER_local System_2 manual 11 06 28 AM Chromeleon server version 6 90 SR6a Build 2502 RC 2 v Update Wellness Database Press for instructions Instructions Upload Loading Pump Flow
101. let Check Check NOTE The pump will not operate Valve 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 Install the inlet check valve 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 IMPORTANT Overtightening may damage the pump head and check valve housing 10 11 and crush the check valve seats Reconnect the liquid lines Turn on the Dionex ICS 1600 main power Open the eluent valve from the Dionex ICS 1600 Control panel in Chromeleon or select Eluent Valve Closed on the touch screen PUMP page Prime the pump see Section 5 17 When the Dionex ICS 1600 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 2 Carefully remove the check valve cartridges from the valve housings Place the check valve housings and cartridges in a beaker with methanol Sonicate or agitate the parts for several minutes Rinse each check valve housing and cartridge thoroughly with filtered deionized water To reinstall the check valves and complete the procedure see Step 6 through Step 11 above
102. librate the pump flow rate Calibrate the vacuum degas assembly Calibrate the conductivity cell Test the conductivity cell electronics using a dummy cell Upload calibration values from the Dionex ICS 1600 to the Chromeleon Wellness database After completing a calibration procedure from the touch screen always update the Chromeleon Wellness database by clicking the Upload button on the Chromeleon Wellness Panel see Figure 5 1 This action ensures that the current calibration information is stored in Chromeleon as well as in the Dionex ICS 1600 Doc 065290 03 10 12 87 Dionex ICS 1600 lon Chromatography System 5 1 2 Diagnostic and Calibration Touch Screen Overview Select DIAGNOSTIC from the touch screen menu of pages The DIAGNOSTIC page opens see Figure 5 2 From there you can access individual diagnostic and calibration pages NOTE The Service button provides access to service functions that are performed only by Thermo Fisher Scientific personnel A code is required to access the service pages DIAGNOSTIC Pump Calibration Flow Rate Detector Calibration Conductivity Cell Electric Conductivity Cell c By passer Figure 5 2 System Diagnostic Menu Page 88 Doc 065290 03 10 12 5 Service 5 1 3 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 ce
103. ling the new column heater write down the two calibration values offset and slope recorded on the back of the heater 5 Align the connector on the back of the new column heater P N 069564 with the connector on the component panel and push the column heater onto the component panel 6 Remove the heater cover and the metal plate on the new heater 7 Install the columns in the new heater and replace the top metal plate and heater cover 8 Turn on the Dionex ICS 1600 power Doc 065290 03 10 12 117 Dionex ICS 1600 lon Chromatography System 9 Enter the column heater calibration values in Chromeleon or on the Dionex ICS 1600 touch screen DIAGNOSTIC page as follows To enter the calibration values in Chromeleon a Open the Wellness Panel see Section 5 1 1 and click Calibration Details b Under Column Heater Calibration Values enter the Column Heater Offset and Column Heater Slope values recorded in Step 4 c In the field next to the Download button verify that Current is selected and then click Download to download the new calibration values to the Dionex ICS 1600 d To ensure the new calibration values are recorded in the Dionex ICS 1600 memory do not turn off the Dionex ICS 1600 power for at least 1 minute after downloading the values To enter the calibration values on the Dionex ICS 1600 touch screen DIAGNOSTIC page a Goto the DIAGNOSTIC page and touch Column Heater Cal Values b Onthe COLUMN
104. ll see the instructions in Section 5 10 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 Dionex ICS 1600 Wellness Panel in Chromeleon see Section 5 1 1 or open the touch screen ELECTRIC CONDUCTIVITY CALIBRATION page see Figure 5 3 ELECTRIC CONDUCTIVITY CALIBRATION Total Conductivity 0 000 pS Cell Constant 0 000000 Wait until this calibration is done before doing slope cal Run Slope Cal WARNING THIS WILL ERASE THE PRIOR SLOPE CALIBRATION AND STORE A NEW VALUE Fine Offset 0 00000000 Slope 0 02483527 X 10 Medium Offset 0 00000000 Slope 0 39736432 X 1075 Coarse Offset 0 00000000 Slope 1 86264525 X 1075 o b pe Figure 5 3 Electric Conductivity Calibration Page Doc 065290 03 10 12 89 Dionex ICS 1600 lon Chromatography System 2 On the Wellness Panel under Electric Conductivity Cell Calibration click Offset Cal or touch Run Offset Cal on the Dionex ICS 1600 touch screen 3 When the offset calibration is complete click Slope Cal on the Wellness Panel or touch Run Slope Cal on the Dionex ICS 1600 touch screen 4 Ifyou are using the Wellness Panel click Log to record the new calibration values in the Audit Trail 5 Disconnect the pump
105. located on the Dionex ICS 1600 rear panel The connector provides two relay outputs two TTL outputs and four TTL inputs see Figure C 1 Connector Pin Function Position Description 1 z 1 Solid State Relay Contacts Output RELAY 2 QUT 3 4 2 E Solid State Relay Contacts Output TTLOUT 1 5 TTL Output 1 1 kO pull up to 5 100 mA sink 2 6 TTL Output 2 1 KQ pull up to 5 100 mA sink 1 7 TTL Input 1 Inject Load TTL IN 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 0 5 12 Ground to different inputs Figure C 1 TTL and Relay Connector on Rear Panel IMPORTANTI Relay loads in excess of 200 mA or with included power supplies over 60 V may damage the relay drivers on the CPU NOTE TTL 1 Input Inject Load applies only to the injection valve not to the auxiliary valve if installed Doc 065290 03 10 12 165 Dionex ICS 1600 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 Dionex ICS 1600 functions e Switch the injection valve position load inject e Perform an autozero command set
106. low Pressure readings can be monitored from the Chromeleon Control panel or the touch screen HOME page The system pressure should remain consistent no more than a 3 difference from one pressure reading to the next High and low pressure limits can be used to stop the pump flow if a limit is exceeded The pressure limits can be set from Chromeleon in the Server Configuration or in the control program or from the touch screen PUMP page see Section B 7 See Section 4 2 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 life of the seals To use this feature an external water source must be connected For connection instructions refer to the Dionex ICS 1600 installation instructions For continued protection of the pump replace the piston rinse seals see Section 5 7 and O rings in the seal wash assembly every 6 months or whenever you replace the main piston seals for the Dionex ICS 1600 pump Injection Valve The injection valve P N 057968 is a six port electrically activated valve A 25 uL sample loop P N
107. lumn 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 of the distance between the two peak maxima to the mean value of the peak width at the baseline Rz 2 t a t W gt WD Where t and t the retention times of components 1 and 2 respectively W 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 188 Doc 065290 03 10 12 F Glossary Siemens S Unit measure of conductance the reciprocal of the electrical resistance of a solution Suppressor A device used to minimize eluent conductivity and convert sample species to a common form thus increasing detection sensitivity Temperature Coefficient The percent of change in the conductivity of a solution with a 1 C change in temperature Every solution has a characteristic t
108. lure Protection Sequential Injection System Trigger Commands and Conditionals Daily Audit Trail Sample Audit Trail Multiple Network Control and Network Failure Protection Storage of System Calibration Settings Numerical device parameters can be plotted e Evaluation mode Standard feature e Isocratic and gradient modes Optional features Standard feature Fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Optional feature Standard feature Standard feature Standard feature Standard feature Standard feature Standard feature Standard feature Optional feature Factory current and previous calibration values are stored the user can reset current values to factory or previous values Doc 065290 03 10 12 137 Dionex ICS 1600 lon Chromatography System Customized Standard feature unlimited report workbooks Reporting Automated Detailed comprehensive qualification reports System Qualification 138 Doc 065290 03 10 12 B Touch Screen Operation The LCD touch screen on the Dionex ICS 1600 front panel allows local control of most Dionex ICS 1600 functions This chapter describes how to operate the Dionex ICS 1600 from the touch screen When the Dionex ICS 1600 starts up the touch screen displays a startup page This is followed by the INFORMATION page which displays version and serial numbers and a list of installed
109. mand button changes the button s appearance to white text on a dark background for example Flow Rate Touching an edit field for example msi opens a page with a number keypad see Figure B 2 Use the keypad to enter the desired numerical value for the field and then touch the ENTER button Flow Rate in mL min range 0 00 0 05 to 500 Touch CANCEL to cancel the entry and return Touch a to the previous numberto page enter the value Touch ENTER to confirm the entry and return to the previous page Figure B 2 Number Keypad 140 Doc 065290 03 10 12 B Touch Screen Operation e Touching the page name for example Hoe MP in the bottom right corner opens a menu of pages see Figure B 3 Touch a page name to display the page DIAGNOSTIC Figure B 3 Dionex ICS 1600 Touch Screen Menu of Pages e Touching a page name on the menu of pages displays the selected page For example touching SUPPRESSOR displays the SUPPRESSOR page see Figure B 4 SUPPRESSOR Setting None MMS amp 4 Touch to select a Current p mA different option Off eu Tous Mani return to the ds pine M 4 XxX Automatically turn on with Home page page Ad Figure B 4 Suppressor Page 141 Doc 065290 03 10 12 Dionex ICS 1600 lon Chromatography System e Touching fy returns you to the HOME page e Touching opens a list of optio
110. manual for additional troubleshooting guidance Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Sample concentration too high Dilute the sample see Section 3 9 3 Wrong eluent Check that you are using the correct eluent for your application RFIC ER systems only Replace the RFIC ER columns if necessary An Audit Trail message will inform you when a column is approaching the end of its useful life span You can also check the life expectancy of the columns on the RFIC ER Wellness panel Background conductivity not offset from conductivity reading Before making an injection allow the background conductivity to equilibrate and then click Autozero on the Dionex ICS 1600Control panel in Chromeleon or the Dionex ICS 1600 touch screen HOME page Cell out of calibration Recalibrate the cell see Section 5 1 3 80 Doc 065290 03 10 12 4 Troubleshooting 4 14 Baseline Noise or Drift Flow system leak erratic baseline Check all fittings and liquid lines for leaks Tighten or if necessary replace all liquid line connections Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is included on the Thermo Scientific Reference Library DVD P N 053891 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 fittin
111. n and select Start Server b If the Server Monitor icon is not on the Windows taskbar click Start gt All Programs gt Chromeleon gt Server Monitor The Server Monitor opens Click Start to start the server 3 To start the Chromeleon client click Start and select All Programs gt Chromeleon gt Chromeleon 4 If Chromeleon is installed the main window and Browser appear Display the panel tabset by i selecting View gt Default Panel Du HC EIH ga iN rs k Tabset or by clicking the Default Panel Tabset toolbar button Chromeleon File View Workspace Tools Help If Chromeleon Xpress is installed starting the application automatically displays the panel tabset 5 To display the Dionex ICS 1600 Control panel click the tab labeled with the Dionex ICS 1600 timebase name see Figure 3 4 42 Doc 065290 03 10 12 3 Operation and Maintenance a System_2 7 gt k ICS 1600 System with Column Heater and AS System 2 CMADLERI RFICER Wellness Sequence Control Status Autosampler Pum Pump Settings Mj tes S Load Inject l Injector Settings Column Heater Temperature 35 0 C Heater Settings 0 025 uS Suppressor Off L oma Detector Settings Detector ampl em Log Audit Trail on System 2
112. n 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 Doc 065290 03 10 12 51 Dionex ICS 1600 lon Chromatography System 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 3 10 Loading and Injecting Samples NOTE Samples can be injected using either the standard injection valve or the optional auxiliary valve if installed For more information see the Chromeleon Help or user s manual The two techniques for loading samples into the sample loop are 1 with an autosampler or 2 with a syringe or vacuum syringe through the injection port on the Dionex ICS 1600 front door For autosampler injections the injection port tubing is disconnected from the Dionex ICS 1600 injection valve and replaced by the autosampler outlet tubing Other setup requirements depend upon the model of autosampler Setup for a Dionex AS Autosampler To use a Dionex AS Autosampler with the Dionex ICS 1600 the following requirements must be met e The Dionex
113. ne use 6 Ifthe degas pump runs when you select Always On but does not run when Monitor is selected recalibrate the degas assembly see Section 5 1 5 Doc 065290 03 10 12 83 Dionex ICS 1600 lon Chromatography System 84 Doc 065290 03 10 12 5 Service This chapter describes Dionex ICS 1600 service and repair procedures that the user can perform All procedures not included here including electronics related repair procedures must be performed by Thermo Fisher Scientific personnel For assistance contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office Before replacing any part refer to the troubleshooting information in Chapter 4 to isolate the cause of the problem IMPORTANT Substituting non Dionex Thermo Fisher Scientific parts may impair 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 can be performed either from the touch screen or from the Chromeleon Wellness Panel see Figure 5 1 For an overview of the Wellness Panel features see Section 5 1 1 For an overview of the diagnostic and calibration touch screen see Section 5 1 2 For instructions on performing calibration and diagnostic procedures see the following sect
114. nected 3 6 Prime the Pump If you changed eluent or if the eluent lines are dry prime the lines first with a syringe before following the procedure below to prime the pump See Section 5 16 1 for instructions on priming the lines with a syringe 1 Verify that the priming valve on the primary pump head see Figure 3 8 is closed turned all the way clockwise Doc 065290 03 10 12 47 Dionex ICS 1600 lon Chromatography System 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 gt Waste Valve GF open Primary 2 Pump Head Priming Valve close Figure 3 8 Priming the Pump 3 Press Prime on the Chromeleon Control panel or the Dionex ICS 1600 touch screen HOME page Confirm that the waste valve is open by pressing OK when the reminder message appears The pump will begin pumping at approximately 3 mL min 4 Continue priming the Dionex ICS 1600 until all air and previous eluent are purged and no air bubbles are exiting the waste line 5 Press Pump Off 6 Close the waste valve Do not overtighten The pump is now ready for operation 3 7 Set System Operating Conditions NOTE This section is an overview of the steps needed to start up the system and begin running samples Actual operating parameters flow rate
115. nex ICS 1600 when you push the assembly into the opening Tighten the screws on the cell front cover fingertight Close the side panel door and tighten the two mounting screws Reconnect the inlet and outlet lines n a Turn on the Dionex ICS 1600 power 10 Calibrate the new cell in Chromeleon or on the Dionex ICS 1600 touch screen DIAGNOSTIC page Calibration of a new cell consists of three parts e Running the offset calibration which measures the output of the cell electronics alone and determines an offset value to be applied to raw conductivity readings e Running the slope calibration which measures the output of the cell electronics when a built in dummy cell which provides a constant conductivity reading of 21 uS is automatically enabled The slope value is applied to raw conductivity readings e Entering the cell constant measured at the factory The Dionex ICS 1600 uses the cell constant to determine the measured conductivity To calibrate the cell in Chromeleon a Open the Wellness Panel see Section 5 1 1 b Under Electric Conductivity Cell Calibration click Offset Cal c When the offset calibration is complete click Slope Cal d Click Calibration Details Under Conductivity Cell Cal Details enter the Cell Constant value printed on the front of the cell e Inthe field next to the Download button verify that Current is selected and then click Download to download the new value to the Dionex ICS 1600
116. ngs 4 Datasource Elapsed Program Time Sequence Sample Program System 2 gt k ICS 1600 System with Column Heater and AS System 2 CMADLERI RFICER Welness Sequence Contol Status Autosampler Sample 11 06 28 AM Manually acquired samples will be stored 11 06 28 AM Chromeleon server version 6 80 SR6a Build e 11 06 A AM M Pump ECD Please verify the solvent and waste level values temporarily in sequence SEQ CMADLER_local System_2 manual CS 1600 System Total Program Time W Connected Startup Shutdown Show Plot 10 05 8 05 20 0 yl from Pos 1 Figure 2 13 Dionex ICS 1600 Control Panel on the Panel Tabset 26 Doc 065290 03 10 12 2 Features e A Sequence Control panel lets you define and run sequences groups of sample injections to be analyzed in the order in which they are listed e A Status panel shows the overall system status e An Autosampler panel included if the Dionex ICS 1600 is connected to a Dionex AS Dionex AS AP Dionex AS DV or Dionex AS HV Autosampler provides access to autosampler functions To open the panel tabset use one of the methods below If Chromeleon is installed start Chromeleon and click the Default Panel Tabset toolbar button or select X View Default Panel Tabset Chromeleon File View Works
117. nit 153 Setting degas parameters 154 Setting pressure limits 153 Pump pressure hardware error 66 Pump priming valve O ring replacement procedure 110 Pump specifications Construction 130 Delay volume 130 Eluent bottle pressure 130 Eluent generation 130 Flow accuracy 130 Flow precision 130 Flow rate 130 Gradient capabilities 130 Operating pressure 130 Pressure ripple 130 Type 130 Vacuum degasser 130 Q Quantification method 58 R Range 148 159 Rear panel 20 Analog output connector 20 Power receptacle 21 USB connections 20 Rebuilding the auxiliary valve 99 Rebuilding the injection valve 99 Recorders Analog output setting 159 Relay connections Rear panel connector 21 165 Relay outputs Controlling 171 Voltage and current specifications 166 Remote Mode 147 Reordering information 177 Reproducibility 36 Reservoir Connecting 47 Monitoring liquid level in 45 Storage on top cover 15 Restriction in liquid lines 67 95 Retention time Adjusting 181 Moving 181 Troubleshooting 79 Reverse peaks 158 RFIC ER compartment 19 RFIC ER Kits 19 RFIC ER mode Components required 19 Flow schematics 22 Specifications 132 Rise time 158 Doc 065290 03 10 12 Index 7 Dionex ICS 1600 lon Chromatography System Running samples 55 See also Processing samples S Safety messages 6 Sample loop 17 32 33 Changing 98 Injecting 33 Injection valve connections 33 99 Lo
118. ns Automated dilution 136 Automation 136 Automation flexibility 136 Online filtration 136 Online sample degassing 136 Semiautomated system qualification 136 Sequential Simultaneous injection 136 Autozero 49 56 146 Auxiliary valve 17 34 52 Applications 34 Configuration 52 Does not switch position 68 Installation instructions 34 Leaking 72 Maintenance yearly 59 Passages blocked 78 Rebuilding 99 Reordering 177 Replacing the mechanical part pod 99 100 Troubleshooting 68 B Background conductivity High 80 Offsetting 49 146 148 Backlight Time out 161 Backpressure 32 Restriction in plumbing 95 Troubleshooting 77 Doc 065290 03 10 12 Index 1 Dionex ICS 1600 lon Chromatography System Bar 154 Baseline Drift 81 Noise 22 24 81 158 Stability 36 Zeroing 146 Batch processing 40 Blockages Liquid lines 67 95 Bottle See Reservoir Busy page 161 C Cables Power cord 127 Calibration 85 Conductivity cell 89 Flow rate 92 Vacuum degas assembly 94 Cation separations 50 Cell See Conductivity cell Cell calibration 89 Cell heater 146 Check valves Cleaning procedure 103 104 Replacement procedure 103 104 Chromatogram 3 Zeroing the baseline 146 Chromeleon 26 Alarm conditions 63 Application Wizard 57 Audit Trail 61 Audit Trail error messages 61 Commands 56 Control panel 55 Degas options 82 Error messages 63 In
119. ns see Figure B 5 SUPPRESSOR Mone MMS Touch an option to select it Current Note To cancel Gm current selection touch outside of XxX Automatically turn on with pump the list o d Figure B 5 Suppressor Page Selecting an Option B 2 Using the Touch Screen with Chromeleon PETS When the Dionex ICS 1600 is connected to a Chromeleon Control panel the status field at the bottom center of the HOME page displays Remote Mode In this mode most of the controls on the touch screen pages are disabled This prevents touch screen commands from conflicting with Chromeleon commands In general when the Dionex ICS 1600 is connected to Chromeleon you can e View all Dionex ICS 1600 operational status information pressure flow rate conductivity readings etc e Go to any of the touch screen pages e View a plot of the conductivity data from the PLOT page and adjust the plot display using the controls on the page See Section B 5 for details To restore touch screen local control clear the Connected check box on the Chromeleon Control panel 142 Doc 065290 03 10 12 B Touch Screen Operation B 3 Overview of Dionex ICS 1600 Touch Screen Pages Figure B 6 illustrates the organization of the Dionex ICS 1600 touch screen pages amp S HOME EN d 7 PLOT NS STATUS NS a gt E MA X PUMP iu d MENU SUPPRESSOR Y 7 DETECTOR
120. nstrument turn off the power switch on the rear panel see Figure 2 10 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 Thermo Scientific Reference Library DVD P N 053891 How do know when a column is dirty See the troubleshooting section of the column manual 182 Doc 065290 03 10 12 E FAQ E 13 How do I clean a column See the troubleshooting section of the column manual E 14 Why is the conductivity high Possible reasons for high conductivity include The suppressor is not on Turn on the suppressor from the Chromeleon Control panel or the Dionex ICS 1600 touch screen SUPPRESSOR page The suppressor needs regeneration See the suppressor manual for troubleshooting information The suppressor manual is included on the Thermo Scientific Reference Library DVD P N 053891 The cell is out of calibration See Section 5 1 3 for calibration instructions See Section 4 13 for additional troubleshooting information E 15 How do I configure and operate the auxiliary valve See Installing the ICS 1100 ICS 1600 ICS 2100 Auxiliary Valve Document No 065288 provided in the Auxiliary Valve Kit Doc 065290 03 10 12 183 Dionex ICS 1600 lon Chromatography System 184 Doc 065290 03 10 12 F Glossary Analytical Column Synonymous with Separator Column Band Spreading The broadening of the
121. omatogram 158 Doc 065290 03 10 12 B Touch Screen Operation B 9 3 Setting Analog Out Options The analog output connector on the Dionex ICS 1600 rear panel outputs an analog voltage signal proportional to the conductivity measured by the cell The output is filtered using the selected data rise time see Section B 9 1 The analog output can be connected to an analog to digital converter device such as an integrator or a chart recorder The Analog Out options on the DETECTOR page see Figure B 17 let you configure the output for your application Output Select Normal to output a signal corresponding to the offset conductivity reading from the detector see Conductivity Readings on page 146 and the selected Analog Out parameters Use the other two settings to calibrate an analog to digital converter device Select Zero to set the output signal to zero volts Select Full Scale to set the output signal to the full scale voltage 1000 mV Offset To adjust the zero position of the analog output when it is plotted enter a percentage in the 96 Offset field The value entered is a percentage of the full scale analog output An offset allows a recording device to plot the signal if it becomes negative The offset percentage does not affect the magnitude of the output signal Polarity Select the polarity of the analog output signal positive the default settings or negative In applications in which the analyte out
122. omponent panel This tubing is initially installed in the Dionex ICS 1600 at the factory 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 included on the Thermo Scientific Reference Library DVD P N 053891 e 8 in fittings P N 052267 and ferrules P N 048949 are used for connections to the suppressor REGEN OUT port and the eluent reservoir 98 Doc 065290 03 10 12 5 Service 5 4 Rebuilding the Injection Valve or Auxiliary Valve Thermo Fisher Scientific recommends rebuilding the injection valve and the auxiliary valve if installed annually The Injection Valve Rebuild Kit P N 057896 contains all required replacement parts for one valve NOTE If you prefer you can replace the auxiliary valve pod instead of rebuilding the valve Replacing the pod is easier and faster than rebuilding the auxiliary valve For instructions see Section 5 5 IMPORTANT Substituting non Dionex Thermo Fisher Scientific parts may impair performance thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information 1 Turn off the pump from the Dionex ICS 1600 Control panel in Chromeleon or from the touch screen HOME page 2 Open the Dionex ICS 1600 front door 3 Disconnect each liquid line connected to the v
123. on including pressure limits pressure unit vacuum degas pump settings and eluent valve control To open this page select PUMP from the menu of pages The current system pressure is displayed at the top of the screen Current PUMP oo system Pressure 0 psi pressure Pressure Limits High Degas Settings Time Off OJ min Eluent Valve Closed c A PUMP Figure B 13 Dionex ICS 1600 Touch Screen Pump Page B 7 1 Setting Pump Pressure Limits and Selecting the Pressure Unit The first time the power to the Dionex ICS 1600 is turned on the maximum system pressure limit is 34 5 MPa 5000 psi and the minimum pressure limit is 0 NOTE Pump pressure limits can also be changed in Chromeleon in the Server Configuration program or in the control program e To change the high pressure limit touch the HIGH field and enter the desired limit on the number pad The high limit must be at least 0 7 MPa 100 psi above the low limit Doc 065290 03 10 12 153 Dionex ICS 1600 lon Chromatography System e To change the low pressure limit touch the LOW field and enter the desired limit on the number pad To select the pressure unit for all touch screen pages that display pressure values touch the pressure unit field and select the desired unit on the list PSI bar or MPa see Figure B 14 PUMP Select the PRESSURE 0 psi pressure unit Pressure Limits Figure B 14 Pump Page Selecting the Pressure Unit B 7 2 Set
124. on and this error message appears To troubleshoot l Ifasequence is being executed terminate the sequence by selecting Batch Stop in Chromeleon 68 Doc 065290 03 10 12 4 Troubleshooting 2 Try to toggle the valve from position A to position B by clicking the corresponding buttons on the Dionex ICS 1600 Control panel in Chromeleon or by clicking the Valve 2 commands under Pump ECD in the Commands dialog box Turn off the Dionex ICS 1600 power briefly and then restart 4 Ifthe problem persists repeat Step 2 If the problem persists contact Thermo Fisher Scientific for assistance SUPPRESSOR NOT CONNECTED This error occurs if you turn on the suppressor and the Dionex ICS 1600 cannot establish a connection with the suppressor To troubleshoot 1 Check the suppressor cable connection see Section 5 11 2 Ifthe error persists contact Thermo Fisher Scientific for assistance There may be a problem in the suppressor controller electronics The Dionex ICS 1600 electronics components cannot be serviced by the user SUPPRESSOR OVER CURRENT This error may be caused by an expended 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 Thermo Scientific Reference Library DVD P N 053891 2 Follow the instructions in the suppressor manual
125. onex AS Method for Stand Alone Operation 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 RLY 1 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 Dionex ICS 1600 injection valve automatically see Enable Dionex AS Control of the Injection Valve on page 174 To run the above method set up a Dionex AS schedule The example in Figure C 11 includes a four point calibration Lines 1 4 followed by two samples Lines 5 and 6 SCHEDULE EDIT 1 SAVETO 1 RUN 1 MISSING VIAL ACTION SKIP VIAL INJ INJ LINE START END VIAL VOL uL METHOD 1 1 4 1 4 3 25 0 5 5 5 1 25 0 1 6 6 1 5 0 1 Help Prompt Figure C 11 Example Dionex AS Schedule for Stand Alone Operation 176 Doc 065290 03 10 12 Part Number 046548 039164 057937 057938 045721 045722 045994 052840 055870 048722 055752 057945 079803 042857 057968 024305 016388 057896 069472 069473 057896 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 Secon
126. ontrol b Plugthe connector into the 12 pin connector on the Dionex ICS 1600 rear panel c Connect the wires from the Dionex ICS 1600 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 If you 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 if necessary Input functions and control types are assigned from either the INPUT OUTPUT touch screen page or Chromeleon see Section C 1 1 Doc 065290 03 10 12 167 Dionex ICS 1600 lon Chromatography System C 1 1 Selecting TTL Input Functions and Control Types To select TTL input functions and the control type from Chromeleon open the Chromeleon Server Configuration program and double click the Dionex ICS 1600 icon under the timebase Select the TTL Inputs tab see Figure C 3 Dionex ICS 1600 IC System Solvents StateDevices InjectValve EtrorLevels Demo Chromatogram General Options Signals HeadTypetlimits TTLinputs Trend Calibration Diagnosis TTL Input Mode TTL Input Functions TTL Input 1 LoadAniecVave TTL Input 2 auc o o e TTL Input 3 Pump Suppressor ON OFF v TTL Input 4 Recorder mark X Figure C
127. ontrol panel click Load Sequence b Select the sequence created in Step 4 and click Open c Click Start Batch 3 12 Maintenance This section describes routine maintenance procedures that users may perform All other maintenance procedures must be performed by Thermo Fisher Scientific personnel As Needed e Regularly check the eluent reservoir and refill when needed e Make fresh eluent as needed e RFIC ER systems only The Chromeleon RFIC ER Wellness feature tracks the usage of the RFIC ER eluent and columns An Audit Trail message will inform you when an item is approaching the end of its useful life span You can also check the life expectancy of these components on the RFIC ER Wellness panel Daily e Check the Dionex ICS 1600 component panel see Figure 2 8 for leaks or spills Wipe up spills Isolate and repair leaks see Section 4 3 Rinse off any dried eluent with deionized water 58 Doc 065290 03 10 12 3 Operation and Maintenance e Check the waste container daily and empty when needed Weekly e Once a week check fluid lines for crimping or discoloration Replace any pinched lines Replace damaged lines e Check the junctions between the pump heads and the pump casting for evidence of liquid leaks If the piston seal wash tubing is not connected check the drain tubes at the rear of the pump heads for evidence of moisture Normal friction and wear may gradually result in small liquid leaks around t
128. operating features and system components introduces the Chromeleon user interface Provides operating instructions and describes routine preventive maintenance procedures Lists problems and presents step by step procedures for how to isolate and eliminate the cause of each problem Provides step by step instructions for routine service and parts replacement procedures that the user can perform Lists the Dionex ICS 1600 specifications and installation site requirements Describes the operating features available from the front panel touch screen Describes the Dionex ICS 1600 TTL and relay control features Lists spare parts for the Dionex ICS 1600 Doc 065290 03 10 12 Dionex ICS 1600 lon Chromatography System Appendix E Provides answers to frequently asked questions about FAQ Dionex ICS 1600 operation Appendix F Defines terms commonly used in ion analysis Glossary 1 3 4 Safety Messages and Notes This manual contains warnings and precautionary statements that when properly followed can prevent personal injury and or damage to the instrument Safety messages appear in bold type and are accompanied by icons as shown below Indicates an imminently hazardous situation which if not avoided will result in death or serious injury gt DANGER Indicates a potentially hazardous situation which if not avoided could result in death or serious injury gt WARNING Indicates a potentially hazardou
129. options After a few seconds the HOME page see Figure B 1 is displayed The HOME page provides controls for all normal daily operation of the Dionex ICS 1600 B 1 Using the Touch Screen Pump 0 psi Limit 1000 4000 Edit Field Flow Rate Command ais Button 1 0n uni Command Eluent Level Button unselected 0 00 Column Heater Elapsed Time 0 00 min Remote Mode KD Total 146 99 pS Autozero Cell Heater Type None MMS OFF Status Field Figure B 1 Dionex ICS 1600 Touch Screen Home A Page NOTE To adjust the screen contrast open the front door and adjust the knurled knob under the screen see Figure 2 8 Doc 065290 03 10 12 139 Dionex ICS 1600 lon Chromatography System Edit fields and command buttons have blue text on a lightly shaded background Fields that display status information are not shaded Edit fields have square corners while command buttons are rounded To edit a field or select a command button touch and release the field or button with your fingertip NOTE When you touch a button or edit field the action takes effect when you lift your finger If you unintentionally touch a button or field you can cancel the action by sliding your finger away from the button or field before lifting Touching a command button for example inject executes the command immediately Selecting a com
130. or the sequence 7 Ifyou are controlling the Dionex ICS 1600 from the touch screens select the PLOT button on the HOME page to view a plot of the conductivity data 3 11 2 Automatic Batch Sample Processing You can use Chromeleon or Chromeleon Xpress to create a list of samples a sequence to be processed automatically For each sample the sequence includes the following e A program with commands and parameters for controlling the Dionex ICS 1600 and autosampler if used and for acquiring sample data A quantification method for peak identification and area determination e Additional sample processing parameters sample name sample type injection volume etc After creating the sequence you can start batch processing 56 Doc 065290 03 10 12 3 Operation and Maintenance Summary of Automatic Sample Processing 1 Complete the instructions in Section 3 2 through Section 3 8 to prepare the Dionex ICS 1600 for operation and to prepare the sample for processing 2 Ifanautosampler is installed prepare and fill the sample vials and place them in the autosampler tray or cassette Refer to the autosampler manual for detailed instructions Autosampler manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 3 Ifan autosampler is not installed load the sample into the injection valve sample loop through the sample port on the Dionex ICS 1600 front door see Section 3 10 1 4 Use
131. osampler output line is connected to port S 5 of the Dionex ICS 1600 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 e Include the commands for controlling sample loading in a Chromeleon program If necessary refer to the Chromeleon Help or user manual for assistance e Enter the commands for loading the sample on the autosampler front panel Switch the injection valve to the Inject position see Section 3 10 4 54 Doc 065290 03 10 12 3 Operation and Maintenance 3 10 4 Injecting Samples After loading the sample in the sample loop use one of the following methods to switch the injection valve to the Inject position Manually Click the Inject button on the Chromeleon Control panel see Figure 3 4 or touch the Inject button on the HOME page Automatically Include the Inject command in a Chromeleon program If necessary refer to the Chromeleon Help or user manual for assistance 3 11 Processing Samples Samples can be run manually one at a time or else they can be grouped and run automatically in batches 3 11 1 Manual Sample Processing To process samples manually select operating parameters and commands from the touch screen
132. outine 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 Monitor default mode The Dionex ICS 1600 monitors the degas pressure reading and turns the degas pump on and off as required Doc 065290 03 10 12 29 Dionex ICS 1600 lon Chromatography System 2 4 2 Eluent Valve PE AQ IN The eluent valve controls the flow from the eluent reservoir The valve opens automatically when the pump is started and closes when the pump is turned off The valve can also be opened and closed manually from the Chromeleon Control panel see Section 2 3 1 or the touch screen PUMP page see Section B 7 This lets you perform service procedures on pump components without eluent leaks occurring Figure 2 15 Eluent Valve 2 4 3 Pump The Dionex ICS 1600 pump is a microprocessor based isocratic eluent delivery system Its variable speed dual piston series design ensures pulse free pumping for the most demanding applications Primary Pump Head The primary pump head pumps eluent into the secondary head see Figure 2 16 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 To open the priming valve
133. pace Tools Help D SHES e If Chromeleon Xpress is installed start the application this automatically displays the Dionex ICS 1600 panel tabset 2 3 2 Software Control Modes Two modes of software control are available direct control and programmed control e With direct control you select operating parameters and commands from the Control panels Direct control commands are executed as soon as they are entered e With programmed control you create a list of control commands to be executed in chronological order Programs can be created automatically with the help of a software wizard 2 3 8 System Wellness System Wellness monitors the overall health of a chromatographic system It provides built in diagnostic and calibration features that help prevent unscheduled system shutdowns and assure reliable operation of system devices For details about System Wellness see Section 5 1 Doc 065290 03 10 12 27 Dionex ICS 1600 lon Chromatography System 2 4 System Component Details This section provides details about Dionex ICS 1600 system components including the vacuum degas assembly optional pump RFIC ER components injection valve column heater suppressor and conductivity cell 2 4 1 Vacuum Degas Assembly Optional The vacuum degas assembly provides online eluent degassing at the time and duration specified by the user The assembly which must be installed in the Dionex ICS 1600 at the factory consis
134. pages or from the Chromeleon menu bar toolbars and Control panel Commands are executed as soon as they are entered NOTE When you run samples manually from the front panel without using Chromeleon the data is saved only temporarily in the Dionex ICS 1600 memory For a permanent record of the data connect a recording device chart recorder integrator etc to the analog output For output connection instructions refer to Complete the instructions in Section 3 2 through Section 3 8 to prepare the Dionex ICS 1600 for operation and to prepare the sample for processing Load the sample using a syringe vacuum syringe or autosampler see Section 3 10 In Chromeleon select Control gt Acquisition On Chromeleon records the signal supplied by the detector and displays the signal plot on the Control panel Doc 065290 03 10 12 55 Dionex ICS 1600 lon Chromatography System 4 Click the Autozero button on the Control panel or the touch screen HOME page 5 Inject the sample see Section 3 10 4 6 In Chromeleon monitor the chromatogram on the Control panel and select Control gt Acquisition Off when sample data is collected NOTE Data from Chromeleon manual processing is saved in the MANUAL sequence folder under the local datasource This data is overwritten each time a new manual sample is processed To save the data from a manual run select the MANUAL folder select File gt Save As and enter a new name f
135. pped in the syringe through the pump Check the waste line from the secondary pump head to verify that there are no air bubbles Close the priming valve Do not overtighten Disconnect the syringe from the priming valve Let the pump run for several minutes to purge alcohol from the pump heads Then click the Prime button in the Pump Settings window to flush the heads with the desired eluent 126 Doc 065290 03 10 12 5 Service Isopropyl alcohol may damage some columns Be sure to thoroughly IMPORTANT A rinse the alcohol from the pump using the process described in Step 7 8 Close the waste valve Do not overtighten 9 Select the flow rate required for the analysis 10 In the Pump Settings window click Pump Off 5 18 Changing Main Power Fuses 1 Turn off the main power switch HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the Dionex ICS 1600 DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arriere du Dionex ICS 1600 DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des Dionex ICS 1600 ACHTUNG 2 The fuse holder is part of the main power receptacle see Figure 5 33 on the Dionex ICS 1600 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 Main Po
136. ppressor for your application refer to the suppressor manuals The manuals are on the Thermo Scientific Reference Library DVD P N 053891 DS6 Heated Conductivity Cell The 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 higher 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 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 when the operating temperature is d
137. psi increments e Lower limit Up to one unit lower than upper limit Optional feature automatic control Polypropylene Not required Built in optical sensor Doc 065290 03 10 12 131 Dionex ICS 1600 lon Chromatography System A 6 Eluent Regeneration Eluent Regeneration Eluents Flow Rates Continuous Operation 4 L of Eluent Always On Always Ready Capable Remains Fully Calibrated for Extended Periods x28 days System Wellness Maximum Operating Pressure Operating Temperature Range Optional feature RFIC ER Startup Kit required e Carbonate and carbonate bicarbonate up to 20 mM e MSA up to 34 mM 0 01 to 2 00 mL min Up to 28 days or 2000 samples typically Standard feature Standard feature results are traceable to a single calibration Consumables usage monitoring for predictive maintenance 21 MPa 3000 psi 4 to 40 C 40 to 104 F A 7 Detector Electronics Type Cell Drive Detector Linearity Resolution Microprocessor controlled digital signal processor 8 kHz square wave 1 up to 1 mS 0 00238 nS cm 132 Doc 065290 03 10 12 A Specifications Full Scale Output Ranges Electronic Noise Filter Temperature Compensation Temperature Range Temperature Stability e Digital signal range 0 to 15 000 uS e Analog signal range 0 to 15 000 uS 0 1 nS cm when background conductivity is 0 to 150 uS cm 2 nS cm when background conductivity is 1
138. 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 065290 03 10 12 1 Introduction 3 Separation e As the eluent and sample are pumped through the separator column the sample ions are separated In the Dionex ICS 1600 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 Dionex ICS 1600 this is the Chromeleon Chromatography Management System 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
139. put is lower than the background conductance the polarity must be negative to have peaks instead of dips on the chromatogram Range Select the range in microSiemens uS of a full scale detector response For the Dionex ICS 1600 the full scale voltage is 1000 mV For example if the range is 100 uS then 1 uS is equal to 10 mV from the analog output The range to use depends on the conductivity readings expected for the application Doc 065290 03 10 12 159 Dionex ICS 1600 lon Chromatography System B 10 Information Page The INFORMATION page displays the version numbers of the Dionex ICS 1600 control programs Moduleware and Boot Block the serial number of the Dionex ICS 1600 and the options that are installed in the Dionex ICS 1600 The INFORMATION page is displayed at start up You can open the page from the menu of pages at any time ICS 1600 Moduleware Version XXXXXX Boot Block Version XXXXXX Serial Number 123456789 Options Installed Figure B 18 Information Page Moduleware is the firmware program installed in the Dionex ICS 1600 that controls instrument functions Moduleware also sends status information and data to Chromeleon and receives control parameters from Chromeleon The Boot Block is the first program to be executed when the Dionex ICS 1600 power is turned on It starts the Moduleware program 160 Doc 065290 03 10 12 B Touch Screen Operation B 11 Module Setup Page The MODULE SET
140. r On 0 120 sec Off 0 5940 sec M Column Heater M Valve 2 RFICER Link to ERC Controller None Cancel Help Figure 4 1 Dionex ICS 1600 Server Configuration Properties Options Doc 065290 03 10 12 73 Dionex ICS 1600 lon Chromatography System 3 Verify that the Degas check box is selected 4 Check the Degas settings Select either the Monitor option or the Cycle option If you select Cycle set the time On to 30 seconds and the time Off to 600 seconds If Cycle is already selected try increasing the time on or decreasing the time off NOTE Degas options can also be selected from the touch screen PUMP page see Section B 7 End line filter is dirty or clogged When new end line filters P N 045987 are pure white 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 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 6 Liquid leaks at junction between pump head
141. r see Section B 4 1 The Dionex ICS 1600 monitors the eluent usage based on the flow rate and the length of time the pump is on The liquid level in the bottle falls as the reservoir empties An error message is first displayed on the screen when the level falls below 200 mL The message is repeated at 100 mL and then at 0 mL In order for the eluent level displayed on the screen to be accurate the level must be entered by the user when the reservoir is filled The Dionex ICS 1600 does not automatically detect when the reservoir is filled nor when it is empty Doc 065290 03 10 12 149 Dionex ICS 1600 lon Chromatography System e The fields to the right of the bottle display the status of four other operating parameters You can choose from six possible parameters to display here Figure B 9 shows the default parameters Eluent time Flow rate Cell temp and Suppressor To select different parameters touch the Setup button See Section B 6 1 for details about how to change the status parameters and Section B 6 2 for a description of each parameter e Touching the Busy button displays the BUSY page see Figure B 10 BUSY PLEASE DO NOT DISTURB o d Bs M Figure B 10 Busy Page 150 Doc 065290 03 10 12 B Touch Screen Operation B 6 1 Viewing Other Status Parameters Follow the steps below to view the status of a parameter that is not currently displayed on the STATUS page 1 Touch the
142. rammable online degassing The degas assembly must be installed in the Dionex ICS 1600 at the factory If the Dionex ICS 1600 does not contain a degas assembly manually degas eluent daily following the instructions below and store it in pressurized reservoirs Manual Degassing of Eluent 1 Prepare the eluent required for the application and pour it into a vacuum flask Attach the flask to a vacuum pump or water aspirator Vacuum degas the eluent for 5 to 10 minutes by shaking or sonication Remove the flask from the vacuum Do not allow eluent to flow from the aspirator back into the flask Pour the degassed eluent into a pressurizable reservoir Do not shake the eluent 44 Doc 065290 03 10 12 3 Operation and Maintenance 6 Install an end line filter on the eluent line see Section 3 4 3 7 Optional Pressurize the reservoir The Dionex ICS 1600 does not require pressurized reservoirs However if eluent is manually degassed or is sensitive to contamination Dionex recommends pressurizing the reservoir with helium or nitrogen The air regulator accessory bracket and other items needed for pressurizing the eluent reservoir must be ordered separately P N 060054 For more information refer to the Dionex ICS 1600 installation instructions 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
143. rd column The heater temperature can be set to between 30 C and 60 C However the set temperature must be at least 5 C above the ambient temperature A thermistor mounted in the heater block monitors the temperature Setting the temperature to 0 C turns off the column heater If the temperature exceeds 65 C the column heater is shut off and the error message Column heater exceeds safe temperature is displayed on the touch screen and in the Chromeleon Audit Trail See Section 4 2 for troubleshooting information For best results with 2 mm columns a microbore heat exchanger P N 060943 should be installed in the column heater see Section 5 13 The tubing connections between the injection valve and column heat exchanger guard column and separator column and separator column to detector cell should all use red 0 125 mm 0 005 in ID PEEK tubing P N 044221 rather than the standard black tubing Figure 2 19 Column Heater Doc 065290 03 10 12 35 Dionex ICS 1600 lon Chromatography System 2 4 7 2 4 8 Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions thereby increasing detection sensitivity Either a Dionex Atlas Electrolytic Suppressor Dionex Self Regenerating Suppressor or Dionex MicroMembrane Suppressor can be used with the Dionex ICS 1600 For details about any of the suppressors or for information about selecting a su
144. reasing detection sensitivity Either a Dionex AES Atlas Electrolytic Suppressor Dionex SRS Self Regenerating Suppressor or Dionex MMS MicroMembrane Suppressor can be used with the Dionex ICS 1600 See Section 2 4 7 for details about the suppressor 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 The column heater controls the temperature of the separator and guard columns The temperature can be set to between 30 and 60 C however it must be set to at least 5 C above the ambient temperature See Section 2 4 6 for details about the column heater Eluent Valve The eluent valve controls the flow from the eluent reservoir The eluent valve opens automatically when the pump is started and closes when the pump is turned off Screen Adjustment Knob Use this knob to change the LCD touch screen contrast 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 interior of the Dionex ICS 1600 to the rear panel It also routes tubing from the RFIC ER compartment through the interior of the Dionex ICS 1600 to the component panel 18 Doc 065290 03 10 12 2 Features 2 1
145. rlying problem see the table below You can change the severity level assigned to a problem whenever appropriate Icon Severity Level Description Warning A message is displayed in the Audit Trail but the current run is not interrupted A Error A message is displayed in the Audit Trail and the system attempts to correct the problem sometimes by using an alternative parameter An Error never interrupts the current analysis however if it occurs during the Ready Check the analysis will not be started Abort A message is displayed in the Audit Trail and the running batch is aborted Doc 065290 03 10 12 61 Dionex ICS 1600 lon Chromatography System The table below lists the most frequently observed Dionex ICS 1600 error messages For troubleshooting assistance refer to the page indicated in the table 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 over pressure Pump pressure hardware error Pump stopped due to lost USB communication error Pump under pressure Second valve error Suppressor not connected Suppressor over current Suppressor over power Suppressor over voltage Suppressor stopped for zero flow rate Table 4 2 Alarms and Error Messages Summar
146. ropyl 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 Closethe priming valve knob or waste valve knob 108 Doc 065290 03 10 12 5 Service Reinstalling the Head and Piston Thermo Fisher Scientific recommends reinstalling the head and piston as a single assembly so that the piston centers itself onto the magnetic follower 1 Hold the assembled spacer and guide with the drain tubes aligned vertically and press the spacer into the head until it is flush with the indented surface of the head 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 Ib 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 5 17 5 8 Replacing a Pump Piston Continued leaking of the piston seal after installation of a new seal assuming the pump head is tight indicates a dirty scratched or broken piston Follow the instructions in Section 5 7 to install a new piston P N 052840 and piston seal P N 055870 Doc
147. roubleshooting information if the conductivity is too high See Section 4 14 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 the Current Temperature readings on the Control panel are the same or when the symbol is displayed next to the Column Heater temperature on the HOME page Verify that the column heater temperature is at the set point and stable The temperature is at equilibrium when the Set Temperature and the Current Temperature readings on the Control panel are the same or when the symbol is displayed next to the Column Heater temperature on the HOME page The system is now ready for sample processing 3 9 Prepare Samples NOTE Sample preparation can be performed while the system is equilibrating 3 9 1 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 50 Doc 065290 03 10 12 3 Operation and Maintenance 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 caus
148. s off Suppressor Controls Suppressor Type SRS The Suppressor controls indicate the suppressor current setting and the type of suppressor installed To set the suppressor type change the current setting or turn the suppressor on or off touch the suppressor button The SUPPRESSOR page appears see Section B 8 B 4 5 Other Home Page Controls This field displays Remote Mode when the Dionex ICS 1600 is connected to Chromeleon and Local Mode when the system is not connected to Chromeleon Remote Mode Opens the PLOT page which provides a real time plot of the detector PLOT X conductivity output See Section B 5 for details Opens the STATUS page which displays the status of various operating STATUS f parameters See Section B 6 for details Doc 065290 03 10 12 147 Dionex ICS 1600 lon Chromatography System B 5 Plot Page The PLOT page provides a real time plot of the detector conductivity output To open the page touch the PLOT button on the HOME page or select PLOT from the menu of pages The page can display up to 60 minutes of data Data older than 60 minutes is discarded You can view the plot and adjust the display when the Dionex ICS 1600 is under either local or computer control 20 ps 15 ps 10 0 0 5 min 1 range IT a 15525599559 feel dint Figure B 8 Plot Page Plot Controls The plot offset button offsets the current background conductivity reading and sets
149. s safe temperature 63 Column heater open circuit 64 Column heater short circuit 64 Degas calibration failed 64 Hardware not present 64 Leak sensor wet 65 Load inject valve error 65 Option not installed 66 Pump motor lost control 66 Pump over pressure 67 Pump pressure hardware error 66 Pump stopped due to lost USB communication 68 Pump under pressure 68 Second valve error 68 Suppressor not connected 69 Suppressor over current 69 Suppressor over power 70 Suppressor stopped for zero flow rate 70 F Filter end line Bacterial contamination 59 74 Dirty or clogged 59 74 Installation 45 Filtering data 158 Fittings Leaking 71 Replacing 98 Requirements 98 Flow rate 17 130 145 Calibration 92 Troubleshooting 75 Front panel 11 See also Touch screen Full scale analog output 159 Fuses Replacement procedure 127 Requirements 129 G Ghosting 78 Guard column 18 H Hardware not present error 64 Heater column 35 See also Column heater High pressure alarm 67 Home page 12 139 144 147 Column Heater control 145 Detector controls 146 Injection valve controls 146 Pump controls 144 Humidity operating 130 I Information page 160 Injecting samples 52 Via autosampler 54 Via syringe 53 Via vacuum syringe 54 Injection port 11 Injecting via syringe 53 Injection valve 17 32 Controlling with a Dionex AS 174 Home page controls 146 Leaking 72 Passages blocked 78
150. s situation which if not avoided may result in minor or moderate injury Also used to identify a situation or practice that may seriously damage the instrument but will not cause CAUTION injury gt 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 gt DANGER Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves a mortelles gt AVERTISSEMENT 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 Sa gravement endommager l instrument mais qui n entrainera pas de blessures gt 6 Doc 065290 03 10 12 1 Introduction Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr MiBachtung kann zum Tod oder schwerwiegenden Verletzungen f hren ACHTUNG Bedeutet eine m gliche Gef hrdung MiBachtung kann zum Tod oder schwerwiegenden Verletzungen f hren WARNUNG Bedeutet eine m gliche Gef hrdung MiBachtung kann zu kleineren oder mittelschweren Verletzungen f hren Wird auch verwendet wenn eine Situation zu schweren Schaden am Gerat f hren kann jedoch VORSICHT k
151. signing functions to 169 174 Control type 174 Default function assignments 166 Rear panel connector 21 TTL outputs Controlling 171 Rear panel connector 21 Tubing Replacing 98 Requirements 98 Routing clips 21 Tubing connections Isolating a restriction 67 95 U USB connections 20 V Vacuum degas assembly 28 Calibration 94 Components 28 Fails to run 82 Setting operating parameters 154 Specifications 134 Troubleshooting 73 Valve See Auxiliary valve See Eluent valve See Injection valve See Waste valve Version number 160 W Warranty voiding 85 99 100 Waste lines Blocked 71 Waste valve 31 Opening 31 105 O ring replacement procedure 110 Water samples 51 Weekly maintenance 59 Weight 129 Wellness 27 Wellness panel 85 Y Yearly maintenance 59 Z Zero position analog out 159 Zeroing the baseline 146 Index 10 Doc 065290 03 10 12
152. stem to equilibrate During equilibration the Chromeleon Control panel displays the background conductivity the conductivity of the eluent before sample injection and the system backpressure 2 Monitor the background conductivity Refer to the column manual for the appropriate background conductivity for your application 3 Offset the background and zero the reading by clicking the Autozero button on the Chromeleon Control panel see Figure 3 4 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 is stable Doc 065290 03 10 12 49 Dionex ICS 1600 lon Chromatography System e Ifthe pressure is less than the expected amount gas may be trapped in the system To release the gas remove the pump fitting on the injection valve port labeled P 2 Allow the air to escape and then reconnect the fitting e Ifthe pressure fluctuates by more than about 0 13 MPa 20 psi prime the pump See Section 4 4 for additional troubleshooting information e Ifthe pressure is too high there may be a restriction in the system plumbing See Section 4 8 for troubleshooting information 5 Verify that the baseline conductivity is at the expected reading for your application and is stable In general it should be 30 uS for a system set up for anion analyses and 2 uS for a system set up for cation analyses See Section 4 13 for t
153. te accurate or error free and assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this document even if the information in the document is followed properly This document is not part of any sales contract between Thermo Fisher Scientific Inc and a purchaser This document shall in no way govern or modify any Terms and Conditions of Sale which Terms and Conditions of Sale shall govern all conflicting information between the two documents Revision history Revision 01 released March 2009 initial release of system Revision 02 released December 2011 Thermo Fisher Scientific transition Revision 03 released October 2012 new part numbers assigned For Research Use Only Not for use in diagnostic procedures Contents 1 Introduction 1 1 1 Introduction to Ion Chromatography IC 0 000000 1 1 2 Overview of the Dionex ICS 1600 0 0 0 0 00 2 4 1 3 About This M nual assu e a rrenen i dae cach eds 5 1 3 4 Safety Messages and Notes 00 0 0 e eee ee eee 6 1 4 Safety and Regulatory Information 0 0 0 20 e eee 8 141 Safety Labels 2 co ceca ies ER 8 2 Features 11 2 Operating Features eh 11 2 1 Front Panel 41552 e ERES etr Ce uber e dub 11 2 1 2 Top COVED oc oorr ok es a Er Ege uds 15 2 1 3 Component Panel 0 cee ee eee eee 16 2 1 4 Right Side Panel scrise cece eee
154. terface 26 Menu 55 Overview 26 Panel tabset 26 Programs 54 Quantification method 58 Starting 42 Timebase 26 Toolbars 55 Using the touch screen with Chromeleon 142 Wellness panel 85 Chromeleon Server Starting 42 Chromeleon Server Monitor 42 Column heater 18 35 Home page control 145 Replacement procedure 116 Specifications 134 Column heater alarms Column heater exceeds safe temperature 63 Column heater open circuit 64 Column heater short circuit 64 Columns 18 Cleaning 182 183 Contaminated 79 Damage from IPA 127 Storing 182 Component panel 16 Conductivity 146 Causes of high conductivity 183 Changing the display 161 Offset 146 161 Temperature effect 36 Total 146 161 Conductivity cell 17 18 36 Calibrating 89 Calibration constant 113 High cell output 80 Leaking 72 No response 79 Replacement procedure 112 Setting the temperature 146 Volume 36 Conductivity cell specifications Active volume 133 Index 2 Doc 065290 03 10 12 Index Cell body 133 Chemical compatibility 133 Electrodes 133 Maximum pressure 133 Temperature 133 Conductivity polarity 158 Contacting Thermo Fisher Scientific 8 Contamination Column 77 79 Eluents 78 Sample 79 Standard 78 Control panel Chromeleon 26 55 Autosampler 27 Sequence Control 27 Status 27 Current 156 D Daily maintenance 58 Data Backing up 182 Deleting 182 Filtering 158 Saving
155. the Application Wizard to specify a program and quantitation method and create a sequence a Onthe Sequence Control panel click Application Wizard b Select an application template from the list see Figure 3 10 Chromeleon Application Wizard Application Tool Specify Suppressor Type Choose an application tool for generating Program and Method files Application Templates 45124 Production Test Chromatogram 45124 Production Test Chromatogram A514 Production Test Chromatogram 45144 Production Test Chromatogram 4S44 SC Production Test Chromatogram ASS HC Production Test Chromatogram C5124 Production Test Chromatogram Virtual Column Separation Si anand aas aiii Ahana hh i Tai San nia iiai aina ann diniin ihhh aian ainin haha anina Figure 3 10 Application Wizard Doc 065290 03 10 12 57 Dionex ICS 1600 lon Chromatography System c Click Next gt and select the in a new sequence via Sequence Wizard option d Click Next gt to go to the Sequence Wizard e Complete the steps in the Sequence Wizard adding the desired number of samples and standards to the list For help click the Help button on the Sequence Wizard page After you click Finish a sequence is created and a program appropriate for the selected application is copied to the sequence If you are using Chromeleon a quantification method is also copied to the sequence 5 Load the sequence and start batch processing a On the Sequence C
156. the piston CAUTION Un mouvement lat ral pendant la s paration de la t te et du piston peut casser le piston MISE EN GARDE Vermeiden Sie Seitwartsbewegungen wenn Sie den Kopf vom Kolben l sen Andernfalls kann der Kolben brechen VORSICHT Doc 065290 03 10 12 105 Dionex ICS 1600 lon Chromatography System Place the head front end down on a clean work surface and lift off the spacer to expose the piston seal see Figure 5 13 or Figure 5 14 Priming Valve Knob P N 055709 4 Outlet Check Valve Assembly P N 045721 z O Ring P N 055752 Piston Seal P N 055870 Spacer with Drain p v P N 057913 lt Primary Pump Head P N 055711 Piston Rinse Seal V 4 P N 048722 NS a O Ring SE P N 014895 J O Ring T N P N 059283 valve Assembly Seal Guide P N 045722 Piston P N 058032 P N 052840 Figure 5 13 Primary Pump Head Waste Valve Knob P N 055710 f O Ring P N 055752 Piston Seal P N 055870 Spacer with Drain i j Secondary P N 057913 1 H Pump Head ON P N 055712 Piston Rinse Seal Z DO NA P N 048722 if A O Ring an p P N 014895 SealGuide S P N 058032 NS O Ring P N 059283 Piston P N 052840 Figure 5 14 Secondary Pump Head 106 Doc 065290 03 10 12 5 Service 6 The piston does not come off as part of the pump head assembly because it is captured by a ma
157. the plot baseline to zero Subsequent output is plotted in relation to the new zero point Offsetting the plot does not affect the data sent to Chromeleon the analog output or the data displayed on other pages The range field sets the highest conductivity reading displayed on the plot the vertical scale If the tops of peaks are cut off select a higher range If peaks are short select a lower range Select Auto to have the scaling of the signal plot automatically adjusted to the height of the signal The elapsed time field displays the time since injection The plot time field sets the length of time plotted on the page the horizontal scale 148 Doc 065290 03 10 12 B Touch Screen Operation B 6 Status Page The STATUS page displays the current status of various operating parameters To open this page touch the STATUS button on the HOME page or select STATUS from the menu of pages 1234 B 6 is Total 1258 14 Ss Eluent time 10 5 hours Flow rate 100 mL min Cel temp 25 c Suppressor 50 mA an Rv GH FROM Figure B 9 Status Page Status Page Controls e Pressure and conductivity readings are the same as those displayed on the HOME page e The eluent bottle depicts the level of liquid in the eluent reservoir The scale is always 0 to 4 liters regardless of the size of reservoir installed After filling the reservoir go to the HOME page and enter the amount of liquid in the reservoi
158. the reservoir L field is updated as the liquid is depleted Figure 3 5 Home Page Setting the Eluent Level 3 ICS 1 600 Pump Settings System _ X Pump Settings 1 00 ml min Enter the volume of liquid in the Eluent Prime reservoir in liters 2 00 Eluent Flow Valve o Closed Open 3 d Max Pressure 5000 psi Curr Pressure 800 psi Min Pressure k 0 psi Eluent Level 2 00 1 Note The Eluent Bot field and slider gaug d are updated as the _ Close liquid is depleted Figure 3 6 Pump Settings Windows Setting the Eluent Level The STATUS page see Figure 3 7 also displays the amount of liquid remaining in the reservoir and an estimate of how many hours remain before the eluent reservoir is empty 46 Doc 065290 03 10 12 3 Operation and Maintenance See Section B 6 for details about the STATUS PAGE 1234 15767 Total 1258 14 5 4 Eluent time 10 5 hours Flow rate 100 mL min Cel temp 25 C Suppressor 5Q mA Eluent a Figure 3 7 Status Page 3 4 6 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 Dionex ICS 1600 3 5 Check All Connections Make sure the eluent reservoir is filled and the tubing connecting the reservoir to the Dionex ICS 1600 tubing is securely con
159. ting Degas Operating Parameters Optional By default the Dionex ICS 1600 monitors the degas pressure reading and turns the degas pump on and off as required To change the degas operating option 1 Select PUMP from the menu of pages 2 Under Degas Settings touch the options drop down list A list of available options appears see Figure B 15 Degas Settings Duty Cycle fe sec Time Off fe min Select the degas option Figure B 15 Pump Page Selecting Degas Options NOTE Degas options can also be selected from the Chromeleon Server Configuration program see Section 2 4 1 154 Doc 065290 03 10 12 B Touch Screen Operation 3 Select the desired option Always Off The degas pump is always off Always On The degas pump is always on This setting is reserved for test purposes by a Thermo Fisher Scientific Service Representative Select the Degas Always On option only when testing the vacuum degas assembly Do not select the Always On option for routine use Duty Cycle The degas pump cycles on and off according to the times specified in the Duty Cycle and Time Off fields Duty Cycle specifies for how long the degas pump runs during a cycle Time Off specifies the time between cycles Monitor The Dionex ICS 1600 monitors the degas pressure reading and turns the degas pump on and off as required B 7 3 Controlling the Eluent Valve Eluent Valve The eluent valve controls flow from the
160. to clean the suppressor 3 Ifamalfunction in the suppressor controller is suspected contact Thermo Fisher Scientific for assistance The Dionex ICS 1600 electronics components cannot be serviced by the user Doc 065290 03 10 12 69 Dionex ICS 1600 lon Chromatography System SUPPRESSOR OVER POWER This error occurs when in order to maintain the selected current the Dionex ICS 1600 is required to apply a higher voltage than the suppressor can support To troubleshoot 1 Reduce the flow rate 2 Rehydrate the suppressor Refer to the suppressor manual for instructions Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 3 If the error persists replace the suppressor see Section 5 11 SUPPRESSOR OVER VOLTAGE This error occurs if you turn on the suppressor but the Dionex ICS 1600 cannot establish a connection with the suppressor To troubleshoot 1 Check the suppressor cable connection see Section 5 11 2 Ifthe error persists replace the suppressor see Section 5 11 SUPPRESSOR STOPPED FOR ZERO FLOW RATE This error message appears when you click the Shutdown button on the Dionex ICS 1600 Control panel in Chromeleon 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 If the pump stopped unexpectedly see Section 4 6 for pump
161. tput signal to rise from 10 of its final value to 90 of its final value The selected data rise time is used to filter both the digital data output which is sent to the computer and the PLOT page and the analog data output The default rise time is 2 seconds Choosing an appropriate rise time value can optimize performance by keeping the signal to noise ratio at a minimum level A longer rise time allows averaging of the noise frequencies and subsequently the baseline will contain much less short term noise However longer rise times may have the following effects on peaks e Peak shape will become asymmetric e The peak maximum will be shifted e The peak height will be reduced The rise time should be approximately 25 of the peak width at one half the height of the narrowest peak of interest For example for a peak width of 5 seconds calculate the rise time as 5 sec 25 1 25 sec Because 1 25 seconds is not one of the available settings for rise time select the next fastest rise time 1 second To set the data rise time touch the Data Rise Time field and select the desired time from the list see Figure B 17 Selecting the Conductivity Polarity To change the polarity of the conductivity data touch the Conductivity Polarity field Select either Normal or Inverted In applications in which the analyte output is lower than the background conductance the polarity must be inverted to have peaks instead of dips on the chr
162. troubleshooting information 70 Doc 065290 03 10 12 4 Troubleshooting 4 3 Liquid Leaks Leaking fitting Locate the source of the leak Tighten or if necessary replace the liquid line connection see Section 5 3 Refer to Installation of Dionex Liquid Line Fittings Document No 031432 for tightening requirements The manual is included on the Thermo Scientific Reference Library DVD P N 053891 Broken liquid line Replace the line and fittings with the same length and internal diameter tubing see Section 5 3 Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked Also if the blocked line is a waste line make sure it is not elevated at any point after it exits the Dionex ICS 1600 If a line is blocked replace it see Section 5 2 Loose pump check valve 1 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 2 Ifthe leak persists replace the check valve see Section 5 6 Leaking seal wash port Leaking from the seal wash port indicates a leaking piston seal Replace the seal see Section 5 7 Damaged pump piston seal 1 Replace the piston seal see Section 5 7 2 Ifthe leak persists replace the piston see Section 5 8 Pump head not tight against casting Carefully tighten the pump head mounting nuts just until the leak stops DO NOT OVERTIGHTEN
163. ts of e A single channel degas chamber with degas membranes with internal capacity of 17 mL e A dual stage diaphragm vacuum pump e A solenoid valve e An on board vacuum sensor e The electronics required to operate the vacuum pump e Tubing fittings and other accessories By default the Dionex ICS 1600 monitors the degas pressure reading and turns the degas pump on and off as needed Different degas operating modes can be selected from the touch screen PUMP page see Section B 7 or from Chromeleon To select the degas operating options open the Chromeleon Server Configuration program right click the Dionex ICS 1600 device in the timebase and select Properties 28 Doc 065290 03 10 12 2 Features Select the Options tab see Figure 2 14 Dionex ICS 1600 IC System Solvents State Devices Inject Valve Error Levels Demo Chromatogram TTL Inputs Trend Calibration Diagnostics General Options Signals Head Type amp Limits M Degas C Always Off C Always On C Cycle On 0 120 sec Off 0 5940 sec Monitor IV Column Heater M Valve 2 RFIC ER Link to ERC Controller None Cancel Help Figure 2 14 Server Configuration Properties Degas Options Degas 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 Thermo Fisher Scientific Service Representative Do not use this setting for r
164. 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 5 16 30 Doc 065290 03 10 12 2 Features Outlet Check Valve Secondary Primar Pump Head Pump Hbad Waste Valve Priming Valve Inlet Check Valve Pressure Transducer Figure 2 16 Dionex ICS 1600 Pump Components Secondary Pump Head The secondary pump head delivers eluent to the remainder of the chromatography system the injection valve column and detector The waste valve is located on the front of the secondary pump head see Figure 2 16 To open the waste valve turn the knob one quarter to one half turn counterclockwise When the waste valve is in the open position all pump flow 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 5 16 Doc 065290 03 10 12 31 Dionex ICS 1600 lon Chromatography System 2 4 4 Pressure Transducer Flow exiting the secondary pump head is directed to the pressure transducer see Figure 2 16 which measures the system pressure Pressure readings indicate that the pumping system is delivering smooth accurate f
165. uisition or data processing functions An analog output on the rear panel can be connected to a separate data acquisition device For communication between the Dionex ICS 1600 and Chromeleon the Dionex ICS 1600 is connected to a USB Universal Serial Bus port on the computer or a USB hub For details see the Dionex ICS 1600 installation instructions Also refer to Installing the Chromeleon Chromatography Management System with a Dionex Ion Chromatograph IC Document No 031883 Doc 065290 03 10 12 1 Introduction 1 3 About This Manual The electronic version i e PDF file of this operator s manual contains numerous hypertext links that can take you to other locations within the file These links include e Table of contents entries e Index entries e Cross references underlined in blue to sections figures tables etc If you are not familiar with how to navigate PDF files refer to the Help system for Adobe Acrobat or Adobe Reader for assistance Chapier 1 Introduction Chapter 2 Features Chapter 3 Operation and Maintenance Chapter 4 Troubleshooting Chapter 5 Service Appendix A Specifications Appendix B Touch Screen Operation Appendix C TTL and Relay Control Appendix D Reordering Information Introduces ion analysis and the Dionex ICS 1600 explains the conventions used in this manual including safety related information Provides an overview of Dionex ICS 1600
166. ump Difficult to Prime or Loses Prime 0 73 4 5 Pump Does Not Start 2 2c eee t RR Re eh 75 46 NOHOW ni e eee ae ee de Eee nei ers 75 4 7 Erratic Flow Pressure Reading 0 0 0 c eee ee eee eee 76 Doc 065290 03 10 12 iii Dionex ICS 1600 lon Chromatography System 4 8 Excessive System Backpressure 0 0 e eee eee eee TI 4 9 Peak Ghostng ior ep De eee eb Neb ies et i eise 78 4 10 Nonreproducible Peak Height or Retention Time 79 4 11 Abnormal Retention Time or Selectivity 0000 79 4 12 No Cell Response sirrien anete r de iat teer E Ee 79 4 13 High Cell Output i ios eme verres 80 4 14 Baseline Noise or Drift 0 0 0 0 cee cece eee 81 4 15 Vacuum Degas Assembly Does Not Run 00004 82 BG SSBIVIGO d dott beri Ce RE aN a De gs 85 5 1 Diagnostic and Calibration Procedures 20 000 ee eee 85 5 1 1 Chromeleon Wellness Panel Overview 86 5 1 2 Diagnostic and Calibration Touch Screen Overview 88 5 1 3 Calibrating the Conductivity Cell 89 5 1 4 Calibrating the Flow Rate 0 0 0 cee eee eee 92 5 1 5 Calibrating the Vacuum Degas Assembly 94 5 2 Isolating a Restriction in the Liquid Lines 95 5 3 Replacing Tubing and Fittings 0 0 0 cee eee eee 98 5 4 Rebuilding the Injection Valve or Auxiliary Valve
167. up 41 Status 49 System backpressure 32 System components Descriptions 28 System overview 4 System Wellness 27 T Technical Support 8 61 85 Temperature Cell heater 36 146 Column heater 18 35 145 Minimizing the effect of variations 36 Temperature compensation 36 Temperature operating 130 Thermo Fisher Scientific Contacting 8 Thermo Fisher Scientific Technical Support 8 61 85 Timebase 26 Time out screen 161 Top cover 15 Total conductivity 146 161 Touch screen 11 139 Adjusting the contrast 12 139 Number keypad 13 140 Operation 12 139 Specifications 130 Time out 161 Using with Chromeleon 142 Touch screen pages Busy page 161 Detector page 157 Diagnostic pages 162 Home page 12 139 144 146 147 Information page 160 Input Output page 162 174 Module Setup page 161 Overview 143 Plot page 147 148 Pump page 153 Status page 147 149 Suppressor page 156 Doc 065290 03 10 12 Index 9 Dionex ICS 1600 lon Chromatography System Troubleshooting 61 Alarm conditions 63 Baseline noise or drift 81 Calibrations 85 Diagnostics 85 Error messages 63 Excessive backpressure 77 Flow rate 75 High cell output 80 Liquid leaks 71 No cell response 79 Peak ghosting 78 Peak height 79 Pump 73 75 Retention time 79 Selectivity 79 Vacuum degas assembly 82 TTL and relay connector 165 Connection instructions 166 Pin assignments 165 TTL inputs As
168. ut 15 minutes and then select Calibrate on the Wellness Panel or the touch screen CONDUCTIVITY CELL page After calibration the conductivity reading should be 147 00 2 uS and the cell constant should be between 120 and 180 If this is not the case contact Thermo Fisher Scientific for help If you are using the Wellness Panel click Log to record the new calibration values in the Audit Trail If you are using the touch screen record the new calibration values in the Chromeleon Wellness database To do this open the Wellness Panel see Section 5 1 1 and click Upload under Update Wellness Database 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 ELUENT OUT port to the cell inlet Reconnect the cell outlet to the suppressor REGEN IN port Doc 065290 03 10 12 91 Dionex ICS 1600 lon Chromatography System 5 1 4 Calibrating the Flow Rate When to Calibrate If you run the Dionex ICS 1600 Operational Qualification or Performance Qualification and it fails Items Needed e 0 076 mm 0 003 in ID yellow PEEK tubing P N 049715 to create 14 2 MPa 2000 x 300 psi of backpressure if needed High purity ASTM filtered Type I 18 megohm cm deionized water Balance capable of weighing more than 10 g with 0 001 g readability Tar
169. w rate troubleshooting If a contaminated column is suspected clean the column as instructed in the column manual The column manual is included on the Thermo Scientific Reference Library DVD P N 053891 How do 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 manual for details When should I remake standards Standards are used only for calibration and should always be made fresh they have a lifetime of only one week Doc 065290 03 10 12 181 Dionex ICS 1600 lon Chromatography System E 6 E 7 E 8 E 9 E 10 E 11 E 12 When should I remake eluents Eluents should be remade every two or three weeks How do I start Chromeleon Click Start on the Windows taskbar and then select All Programs Chromeleon Chromeleon How do delete data In the Chromeleon Browser highlight the sequence you want to delete and then select File gt Delete How do back up data In Chromeleon select File Export Backup Back up the data and indicate the backup source How do shut off the system In Chromeleon click the System Shutdown button on the Dionex ICS 1600 Control panel On the i
170. ween 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 If the system is not operating in the RFIC ER mode refer to the instructions in the column manual The manual is included on the Thermo Scientific Reference Library DVD P N 053891 If this is an RFIC ER system refer to the instructions in the manual provided in your RFIC ER Installation Kit Install or replace the end line filter on the end of the deionized water line see Section 3 4 3 Malfunctioning injection valve or auxiliary valve 1 Rebuild the valve see Section 5 4 2 Ifthe valve leak persists contact Thermo Fisher Scientific for assistance 78 Doc 065290 03 10 12 4 Troubleshooting 4 10 Nonreproducible Peak Height or Retention Time Column overloading Dilute the sample see Section 3 9 3 Liquid leaks Locate and eliminate the leaks see Section 4 3 Incomplete or imprecise filling of the sample loop 1 Hill the sample loop until excess sample exits the waste line 2 Inspect the 1 cc syringe P N 016388 and replace if damaged Pump not primed properly Prime the pump see Section 5 17 4 11 Abnormal Retention Time or Selectivity Incorrect or contaminated eluent Remake the eluent using concentrated eluent and ASTM filtered Type I 18 megohm deionized water
171. wer Receptacle Tab Fuses 2 Fuse Holder Fuse Holder Side View Figure 5 33 Main Power Fuse Holder Doc 065290 03 10 12 127 Dionex ICS 1600 lon Chromatography System 3 Replace the two fuses in the holder with new IEC 127 fast blow fuses rated 3 15 amps P N 954745 Thermo Fisher Scientific recommends always replacing both fuses 4 Reinsert the fuse holder into its compartment and push in until the tab clicks in place 5 Reconnect the main power cord and turn on the power 128 Doc 065290 03 10 12 A Specifications A 1 Electrical Main Power 100 to 240 Vac 50 to 60 Hz Auto sensing power supply no manual voltage or frequency adjustment required Fuses Two 3 15 amp fast blow IEC 127 fuses P N 954745 A 2 Physical Dimensions Height 56 1 cm 22 1 in Without Width 22 4 cm 8 8 in reservoir Depth 53 3 cm 21 0 in Weight 24 5 kg 54 Ib Decibel Level 52 dBA Control Modes Full control through front panel and Chromeleon software alternative control through TTL or relay closure two relay outputs two TTL outputs four programmable inputs USB One USB input one built in USB hub with two outputs Communication Protocol Doc 065290 03 10 12 129 Dionex ICS 1600 lon Chromatography System A 3 Environmental Operating 4 to 40 C 40 to 104 F cold room compatible 4 C as long Temperature as system power remains on Operating 5 to 95 relative humidity noncondensin
172. wn 8 Gently press the guide into the cavity in the spacer until it is fully seated Doc 065290 03 10 12 107 Dionex ICS 1600 lon Chromatography System 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 3 mm 0 125 inch into the seal If this is the primary pump head install a 10 32 fitting 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 Step 2 and Step 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 isop
173. y See page 63 page 64 page 64 page 64 page 64 page 65 page 65 page 66 page 66 page 66 page 67 page 66 page 68 page 68 page 68 page 69 page 69 page 70 page 70 page 70 62 Doc 065290 03 10 12 4 Troubleshooting 4 2 Troubleshooting Error Messages o COLUMN HEATER EXCEEDS SAFE TEMPERATURE This error occurs when the column heater temperature is higher than the maximum allowed This error may occur if the Dionex ICS 1600 is operating in an extreme environment greater than 40 C 104 P To troubleshoot Refer to Section A 3 for environmental specifications Doc 065290 03 10 12 63 Dionex ICS 1600 lon Chromatography System o COLUMN HEATER OPEN CIRCUIT This error occurs when the column heater is unplugged from the component panel To troubleshoot 1 Check that the column heater is plugged into the component panel 2 Ifthe error persists the column heater may be faulty Replace the column heater see Section 5 12 COLUMN HEATER SHORT CIRCUIT This error occurs when there is a short circuit on the thermistor input used to measure the column heater temperature This error indicates a faulty column heater To troubleshoot Replace the column heater see Section 5 12 DEGAS CALIBRATION FAILED This error occurs when the degas vacuum does not reach the expected level during calibration To troubleshoot Retry the calibration 2 If calibration still fails the vacuum

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