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ICS-3000 Ion Chromatography System Operator`s Manual

1. 19 2 2 Pump H ads amp ist siens beau sha dis EEPE ous 20 2 2 2 Pressure Transducer 20 2 2 3 Proportioning Valves Gradient pump only 20 2 24 Vacuum Degassing Module 21 2 2 5 Piston Seal Wash System 22 22 6 Static MIKEL 2541 rs ester howe db male 22 Doc 065031 04 1 08 ICS 3000 lon Chromatography System 2 3 2 4 2 5 2 6 DP SP Flow Schematics 23 2 3 1 Isocratic Pump Flow Schematic 23 2 3 2 Gradient Pump Flow Schematic 24 DP SPReat Panel ss scene en bre ela teen ete te 2 25 luent R SERVOMS seen enter A eA eee ee Mass is ae 29 EO Optional 25e de ne Sara end og Sos eee ia eae ale aes Bale 30 EG Description Zh 2 8 2 9 2 10 EG Front Features nonr ionga screen a needa pme An EG 31 EG Interior Components 33 EG Rear Panel seroren eonna ew Hes ne H Se RSS 37 EG Flow Schematic 39 DC Description 2 11 2 12 2 13 2 14 2 15 2 16 DC Front Features 4 2 state nant tel eck ed ek ee cet el ate 41 DC Interior Components 44 DC Rear Panel Seese ae RE Malay ab RAR AMEN AN re 47 Injection Valve 545 anne mit nt E ras eae 50 2 14 1 Injection Valve Operation
2. To AS Waste Figure 3 5 RFIC with Matrix Elimination Using a DP and a 6 Port Valve Doc 065031 04 1 08 3 Configurations To pump 2 inlet via the pump rear chase Pump front view PER To pump 1 inlet A via the pump rear chase Injection Valve Connections Key 7 ony oo af Wash Concentrator Pump y E To column E Pump 2 a ci Sample in Eluent in CSS Miner ea To wastes To waste I I pump not to scale UT 2 2 ale d d S Piston lo E Seal Carrier pump in eT a c D To waste amp Deionized Deionized Pump 1 Water Water carrier ao Os 7 Mixer D Gc y ca From the suppressor Regen Out via the DC rear chase DC front view EG left side view Cell In Cell Out Regen Out Eluent Out 5 Eluent In Regen In Concentrator Backpressure Device From A Large Loop To AS Waste To Waste To waste Ld RFIC Eluent Degasser Regen Regen Out In Regen In CR TC Figure 3 6 RFIC with Matrix Elimination Using a DP and a 10 Port Valve Doc 065031 04 1 08 111 ICS 3000 lon Chromatography System To pump 2 inlet via the pump rear chase To Regen In via the DC A rear chase a Deionized Water Reagent Regen From the suppressor Regen Out via the DC L DC fron
3. 92 Doc 065031 04 1 08 TC Description 2 20 TC Interior Components Figure 2 52 illustrates the interior of the TC The components installed in your TC may vary depending on your application Slots for Column ID Chip l cards A B C and D Guard Column Injection Valves Column Brackets Separator Column QO Temperature Stabilizer Figure 2 52 TC Interior View Example Configuration Injection Valves The TC can hold one or two electrically actuated high pressure injection valves Two valve models are available e A 2 position 6 port Rheodyne TitanHP injection valve e A 2 position 10 port Rheodyne TitanHP injection valve See Section 2 22 for details about the injection valves Doc 065031 04 1 08 93 ICS 3000 lon Chromatography System Column Brackets The column brackets are installed in the TC at the factory The TC can hold up to three columns with an inner diameter of 1 to 9 mm and a maximum length of 30 cm 11 8 in Columns are attached to the brackets with special column clips P N 064786 set of six clips Temperature Stabilizers Optional Installation of a temperature stabilizer standard bore P N 064548 microbore P N 064650 ensures that a the temperature of the stationary phase remains constant over the total column length and b the column and the eluent have the same temperature during the analysis When these conditions are met the analytic
4. Energized Relay The relays are capable of switching 2 A at 24 VDC For a normally open connection connect a COM pin and an N O pin For a normally closed connection connect a COM pin and an N C pin Figure 2 47 Relay Output Configuration 84 Doc 065031 04 1 08 2 DC Description You can control the power relays and TTL outputs from the DC Control panel in Chromeleon or Chromeleon Xpress see Figure 2 48 ICS 3000_1 52 Home Sequence Control Status Autosampler Gradient Pump Eluent Generator Detector Compart Cond Detector 1 EC Detector 1 3D Amp Plot System Log Audit Trail 4 50 56 PM DC_TTL_1 State Ov 4 50 59 PM DC_TTL_1 State 5v 14 51 10 PM DC_ACRelay_1 State Closed 14 51 16 PM DC_Relay_1 State Closed 24 51 20 PM DC_TTL_2 State Ov Control the relays and TTLs from here Output Relays and TTLs DC TILA iv DC TTL 2 Detector Compartment F Connected Serial Number 123456789012 Upper Door is Closed Lower Door is Closed Compartment_TC Set Point 35 00 C 3 Mode On Temperature 35 00 C Status Ready ReactionCoilHeater Set Point 35 00 C y Mode On z Temperature 35 00 C Status Ready Column_TC Set Point 35 00 C 4 Mode On fa Temperature Status Valves InjectValve 2 LoadPositic z AM_HP1 AM_HP2 AM_LP1 AM_LP2
5. 108 Doc 065031 04 1 08 3 Configurations To pump 2 inlet via the pump rear chase To pump 1 inlet via the pump rear chase System 2 4 Mixer To waste pump not to scale d gt To inject valve 2 port P 2 System 1 Deionized Eluent Water Mixer gt From suppressor 1 Regen Out via the DC rear chase ee DC front view EG left side view Cell In Cell Out Separator 2 Separator 1 To waste System 1 System 2 To waste Pump front view A OB D Oc System 1 RFIC Eluent Degasser Regen Regen Figure 3 4 RFIC Dual System with CD and ED Doc 065031 04 1 08 109 ICS 3000 lon Chromatography System To pump 2 inlet via the pump rear chase To pump 1 inlet A via the pump rear chase Va d Deionized Deionized Water Water carrier gt From the suppressor Regen Out via the DC rear chase DC front view Large Loop To inject valve sample port Separator pump not to scale Pump front view Pump 2 Mixer To waste LL Piston la B l Seal la cl Wash 6 Pump 1 40 08 Mixer y p Gc LE To waste EG left side view RFIC Eluent Degasser Regen Regen Out In Backpressure Device
6. 261 9 4 Replacing the Check Valves 262 9 5 Replacing a Piston Seal 265 9 5 1 Removing the Pump Head and Piston 265 9 5 2 Cleaning the Piston 268 9 5 3 Removing the Main Piston Seal 268 9 5 4 Removing the Piston Seal Wash Seal 269 9 5 5 Installing the Piston Seals 269 9 5 6 Reinstalling the Piston and Pump Head 270 9 6 Replacing the Piston 271 9 6 1 Removing the Pump Head and Piston 271 9 6 2 Installing the New Piston 273 9 6 3 Reinstalling the Pump Head 273 9 7 Replacing the Piston Seal Wash Tubing 274 9 8 Replacing the DP SP Priming Valve Knob Seal 276 9 9 Changing the DP SP Main Power Fuses 278 EG Service 9 10 Replacing Tubing and Fittings 281 9 11 Isolating a Restriction in the Liquid Lines 282 9 12 Replacing the EluGen Cartridge 282 9 12 1 EG Flow Schematic 283 9 12 2 Removing the Old EluGen Cartridge 284 Doc 065031 04 1 08 Contents 9 12 3 Disposing of the Old EluGen Cartridge 286 9
7. Cell Heater Temp 35 00 C Cell Heater Status At_setpoint Figure 2 46 Analog Out Range 100HS 4 Full Scale 1 00V Offset Level 0 Polarity Negative 1 00 ml from Pos R1 CD_1_Total CD_1 Conductivity Detector Control Panel Doc 065031 04 1 08 83 ICS 3000 lon Chromatography System 2 18 3 Power Relay and TTL Outputs The power relays and TTL outputs can be used to control functions in external devices such as an autosampler or another Dionex module Depending on which pins are connected the relay connection can be either normally open N O or normally closed N C see Figure 2 47 Choose N O or N C based on what you want the state of the connected device to be when the DC power is turned off A normally open relay is open when the relay is switched off and closed when the relay is turned on A normally closed relay is closed when the relay is off and is open when the relay is on The relays can be programmed to switch any low voltage device Switched current must be no more than 2 A at 24 VDC Refer to Section 2 18 1 and the documentation for the external device for connection instructions RELAY OUTPUT CONFIGURATION NOTES Rear Panel Relay Output Pins on DC Electronics N O O com O0 e N C O Non Energized Relay NO Om com O e o N C O
8. When the chip card is installed correctly the LED next to the slot is green lt Figure 9 44 Inserting a Column ID Chip Card 3 Install a chip card for any other columns to be monitored To select the column properties to be monitored 1 Close the TC door if it is open You cannot select column properties unless the door is closed 2 On the TC Control panel click the Column Details button This opens the Column Details screen 3 For each column specify the properties the column ID system will monitor When you finish click Close Doc 065031 04 1 08 329 ICS 3000 lon Chromatography System 9 27 Rebuilding an Injection Valve Dionex recommends rebuilding the TC injection valve annually The Injection Valve Rebuild Kit P N 057896 6 port valve P N 061759 10 port valve contains all required replacement parts NOTE Substitution of non Dionex parts may impair valve performance and void the product warranty NOTE If you prefer you can replace the injection valve pod instead of rebuilding the valve Replacing the pod is easier and faster than rebuilding the valve 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 2 Press the POWER button on the front of the TC to turn off the power To avoid injury wait for the TC to cool down before opening the door or performing any maintena
9. 178 Poor Retention Time Reproducibility 181 Peak Retention Times Are Too Early 183 Peak Retention Times Are Too Late 183 ING PEAKS sac nn re pease ee a Rate ae Re se eue 183 Wailing Peaks ss bt soles ne ds Re as oR 185 Low System Backpressure 185 High System Backpressure 186 Low D tector Output noi sisi tement a peter 186 High Backgrounds sut inter RAA eh GA RAR 187 DP SP Troubleshooting 8 12 Troubleshooting DP SP Error Messages 189 8 13 DP SP Does NOESIS M em tee daw eke n 197 8 14 DP SP SOPS rie lens Drome baad ti dt SNS 198 8 15 DP SP Liquid Leaks Leak Alarm 199 8 16 Vacuum Degassing Module Low Vacuum 201 8 17 Vacuum Degassing Module Does Not Run 201 8 18 DP SP Digital I O Port Inoperative 201 EG Troubleshooting 8 19 Troubleshooting EG Error Messages 203 8 20 EG ALARM LED Is LIBRE 2588 Kodak LS SANS de 207 8 21 EG POWER LED Fails to Light 208 8 22 Liquid Leaks inthe EG 208 viii Doc 065031 04 1 08 Contents 8 23 NO FIOW 2252 Same RE aiid MEA Baek REG Als AA WOR tale MEE 209 8 24 EG Stops Operation 210 DC Troub
10. 9 12 3 Disposing of the Old EluGen Cartridge If the EluGen cartridge is expended follow these steps to dispose of it 1 Hold the cartridge upright Unscrew the eluent generation chamber from the electrolyte reservoir and pour the remaining electrolyte solution into an appropriate hazardous waste container NOTE Refer to the Material Safety Data Sheet MSDS shipped with the EluGen cartridge for the chemical description Rinse the electrolyte reservoir and membranes with ASTM Type I 18 megohm cm filtered and deionized water three times Rinsing should render the reservoir and membranes nonhazardous however check your local state and federal regulatory agency regulations for proper disposal If the EluGen cartridge is not expended it can be stored for up to two years Follow these steps to prepare the cartridge for storage 1 Plug all fittings Cap the vent port this will prevent the evaporation of water in the electrolyte reservoir Store the cartridge in an upright position with the electrolyte reservoir at top at 4 to 40 C 39 to 104 F until its next use The original shipping container is ideal for storage Before resuming operation condition the cartridge For instructions see Conditioning the New EluGen Cartridge on page 288 9 12 4 Installing the New EluGen Cartridge 1 Remove the new EluGen cartridge from the shipping container NOTE Save the shipping container it may be required for s
11. DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du DC DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des DC ACHTUNG 4 The fuse drawer is located above the main power switch see Figure 9 28 A Fuse small tab locks the fuse drawer in place Drawer Using a small screwdriver press the tab Tab in and then up to release the fuse drawer 5 Pull the fuse drawer out of the rear panel and remove the old fuses 6 Replace the two fuses with new 10 A IEC 60127 2 slow blow fuse P N 954772 Dionex recommends always replacing both fuses Figure 9 28 DC Fuse Drawer 7 Insert the fuse drawer into the rear panel and press until the drawer snaps into place 8 Reconnect the main power cord and turn on the power Doc 065031 04 1 08 307 ICS 3000 lon Chromatography System 9 23 CD Service Procedures 9 23 1 Calibrating the CD Cell When to Calibrate e After every 6 months of use NOTE Do not use this procedure to calibrate a new cell New cells are calibrated at the factory Items Needed Description 1 0 mM KCI solution Prepare by dissolving 0 07456 g of reagent grade KCl in 1 liter of 18 megohm cm DI water Backpressure tubing to provide Use 0 25 mm 0 010 in ID black PEEK at least 7 MPa 1000 psi tubing P N 042690 1 Click the Cond Detector tab in Chrome
12. Pump_2 Eluent Level Display Current Pressure 0 psi Pump_2 Flow Control A B ie D 0 001 2 0 001 2 0 001 2 0 001 2 6 Select the Flow rate required for your application under Flow Control on the Control panel 7 Click the Motor switch to start the pump flow NOTE After starting the pump or changing the flow rate wait at least 5 minutes longer for flow rates below 1 0 mL min before beginning an analysis This allows the DP SP Moduleware to stabilize the flow rate Doc 065031 04 1 08 129 ICS 3000 lon Chromatography System 8 Enter the Minimum Pressure and Maximum Pressure values under Pressure Display on the Control panel Setting high and low pressure limits ensures that the DP SP will automatically stop if a system malfunction occurs Notes e When the system includes an EG the high pressure limit for the DP SP is 21 MPa 3000 psi and the low pressure limit is 1 4 MPa 200 psi e The DP SP is equipped with a pressure alarm limit that prevents operation above 34 MPa 5000 psi 130 Doc 065031 04 1 08 EG Startup 4 7 Setting the Eluent Concentration 1 In Chromeleon or Chromeleon Xpress select the Eluent Generator tab on the ICS 3000 panel tabset This displays the EG Control panel see Figure 4 4 ICS 3000 2 gt k Home Sequence Control Status Autosampler Gradient Pumps Eluent Generator
13. backpressure replace the component Replace as many components as necessary to resume operation at the standard operating backpressure 8 16 Vacuum Degassing Module Low Vacuum e Leak in the vacuum degassing module Check all tubing connections for leakage tighten loose fitting connections 8 17 Vacuum Degassing Module Does Not Run e Electrical connections incorrectly installed There may be a problem with the connections from the vacuum degassing module to the CPU board Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user 8 18 DP SP Digital I O Port Inoperative e TTL input related error 1 The TTL input mode must match the signal type output by the device connected to the pump Check the user s manual for the device to verify that the correct signal type is selected 2 A programming error occurred in the device sending the signal Refer to the user s manual for the device for troubleshooting assistance e TTL Relay output related error 1 A programming error occurred in the device sending the signal Refer to the user s manual for the device for troubleshooting assistance 2 The device being triggered may require a TTL input not a relay Connect the device to a pump TTL output Doc 065031 04 1 08 201 ICS 3000 lon Chromatography System 202 Doc 065031 04 1 08 EG Troubleshooting 8 19 Troubleshooting EG Error Mess
14. 1 Introduction ICS 3000 System Overview ICS 3000 Dual Chromeleon Chromeleon Xpress Monitor ICS 3000 Eluent Organizer ics 3000 ICS 3000 Eluent Detector Chromatography Generator AS Autosampler Module Figure 1 1 ICS 3000 System for Dual Analysis RFIC The Dionex ICS 3000 Ion Chromatography System offers a full range of Reagent Free IC RFIC components RFIC combines automated eluent generation and self regenerating suppression to make IC easier and more powerful than ever Doc 065031 04 1 08 ICS 3000 lon Chromatography System before It is no longer necessary to spend time preparing eluents and regenerants All you need is deionized water the IC system automatically generates eluent in the exact amount and concentration needed for your application ensuring superior analytical results The dual analysis capabilities both simultaneous and sequential of the ICS 3000 system let you maximize efficiency and throughput and minimize downtime The modular system design lets you quickly configure and customize hardware 1 1 1 ICS 3000 System Components The table below identifies modules in the ICS 3000 product line as well as additional products that can be added to an ICS 3000 system Refer to the page number indicated here for a brief product overview Product Type Product Name Pump ICS 3000 Dual Pump see page 3 ICS 3000 Single Pump see page 3
15. ALARM The leak sensor is wet or there wasa Does not flash SUPPRESSOR 1 The suppressor is on and current is Does not flash temperature SUPPRESSOR 2 being applied OVEN UPPER The upper compartment is at its set The upper compartment is temperature transitioning to the set temperature The compartment is not ready for operation OVEN LOWER The lower compartment is at its set The lower compartment is transitioning to the set temperature The compartment is not ready for operation Doc 065031 04 1 08 41 ICS 3000 lon Chromatography System Button LED Label VALVE 1 LOAD VALVE 2 LOAD VALVE 1 INJECT VALVE 2 INJECT If the LED Is On If the LED Is Flashing Use the VALVE 1 and VALVE 2 Valve error See Section 8 25 buttons to manually switch the for troubleshooting position of the DC injection valves The LEDs indicate whether the valve is in the Load or Inject position POWER Use this POWER button for routine Does not flash on off control of the DC When the power is on this LED is lighted To turn off the DC press and hold this POWER button for 2 seconds Note The main power switch is on the DC rear panel NOTE The VALVE 1 and VALVE 2 buttons can be enabled and disabled in Chromeleon or Chromeleon Xpress When disabled the valve can be controlled only from the software To enable or disable a button open the Commands dialog box press F
16. Do not use a sharp tool such as tweezers to install the seal This may IMPORTANT scratch the seal and the surface of the priming valve knob These scratches will prevent a proper seal and cause leakage Priming Valve Knob Seal a P N 063382 Insert seal with groove facing away from knob Figure 9 10 Replacing the Priming Valve Knob Seal Doc 065031 04 1 08 277 ICS 3000 lon Chromatography System 11 12 Insert the priming valve knob into the secondary pump head turn the knob clockwise and tighten fingertight Push the component mounting panel back into the enclosure Close the DP SP door Press the POWER button on the front of the DP SP to turn on the pump Select the Connected check box on the Control panel to reconnect the pump to the software Click Motor on the Control panel to turn on the pump flow 9 9 Changing the DP SP Main Power Fuses 1 DANGER DANGER ACHTUNG Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow Begin monitoring the Current Pressure reading on the Control panel When the system pressure reaches zero do the following e Disconnect the pump from the software by clearing the Connected check box on the Control panel e Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump Turn off the main power switch on the rear panel of the pump see Figure 2 6 Disconnect
17. Doc 065031 04 1 08 127 ICS 3000 lon Chromatography System limited number of device functions can be controlled directly from this panel You can also access the Audit Trail from here See 128 Doc 065031 04 1 08 4 DP SP Startup 5 To display the pump Control panel select the Pump tab The tab name varies depending on the system configuration ICS 3000 Sequence Control Status Autosampler Gradient Pumps Eluent Generator M Connected Audit Trail Trend Pump_1 Gradient Control Pump_1 Pressure Display Pump_1 Flow Control a 1000 B 00 Current Pressure 0 psi 0 100 mlimi 3 i Bro ff Flow sat C 0 0 El D 0 0 El Minimum Pressure 20 psi Pump_1 Prime Control Bfe of Duration 60 s z Pump_2 Gradient Control A 1000 p 00 Leeson eer rer Prime Rate 2 000 mlimin El El 20 100 2000 3000 l clo dofo Al Pump_1 Eluent Level Display Maximum Pressure 3000 psi Output Relays Pump_2 Pressure Display A B E D a 0001 2 0001 0001 00014 Pump Relay Open x Pump_Relay 2 Open ini 200 psi Pump_Relay 2 open Minimum Pressure psi 0 100 mlimin Fe Boo gii Fier 0 100 mimin Pump Relay 4 Open x Maximum Pressure 3000 psi Pump_2 Prime Control _ Gradient Display Gradient Display 73 00 100 Bpi Off Duration fs 4 1 Prime Rate 2 000 ml min EE
18. OO F Connected Audit Trail Set Point 35 00 C Bj InjectValve 2 LoadPosition z booma v Serial Number 123456789012 Mode On AM_HP1 DC_Relay_1 Open AM_HP2 Temperature 35 00 C a DC_Relay_2 Open AM_LP1 Closed x g DC_ACRelay_1 0 X Status Ready _ACRelay_ pen DEN Closed E DC ACRelay 2 open gt Suppressor1 Settings Column TC DC_LP1 Closed nm z o Input TTLs eee ASRS_2mm E Set Point 35 00 C 3 DC_LP2 Closed TTL_Input_1 Ov Mode Off Mode On DC LP3 Closed TTL_Input_2 Ov TTL_Input_3 Ov DC_LP4 Closed 5 Current 0 mA Temperature TTL Input 4 Ov DC LPS Closed TTL_Input_5 Ov Calculate Current Status Calculate Current DC LPS Closed VAE GE e TTL_Input_7 Ov TTL_Input_8 Ov Upper Door is Closed Lower Door is Closed Suppressor2 Settings Type None Set Point Mode Off Mode Current 0 mA a Temperature Status Figure 2 42 DC Control Panel Doc 065031 04 1 08 77 ICS 3000 lon Chromatography System 2 17 4 RCH 1 Reaction Coil Heater The RCH 1 Reaction Coil Heater P N 061746 can hold up to two reaction coils The heater has an operating temperature range of from 5 C above the temperature of the upper compartment up to 80 C Commands for heater control can be included in a program see Figur
19. 3 Replace all end line filters P N 045987 See Section 4 4 for instructions 4 Prepare new stock solution 5 Prepare fresh eluent To ensure eluent purity prepare all eluents with electrochemical grade chemicals and ASTM Type I 18 megohm cm filtered and deionized water Problem unrelated to the pump 1 The eluent concentration may be wrong or the eluent may have been prepared with impure chemicals eluents or water To ensure eluent purity prepare all eluents with spectro grade eluents reagent grade chemicals and ASTM Type I or better filtered and deionized water 2 The column may be the source of the problem Refer to the column manual for troubleshooting assistance Column manuals are provided on the Dionex Reference Library CD ROM P N 053891 3 The injection valve may be the source of the problem Rebuild the injection valve see Section 9 19 182 Doc 065031 04 1 08 8 Troubleshooting 8 4 Peak Retention Times Are Too Early e Eluent concentration setting is too high The correct eluent concentration setting depends on several factors the flow rate EluGen cartridge type etc Refer to Section 4 7 for a list of valid concentration ranges for the cartridges and then edit the program as required e DP SP flow rate is too low Increase the DP SP flow rate e Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Dionex for assis
20. DIONEX ICS 3000 lon Chromatography System Operator s Manual Now sold under the Thermo Scientific brand Thermo SCIENTIFIC Document No 065031 Revision 04 January 2008 2008 by Dionex Corporation All rights reserved worldwide Printed in the United States of America This publication is protected by federal copyright law No part of this publication may be copied or distributed transmitted transcribed stored in a retrieval system or transmitted into any human or computer language in any form or by any means electronic mechanical magnetic manual or otherwise or disclosed to third parties without the express written permission of Dionex Corporation 1228 Titan Way Sunnyvale California 94088 3603 U S A DISCLAIMER OF WARRANTY AND LIMITED WARRANTY THIS PUBLICATION IS PROVIDED AS IS WITHOUT WARRANTY OF ANY KIND DIONEX CORPORATION DOES NOT WARRANT GUARANTEE OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES TRADEMARKS AES Atlas Chromeleon EluGen IonPac OnGuard and SRS are registered trademarks of Dionex Corporation Carbo
21. Detector Chromatography Compartment ICS 3000 Detector Chromatography Module see page 3 Detector inside DC ICS 3000 Conductivity Detector see page 4 ICS 3000 Electrochemical Detector see page 4 Accessory inside DC ICS 3000 Automation Manager see page 4 Detector outside DC ICS Series Photodiode Array Detector see page 7 ICS Series Variable Wavelength Detector see page 7 Thermal Compartment ICS 3000 Thermal Compartment see page 4 Eluent Generator ICS 3000 Eluent Generator see page 5 Eluent Organizer ICS 3000 Eluent Organizer see page 5 Doc 065031 04 1 08 1 Introduction Autosampler AS Autosampler see page 6 AS40 Automated Sampler see page 7 Mass Spectrometer MSQ Plus see page 8 ICS 3000 Dual Pump DP and ICS 3000 Single Pump SP With flow rates ranging from 0 001 to 10 0 mL min and operating pressures up to 35 MPa 5000 psi the DP SP is designed for both standard bore and microbore applications The pump s patented isokinetic pre compression phase allows a precise almost pulse free flow The SP contains one isocratic pump or one gradient pump The DP contains two gradient pumps two isocratic pumps or one isocratic pump and one gradient pump The isocratic pump delivers one eluent while the gradient pump can deliver gradient mixtures of up to four eluent components The selected
22. Doc 065031 04 1 08 47 ICS 3000 lon Chromatography System Switched AC Sockets The two AC receptacles can be used to control the power to external devices Use Chromeleon or Chromeleon Xpress to switch the power on and off TTL inputs can also be used to control the AC sockets see Section 2 18 4 Fuse Holder Main Power Switch and Power Receptacle The fuse holder contains two 10 amp slow blow fuses P N 954772 For instructions on how to change the fuses see Section 9 19 The rear panel power switch is the main power switch for the DC Turn on the main power switch before initial operation and leave the switch on unless instructed to turn it off for example before performing a service procedure NOTE For routine on off control use the POWER button on the front of the DC see Figure 2 12 To turn off the DC press and hold the POWER button for 2 seconds The power cord plugs into the IEC 320 three prong receptacle The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the DC and is easily accessible CAUTION 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 zugan
23. NE FERMEZ PAS LE CONTENEUR DE GAZ RESIDUEL Le ICS 3000 Eluent Generator EG le Atlas Electrolytic Suppressor et le Self Regenerating Suppressor SRS travaillent avec un proces d lectrolyse qui produit des petites quantit s de gaz d oxyg ne ou d hydrog ne Afin de garantir que le gaz ne soit pas enferm dans un conteneur ferm et puisse s y concentrer connectez un tube noir gaz r siduel diam tre int rieur 1 3 cm n de commande 045460 un conteneur ouvert non ferm Connectez le conteneur r siduel au tube r siduel gaz s parateur d sign Waste Gas Separator VERSCHLIESSEN SIE DEN ABFALLBEHALTER NICHT Der ICS 3000 Eluent Generator EG Atlas Electrolytic Suppressor und Self Regenerating Suppressor SRS verwenden einen Elektrolyseprozess wodurch kleine Mengen an Sauerstoff und Wasserstoff entstehen F hren Sie einen schwarzen Gasabscheiderschlauch ID 1 3 cm Bestell Nr 045460 in einen offenen unverschlossenen Abfallbeh lter damit sich das Gas nicht in einem geschlossenen Behalter sammelt und aufkonzentriert Verbinden Sie die mit Waste Gas Separator bezeichnete Leitung mit dem Abfallschlauch If you select a low flow rate that allows the system pressure to drop below 14 MPa 2000 psi and you do not turn off the EG the EG will continue to generate eluent at the concentration set for the last step of the last Chromeleon or Chromeleon Xpress program If this occurs the eluent concentrat
24. Seal i Wash P Deionized 3 Water 5 g ms ws fonio lt lt Valve From the suppressor Regen Out via the DC rear chase To waste DC front view EG left side view RFIC Eluent Degasser EGC emp Stabilizer From A To AS Waste Backpressure Device To Waste my Figure 3 2 Reagent Free IC RFIC Doc 065031 04 1 08 107 ICS 3000 lon Chromatography System To pump 2 inlet via the pump rear chase DC front view To pump 1 inlet via the pump rear chase Deionized Deionized Water Water gt From suppressor 1 Regen Out via the DC rear chase To AS Waste System 1 Backpressure Device System 2 Backpressure Device Pump front view System 2 To waste pump not to scale From suppressor 2 Regen Out via the DC rear chase Piston 2 BIG Seal c 4 System 1 Wash fio g A OB 7 ss ixer y D c J To waste aoe EG left side view System 1 To the CR TC 1 Regen In via the EG rear chas To waste fa RFIC Eluent Degasser Regen Regen Out In System 2 B RFIC Eluent Degasser Regen Regen Out In To waste EG right side view y To inject valve 2 port P 2 seyo 1891 93 eu eN uj UaBey Z O1 HO EY OL Figure 3 3 RFIC Dual System with two CDs
25. i e the rotor seal or stator may need to be replaced Contact Dionex for assistance e Electrical connections incorrectly installed The electrical cables may not be properly installed Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user 8 15 DP SP Liquid Leaks Leak Alarm NOTE After eliminating the source of a leak always dry the leak sensor thoroughly If the leak sensor is not dry it will remain activated and will continue to report a leak to the Audit Trail e Defective piston seal Check the pump heads for leaks If there is any leakage tighten the fitting connections just enough to stop the leak Dry the components If the pump head continues to leak replace the piston seal see Section 9 5 e Leaking check valve If the leaking check valve is securely tightened but allows leaks despite this the valve is defective Replace both check valve cartridges see Section 9 4 Doc 065031 04 1 08 199 ICS 3000 lon Chromatography System If the leaking check valve is loose follow these steps to tighten it 1 Turn off the pump 2 Loosen the check valve enough to allow it to turn freely 3 Tighten the check valve fingertight and then tighten it one quarter turn with a 1 2 inch wrench 4 Ifthe check valve continues to leak tighten it an additional one quarter turn with the 1 2 inch wrench 5 Ifthe check valve continues to leak
26. on page 226 If soaking the reference electrode does not fix the problem replace the electrode see Section 9 24 4 To prevent a reference electrode from drying out make sure that eluent is being pumped continuously through the cell If the cell will not be used for a short time less than 2 days disconnect the tubing from the inlet and outlet fittings and install fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage bottle filled with saturated KC solution See Section 4 1 2 for detailed instructions Contaminated pH reference electrode Replace the reference electrode see Section 9 24 4 8 28 5 Leak in pH Reference Electrode Compartment Defective pH reference electrode O ring Replace the pH reference electrode O ring see Section 9 24 6 Doc 065031 04 1 08 225 ICS 3000 lon Chromatography System 8 28 6 Shift in Ag AgCl Reference Potential Faulty reference electrode A shift in reference potential causes a shift in the effective potential applied to the working electrode For example when using an electrode with a shift of 50 mV an applied potential of 0 1 V is equivalent to an applied potential of 0 15 V for a new reference electrode with no shift Following the steps below measure the Ag AgCl reference electrode potential shift by comparing it to the potential shift of an unexposed electrode A spare reference electrode P N 061879 stored in 3 M KC
27. 228 Can t execute Disconnect command 228 Can t execute Standby command 228 Can t find TC3000 HEX image 229 Can t start acquisition 229 Can t start TC firmware 230 Can t use device x 231 Card data checksum error 231 Command unavailable in demo mode 232 Communication error 232 Communication interface is closed 245 Communication time out 232 Compartment door is open 246 Configuration doesn t match 233 Configuration mismatch 233 Counter x exceeded its limit 246 Current flow out of limits 233 Current pressure out of limits 233 Current temperature out of limits 234 Data buffer overrun 234 Data format on chip card unsupported 246 Device control feature not available 234 Device is not remote 235 Device not found on USB 235 Either the current date is 236 Error deleting flash memory 236 Error during storing of card data 236 Error finishing download 230 Error programming flash memory 237 Executing this command will reset 237 Firmware download in progress 237 Gas leak detected 238 Humidity leak detected 238 Illegal parameter 238 Injections limit has been exceeded 247 Injections limit will be exceeded 247 Invalid date time format 239 Invalid enumerated value 239 Next qualification is due 239 Next qualification is overdue 239 Next qualification was due on 239 Next service is due in 240 Next service is overdue 240 No chip card in reader 241 No
28. 50 2 14 2 Injection Valve Plumbing 52 CD Conductivity Detector 53 2 15 1 Heated Conductivity Cell 53 2215 2 SUpPPressor piren Soa hh ee Secon ey a bain ie base Sas BE Eb 55 2 15 3 System Flow Schematic for Conductivity Detection 56 ED Electrochemical Detector 57 216 1 Amperometry Cell cece 24 crane eaten ea ee ean eee ees 57 Doc 065031 04 1 08 Contents 2 16 2 Combination pH Ag AgCI Reference Electrode 58 2 16 3 DC Amperometric Detection 60 2 16 4 Integrated and Pulsed Amperometric Detection 61 2 16 5 Cyclic Voltammetry Detection 63 216 0 Waveforms rene de aoa aan es ae eee eee 63 2 16 7 Storing and Reprocessing Amperometry Data 68 2 17 Automation Manager 73 2 17 1 High Pressure Switching Valves 74 2 17 2 Low Pressure Valves 75 2 17 3 High and Low Pressure Valve Control 76 2 17 4 RCH 1 Reaction Coil Heater 78 ZTS TOOPI i 1885 es oe oe ia ae tu os ert ale nie de nie 79 2 18 1 I O Option Connections 80 2 18 2 Analog Outputs 81 2 18 3 Power Relay and TTL Outputs 84 2 184
29. Common Normally open Normally open 5V 500 mA Hold Run Stop Start Not used Table 2 1 25 Pin D Sub I O Port Female Continued The analog pressure output indicates the operating pressure of the pump The pressure output is set to 50 mV MPa 5 mV 14 51 psi To monitor the pressure connect the pressure output to a recorder or an A D converter These are the pin assignments for the 2 pin Cinch connector P N 8005 9001A Signal Level Inner ring Outer ring Function Signal pressure Ground Doc 065031 04 1 08 27 ICS 3000 lon Chromatography System The analog pressure output defaults to the pump 1 bottom pump output signal To redirect the output to pump 2 the top pump follow these steps 1 In Chromeleon or Chromeleon Xpress select Command on the Control menu or press the F8 key 2 Inthe Commands dialog box select the pump name 3 Select the AnalogOut command 4 Select PumpTop in the AnalogOut drop down box and click Execute USB Connections e One USB receptacle B type connector allows a connection from the PC on which Chromeleon or Chromeleon Xpress software is installed e Three USB Universal Serial Bus ports A type connectors are provided for connections to other ICS 3000 modules One 1 8 m 6 ft USB cable P N 960777 is provided in the ship kit DP Ship Kit P N 062463 SP Ship Kit P N 063342 Waste Lines e One waste line is connected to the secon
30. Preventive Maintenance Kit P N 061796 is available 166 Doc 065031 04 1 08 TC Routine Maintenance This section describes routine maintenance procedures for the ICS 3000 Thermal Compartment TC that users may perform All other maintenance procedures must be performed by Dionex personnel 7 13 TC Daily Maintenance e Check the TC components for leaks or spills Wipe up spills Isolate and repair leaks see Section 8 31 Rinse off any dried eluent with ASTM filtered Type I 18 megohm cm deionized water e Check the liquid level in the waste container and empty as needed Neutralize acidic and caustic wastes before disposal Dispose of all wastes in accordance with local regulations CAUTION Neutralisez les d chets acides ou caustiques avant de les jeter Jetez les d chets aux r glements locaux MISE EN GARDE Neutralisieren Sie s urehaltige und tzende Abf lle vor ihrer Entsorgung Entsorgen Sie alle Abf lle entsprechend den lokalen Bestimmungen VORSICHT 7 14 TC Weekly Maintenance e Check liquid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines Doc 065031 04 1 08 167 ICS 3000 lon Chromatography System 7 15 TC Periodic Maintenance e Clean the interior of the TC using a lint free cloth Use paper to absorb any liquid inside the module The cleaner the module the more effective the sensors are at detecting excessive gas or humidity e Check for excess c
31. TC 99 2D data Integrated amperometry 65 68 Pulsed amperometry 68 3D amperometry data 68 71 3D plot description 70 71 Chromatogram 69 Definition 68 Displayed in Chromeleon 69 Isoamperometric plot description 70 I t plot 69 3 way low pressure valves See Low pressure valves 6 port valve DC 50 74 TC 98 100 A AC sockets DC 48 Acetonitrile 58 Ag AgCl half cell 58 Air bubbles conductivity cell 312 Air particulate samples 119 Air pressure requirements 118 124 Alarm conditions See Error messages Index Alarm LED DC LED is lighted 41 Alarm LED DP SP LED is lighted 18 Alarm LED EG LED is lighted 35 207 210 Alarm LED TC LED is lighted 91 Amperometry cell Cell design 58 Cell gasket replacement 314 Description 57 Electrodes 57 Maintenance 115 Monitoring the pH readout 59 pH cannot be set to 7 0 224 pH limits 117 Polishing the working electrode 317 Reference electrode replacement 320 Reordering 353 Solvent compatibility 58 Storage 155 Troubleshooting 223 Amperometry detection See Cyclic voltammetry See DC amperometry See Integrated amperometry See Pulsed amperometry Analog output 81 Connection instructions 80 Connectors 49 79 Description 81 Full scale 82 Mark 82 Offset level 82 Polarity 82 Range 81 Recorder calibration 82 Doc 065031 04 1 08 Index 1 ICS 3000 lon Chromatography System Selecting settings 81 Analog pressure outp
32. e In the single zone shared configuration the upper and lower compartments are in the same temperature zone The temperature can be set to between 15 and 40 C Air flow passages between the compartments allow the temperature to stabilize equally in both compartments e In the dual zone configuration the lower compartment is isolated from the upper compartment in a separate temperature zone There is no common air flow between the upper and lower compartments The temperature of the lower compartment can be set to between 10 and 70 C The temperature of the upper compartment can be set to between 15 and 40 C e When a CD is installed the heated conductivity cell can be set to 5 C above the upper compartment temperature up to 60 C e Ifan RCH 1 Reaction Coil Heater is installed in the AM the temperature of the RCH 1 heater can be set to 5 C above the upper compartment temperature up to 80 C The temperatures achieved for a particular zone can vary from the control range depending on the ambient temperature see the table below Temperature Zone Control Achieved Temperatures Based on Ambient Range Upper compartment 15 to 40 C Ifthe RCH 1 is off or shared zone Minimum temperature gt ambient 10 C If the RCH 1 is at 80 C or the CD cell is at 60 C Minimum temperature gt ambient 5 C Lower compartment 10 to 70 C Minimum temperature gt ambient 5 C Maxi
33. knob Once the knob clicks into place it does not tighten any further The PEEK yoke knob ensures constant pressure is applied to the cell Orient the cell assembly with the PEEK yoke knob on the left and push the cell onto its mounting location in the DC compartment Reconnect the cell s inlet and outlet lines Reconnect the electrical cables Start the pump flow Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage Reapply the electrode potential The baseline will drift for more than 1 hour as the cell re equilibrates Peak area values may require up to 12 hours to stabilize Doc 065031 04 1 08 319 ICS 3000 lon Chromatography System 9 24 4 Replacing an Amperometry Cell Reference Electrode When to Replace the Reference Electrode Replace the reference electrode if performance problems occur that are not corrected by regenerating the electrode Performance problems can include no pH readouts a shift in Ag AgCl reference potential or incorrect readouts baseline spikes or a decreased response even with a freshly polished working electrode The reference electrode typically lasts from 3 months to 1 year depending on use NOTE To regenerate a reference electrode soak it in a solution of 1 M KCI and 1 M HCI Items Needed e pH Ag Ag Cl reference electrode P N 061879 Reference Electrode Replacement Procedure 1 Turn off the cell voltage from the Control panel in
34. on the inside of the DC Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure Reconnect the cell inlet and outlet lines Reinstall the suppressor see Section 9 23 2 Turn on the DC power and restart the pump flow Doc 065031 04 1 08 311 ICS 3000 lon Chromatography System 9 23 4 Removing Trapped Air from the Conductivity Cell Air bubbles in the cell can cause pulsations of the baseline random noise and low readings Air may result from outgassing of the eluent 1 Connect enough backpressure tubing to the cell outlet to shrink bubbles and allow them to pass more easily through the cell Refer to Table 9 2 for the appropriate type and number of backpressure tubing coils required Suppressor Column Flow Rate Backpressure Type Format mL min Coils AES 2 mm 0 25 to 0 50 2 red 3 mm 0 50 to 1 00 2 red 4 mm 1 00 to 2 00 1 red SRS or MMS 2 mm or 3 mm lt 0 25 2 red 2 mm or 3 mm 0 25 to 0 50 1 red 4 mm 0 50 to 1 50 2 black 4 mm 1 50 to 3 00 1 black The red coil P N 045878 consists of 0 125 mm 0 005 in ID PEEK tubing with fittings The black coil P N 045877 consists of 0 25 mm 0 010 in ID PEEK tubing with fittings Table 9 2 Backpressure Coil Requirements Table 9 3 lists the correct pressure range for each type of suppressor Suppressor Type Pressure Range AES 0 14 to 0 70 MPa 20 to 100 psi SRS or MM
35. reaches the stop Disconnect the EluGen cartridge electrical cable from the EGC 1 or EGC 2 bulkhead connector see Figure 2 8 Twist the ring on the cable counterclockwise to loosen it and then pull the cable straight out of the connector Remove the VENT line from the EluGen cartridge by unscrewing the 10 32 luer adapter see Figure 9 13 Tip If necessary use EGC a wrench to hold the Vent Line luer adapter in place Rise while unscrewing the Adapter vent line ll Eno The 2005 Figure 9 13 Detaching the EluGen Cartridge Vent Line 284 Doc 065031 04 1 08 9 EG Service 6 Locate the 10 32 plug P N 053981 removed from the EluGen cartridge vent opening during installation Install the plug in the vent opening This will prevent leakage from the vent opening when you turn over the cartridge in Step 8 Lift the EluGen cartridge straight up and off the cartridge holder Turn the EluGen cartridge upside down and place it on the EG drip tray see Figure 9 14 This is the service position for the cartridge Drip Tray Figure 9 14 EluGen Cartridge in the Service Position Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the EluGen cartridge see Figure 9 15 Figure 9 15 EluGen Cartridge Inlet and Outlet Fittings Shown with fittings removed Doc 065031 04 1 08 285 ICS 3000 lon Chromatography System
36. the piston now by pulling it straight out of the pump mechanism NOTE A magnet secures the piston in place If the magnetic force makes the piston difficult to remove tilt the piston to one side and then pull it out of the pump mechanism If the piston is broken be sure to remove all broken pieces If necessary flush the pump head with ASTM Type I 18 megohm cm filtered and deionized water to remove all debris 272 Doc 065031 04 1 08 9 DP SP Service 9 6 2 9 6 3 Installing the New Piston Slide the new piston P N 062082 partway into the pump head approximately 6 mm 1 4 in of the sapphire part of the piston should extend from the head Reinstalling the Pump Head 1 Place the pump head back on the pump 2 Reinstall the screws in the pump head Using the 3 0 mm hex key P N 062338 tighten the screws just until they come into contact with the pump head Then tighten the screws another one quarter to one half turn one eighth of a turn at a time 3 Reconnect all tubing connections to the pump head Tighten connections fingertight and then tighten an additional one quarter turn only 4 Push the component mounting panel back into the enclosure using the handle in the center of the panel Close the DP SP door 5 Press the POWER button on the front of the DP SP to turn on the pump 6 Select the Connected check box on the Control panel to reconnect the pump to the software 7 Click Motor on t
37. 0 to 3 0 per C PEEK Passivated 316 stainless steel lt 1 0 pL 5 C above the DC detector compartment temperature maximum of 60 C 3 MPa 500 psi 0 to 180 LS 0 to 1000 uS and 0 to 15 000 uS Three separate ranges from 0 to 15 000 uS 344 Doc 065031 04 1 08 A DC Specifications Optional Analog Output Signal Voltage User selectable full scale recorder output of 10 100 or 1000 mV A 18 ICS 3000 Electrochemical Detector Electronics Detection Types Noise Cell Drive Potential Settings Optional Analog Output Range Cell Working Electrode Cell Counter Electrode Cell Reference Electrode Wetted Materials Cell Volume at Working Electrode Cell Maximum Operating Pressure Microprocessor controlled digital signal processing Single or dual electrochemical detection Dual detection can be controlled either simultaneously or independently lt 1 pA DC Amperometry 10 pC Integrated Amperometry 2 00 to 2 00 V in 0 001 V increments 50 pC to 200 uC Integrated Amperometry 5 pA to 74 pA DC Amperometry Disposable gold silver or platinum Non disposable platinum gold silver or glassy carbon Titanium pH Ag AgCI combination PEEK titanium Kel F polyetherimide EPR glass high density polyethylene HDPE ULTEM Teflon working electrode materials lt 0 5 uL 0 7 MPa 100 psi Doc 065031 04 1 08 345 ICS 3000 lon Chromatography System
38. 08 209 ICS 3000 lon Chromatography System 8 24 EG Stops Operation DP SP power is off Turning off the DP SP automatically turns off the EG and the suppressor Current to the CR TC is automatically turned on and off when the EG power is turned on and off Check that the power to the DP SP is turned on Prime the pump see Section 9 3 and resume operation DP SP pressure limit tripped When a system includes an EG the high pressure limit for the DP SP is 21 MPa 3000 psi and the low pressure limit is 1 4 MPa 200 psi Check that the system pressure is within this range NOTE The EluGen cartridge requires at least 14 MPa 2000 psi of backpressure for optimal removal of electrolysis gas from the eluent produced by the cartridge A system backpressure of 16 MPa 2300 psi is ideal DP SP flow rate is too low or too high Select a flow rate between 0 1 and 3 0 mL min Electrical error detected ALARM LED is lighted To prevent damage to the EluGen cartridges the DP SP automatically turns off electrical power to the cartridge when excessive current or voltage is detected Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user EluGen cartridge is expended Replace the cartridge see Section 9 12 No communication with Chromeleon or Chromeleon Xpress 1 Check that the POWER button on the front of the EG is turned on 2 Check that the EG main power swi
39. 10 Push the cartridge s blue electrical cable connector onto the EGC 1 or EGC 2 bulkhead connector see Figure 9 17 Twist the ring on the cable connector fingertight to secure it ES a Figure 9 17 Connecting the EluGen Cartridge Electrical Cable 11 Remove the 10 32 plug from the EluGen cartridge vent opening Install a 10 32 luer adapter in the vent opening 12 Connect the luer adapter and VENT line removed from the old cartridge to the vent opening in the new cartridge see Figure 9 13 The vent line must be connected to the EluGen cartridge to ensure IMPORTANT proper ventilation NOTE Place the 10 32 plug removed from the vent opening in a safe place for storage The 10 32 plug is required for shipping or storing the cartridge 9 12 5 Conditioning the New EluGen Cartridge Always condition a new EluGen cartridge before initial use This requires directing a backpressure coil connected to the cartridge outlet to waste and then generating 50 mM of eluent at 1 0 mL min for 30 minutes 1 Start the Chromeleon Server Configuration program and open the EG Properties dialog box Click the Cartridges tab and enter the serial number of the EluGen cartridge 2 Set a small temporary waste container for example a beaker next to the EG Direct the yellow backpressure coil from the EluGen cartridge OUTLET port to the waste container The backpressure must be at least 1 4 MPa 200 psi 288 Doc 0650
40. 161 7 4 DP SP Periodic Maintenance 162 7 5 DP SP Annual Maintenance 162 EG Routine Maintenance 7 6 EG Daily Maintenance 163 7 7 EG Weekly Maintenance 163 7 8 EG Annual Maintenance 163 DC Routine Maintenance 7 9 DC Daily Maintenance 165 7 10 DC Weekly Maintenance 165 7 11 DC Periodic Maintenance 165 7 12 DC Annual Maintenance 166 TC Routine Maintenance 7 13 TC Daily Maintenance 167 7 14 TC Weekly Maintenance 167 7 15 TC Periodic Maintenance 168 7 16 TC Annual Maintenance 168 8 Troubleshooting 8 1 Audit Trail Error Messages 169 8 1 1 DP SP Error Messages 170 8 1 2 EG Error Messages 171 8 1 3 DC Error Messages 172 Doc 065031 04 1 08 vii ICS 3000 lon Chromatography System 8 2 8 3 8 4 8 5 8 6 8 7 8 8 8 9 8 10 8 11 8 1 4 TC Error Messages 173 Noisy Baseline
41. 163 DC page 165 TC page 167 7 1 2 Weekly Maintenance O Check end line filters on eluent lines When end line filters are new they are pure white Replace filters if they become discolored if bacterial buildup is evident or if eluent flow is blocked See Section 4 4 for instructions O Check for plugged or blocked tubing connections Doc 065031 04 1 08 159 ICS 3000 lon Chromatography System For detailed weekly maintenance instructions for each module see DP SP page 161 EG page 163 DC page 165 TC page 167 Periodic Maintenance O Clean eluent reservoirs when making fresh eluent or as needed see Section 9 2 O Optional Have a Dionex Technical Support Representative perform the performance qualification PQ procedure for IC systems For detailed periodic maintenance instructions for each module see DP SP page 162 DC page 165 TC page 168 NOTE There are no periodic maintenance instructions for the EG Annual Maintenance O Dionex recommends performing preventive maintenance on each module annually Preventive Maintenance Kits contain all the required parts for these procedures DP Preventive Maintenance Kit P N 061794 SP Preventive Maintenance Kit P N 061795 DC TC Preventive Maintenance Kit P N 061796 NOTE Dionex does not offer a Preventive Maintenance Kit for the EG 160 Doc 065031 04 1 08 DP SP Routine Maintenance This section describes routine maintenance procedures
42. Chromeleon or Chromeleon Xpress 2 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 3 Disconnect the cell see Section 9 24 1 320 Doc 065031 04 1 08 9 e DC Service 4 Unscrew the reference electrode and remove it from the cell body see Figure 9 36 Unscrew the reference electrode Figure 9 36 Removing the Reference Electrode 5 Unscrew the storage cap from the new reference electrode see Figure 9 37 Save the cap Always store the electrode in the storage cap filled with saturated KCI solution when the cell is not in use This prevents the reference electrode membrane from drying out and damaging the electrode See Section 6 4 for storage instructions Save the storage cap Figure 9 37 Reference Electrode in Storage Cap 6 Rinse the electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water to remove any precipitated salt 7 Calibrate the reference electrode see Section 9 24 5 Doc 065031 04 1 08 321 ICS 3000 lon Chromatography System 9 24 5 Calibrating the Reference Electrode When to Calibrate e Calibrate after installing a new reference electrode Items Needed e A buffer solution with a pH of 7 00 e A second buffer solution with a different pH typically one that matches the pH of the eluent used in your application either pH 10 or pH 4 in m
43. Cooling DC 46 See also Temperature control DC Counter electrode 57 58 CR TC trap column 5 35 39 Contamination 187 Electrical connections 36 Hydration procedure 291 Replacement procedure 290 Cyclic voltammetry 63 Data collection rate 63 Example 63 Sweep rate 64 Triangle waveform 63 Waveforms 63 64 D Daily maintenance DC 165 DP SP 161 EG 163 TC 167 Data Acquiring 146 Displaying 3D amperometry data 69 Reprocessing amperometry data 68 Saving 147 Data collection rate Cyclic voltammetry 63 Electrochemical detector 68 Integrated amperometry 65 Data compression Cyclic voltammetry 63 DC amperometry 60 Entering the potential 60 Degassing eluents 21 Detector See Conductivity Detector CD See Electrochemical Detector ED Detector output Low 186 Detector signal plot 146 Detector Chromatography Module DC 2 3 Alarm LED is lighted 41 Automation Manager AM 73 343 Conductivity Detector CD 53 Dimensions 341 Electrical specifications 341 Electrochemical Detector ED 57 Front description 41 Fuse requirements 341 T O option 79 Injection valve specifications 342 Maintenance 165 Operating humidity 341 Operating temperature 341 Power requirements 341 Rebuilding the injection valve 300 Service procedures 297 Spare parts 353 357 Specifications 341 System configuration 105 Temperature control 46 342 Weight 341 Dimensions DC 341 DP SP 335 EG 339
44. Doc 065031 04 1 08 69 ICS 3000 lon Chromatography System The raw 3D amperometry data plot can be viewed as either an Iso or a 3D wireframe plot For both plot types colors are used to represent the ranges of response values The Iso view is the default view for the 3D raw data This is a top down view of the data imagine you are looking down on the data from above the plot see Figure 2 33 The x axis is the retention time min and the y axis is the waveform period ms The z axis which is not visible on the plot is the response nA T T T T T T T T T T T T 10 50 1075 1100 1125 1150 1175 12 00 12 25 12 50 1275 13 00 13 25 Figure 2 33 3D Amperometry Data in Chromeleon Iso View NOTE The 3D data shown in Figures 2 33 through 2 36 was collected using an analytical waveform see Analytical vs Scanning Waveforms on page 67 To switch to the 3D plot view right click on the Iso plot select Decoration and click the Iso 3D Plot tab The 3D view projects the response values in the third dimension which allows you to see the height 70 Doc 065031 04 1 08 2 DC Description of responses as well as the color mappings see Figure 2 34 For this view imagine you are standing in front and slightly to the left of the plot T oO 72 Qa 1 o b retention time min fF ps hz rT T T T T T T T T T T T T T T T 1 9 96 10 50 10 75 11 00 1125 1150 1175 12 00 12 25
45. It is also possible to control a suppressor with an ICS 3000 Electrochemical Detector ED Tabs for installing the suppressor are provided on the front of the DC next to the ED The cable connection is the same as for the CD For details about any of the suppressors including guidelines for selecting a suppressor for your application refer to the suppressor manuals The manuals are on the Dionex Reference Library CD ROM P N 053891 NOTE A gas separator waste tube P N 045460 should be connected to the suppressor waste line during installation to prevent accumulation of oxygen or hydrogen gasses For details refer to the CS 3000 Ton Chromatography System Installation Instructions Document No 065032 Doc 065031 04 1 08 55 ICS 3000 lon Chromatography System 2 15 3 System Flow Schematic for Conductivity Detection Figure 2 21 illustrates the flow path through a DC for a conductivity detection application using suppression in recycle mode For information about other suppression modes refer to the suppressor manuals The manuals are on the Dionex Reference Library CD ROM P N 053891 NN LS Q COND CELL yo S gt SUPPRESSOR lt SEPARATOR COLUMN GUARD SAMPLE TEMPERATURE L STABILIZER PE 4 c PUMP or we O ELUENT 1 2 ELUENT GENERATOR Pr AU WASTE VALVE Figure 2 21 DC Flow Schematic for Conductivity Detection Suppressio
46. Level A program with this name already exists Abort page 189 Abnormal drive current for x x seconds Warning page 189 Camshaft index too early Abort page 189 Camshaft index too late Abort page 189 Camshaft sensor always alight Abort page 190 Camshaft sensor missing or dark Abort page 190 Degasser malfunction Warning page 190 Excessive drive current Camshaft x x Abort page 190 Invalid flow value Abort page 191 Leak detected Flow stopped Abort page 191 Left hand pump block carryover pressure is too high Abort page 192 Motor malfunction Abort page 192 Motor position error The motor is overloaded Abort page 192 Pressure fallen below lower limit Abort page 193 Relay 4 is configured for inject synchronization Please Abort page 194 change pump configuration Right hand pump block carryover pressure is too high Abort page 192 The maximum purge pressure was exceeded Abort page 194 The pressure in the left hand working cylinder exceeded Abort page 194 the safety limit The pressure in the right hand working cylinder exceeded Abort page 194 the safety limit The rear seal leak count is x x counted drops and has Warning page 195 exceeded the limit of y y leak detection threshold The rear seal leak sensor is malfunctioning Warning page 196 The system pressure exceeded the safety limit Abort page 194 170 Doc 065031 04 1 08 8 Troubleshooting DP SP Related Audit Trail Error Message Default Sever
47. LowerLimit commands To troubleshoot Select a valid temperature setting Data buffer overrun This error occurs if the system cannot write incoming data to disk fast enough To troubleshoot Increase the buffer size 1 Inthe Server Configuration program right click the system name and select Properties on the context menu 2 Onthe Advanced tab page in the Server Configuration dialog box enter a new value in seconds in the Buffer field and click OK If the error occurs again contact Dionex for assistance Device control feature is not available Please check key code and CM Features see About Chromeleon on the client s Help menu This error occurs if you attempt to select or define a feature that is not available for your TC To troubleshoot Select Help gt About Chromeleon to open the About Chromeleon Client screen On the screen all license features you purchased devices controlled number of timebases and other software options are labeled On If necessary upgrade your software by acquiring the corresponding licenses Contact Dionex for assistance 234 Doc 065031 04 1 08 TC Troubleshooting Device is not remote Or TC is not remote If you try to issue certain commands for example Column_x and InjectValve_x commands when the TC is not under Chromeleon control the appropriate message shown above is displayed To troubleshoot Select the Connect command to
48. N 954776 Dionex recommends always replacing both fuses 5 Reinstall the fuse cartridge 6 Reconnect the main power cord and turn on the power 334 Doc 065031 04 1 08 LI sax A t Electrical Main Power Requirements Fuse Requirements A Specifications DP SP Specifications 90 to 120 VAC 47 to 63 Hz 200 to 240 VAC 47 to 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Typical input power 28 W Maximum line draw 1 2 A at 110 VAC Two IEC 60127 2 slow blow fuses P N 954773 rated at 2 A 250 V A 2 Environmental Operating Temperature Operating Humidity A3 Physical Dimensions Weight 4 to 40 C 40 to 104 F 5 to 95 relative humidity noncondensing Height 40 6 cm 16 in Width 22 cm 8 75 in Depth 55 9 cm 22 in Minimum required clearance behind the pump 6 cm 2 5 in DP 25 kg 55 Ibs SP 20 kg 45 Ibs Doc 065031 04 1 08 335 ICS 3000 lon Chromatography System A 4 Hydraulics Feature Pump Flow Rate Range Flow Rate Accuracy and Reproducibility Operating Pressure Pressure Ripple Gradient Proportioning Accuracy and Reproducibility Number of Eluents Gradient Mixer Delay Volume High Pressure Limit Low Pressure Limit Vacuum Degassing Module Isocratic Pump Dual piston in series variable speed 80 uL per revolution 0 001 to 10 0 mL min in increments of 0 001 mL min 0 1 at 1 0
49. Rapid changes in ambient temperature Make sure the column is installed in a thermostatically controlled compartment and the compartment 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 Noisy Baseline CD Only Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 Cell above or below temperature Contact Dionex for assistance Trapped gases in cell Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them Also loosen and retighten the fittings to and from the suppressor eluent ports Detector electronics not functioning correctly Run the detector dummy cell diagnostics from the Wellness panel see Section 9 23 Inappropriate suppressor operating conditions Refer to the suppressor manual for the correct operating conditions Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 Temperature compensation setting not optimized Optimize the selected setting see Section 2 15 Inadequate system backpressure Add backpressure tubing to the cell outlet see Section 9 23 4 Doc 065031 04 1 08 179 ICS 3000 lon Chromatograph
50. Recourse 313 Doc 065031 04 1 08 xi ICS 3000 lon Chromatography System 9 24 1 Disconnecting the Amperometry Cell 313 9 24 2 Replacing an Amperometry Cell Gasket 314 9 243 Polishing an Amperometry Cell Working Electrode 317 9 24 4 Replacing an Amperometry Cell Reference Electrode 320 9 24 5 Calibrating the Reference Electrode 322 9 24 6 Replacing the Reference Electrode O Ring 324 9 24 7 Replacing an ED Detector 326 TC Service 9 25 Replacing Tubing and Fittings 327 9 26 Setting Up the Column ID System 328 9 27 Rebuilding an Injection Valve 330 9 28 Replacing an Injection Valve Pod 331 9 29 Changing the Main Power Fuses 334 Specifications DP SP Specifications A l A 2 A 3 A4 A 5 A 6 El ctrical is Shane Plots ind PINS MS BE yet ed Sh oye aD 335 Enyironmental Dy pha Gene otek on tos oer een urn en RC 335 Physical 5356 25e se Goh Gx conne E E E EEE 335 Hydraulics 2 essentials ree tats EAA IATA A 336 Computer Connections 337 I O Interfaces and Inputs Outputs 337 EG Specifications A 7 Electrical Met antenne Re a a Re oh tied Re ds 339 Xii Doc 065031 04 1 08 Contents A 8 En
51. SEPARATOR inside the EG NOTE A gas separator waste tube P N 045460 should be connected to the EG waste line during installation For details refer to the ICS 3000 Ion Chromatography System Installation Instructions Document No 065032 Place the free end of the waste line into a waste container To maintain an active drain position the waste container below the level of the EG NOTE To ensure proper drainage each waste line must remain above the liquid level in the waste container 36 Doc 065031 04 1 08 2 EG Description 2 9 EG Rear Panel Figure 2 9 illustrates the rear panel of the ICS 3000 Eluent Generator EG Exhaust Fan Gas Vent Lines USB Receptacle B Connector USB Ports 2 A Connectors Fuse Holder Main Power Switch and Power Receptacle Tubing for Connecting to Suppressors Tubing Chase Drain Port from Drip Tray 606 0000 Figure 2 9 EG Rear Panel Exhaust Fan The exhaust fan cools the interior of the EG and exhausts any hydrogen and oxygen gases that escape during operation USB Connections e One USB receptacle B type connector allows a connection from the PC on which Chromeleon or Chromeleon Xpress software is installed e Two USB Universal Serial Bus ports A type connectors are provided for connections to other ICS 3000 modules One 1 8 m 6 ft USB cable P N 960777 is provided in the EG Ship Kit P N 062
52. Stop and Hold Doc 065031 04 1 08 337 ICS 3000 lon Chromatography System 338 Doc 065031 04 1 08 t EG Specifications A 7 Electrical Main Power 90 to 264 VAC 47 to 63 Hz Auto sensing power supply no Requirements manual voltage or frequency adjustment required Typical input power 18 W Maximun line draw 1 A at 110 VAC Fuse Two IEC 60127 2 slow blow fuses P N 954773 rated at 2 A Requirements 250 V A 8 Environmental Operating 4 to 40 C 40 to 104 F Temperature Operating 5 to 95 relative humidity noncondensing Humidity Operating Pressure Minimum 14 MPa 2000 psi Maximum 21 MPa 3000 psi A 9 Physical Dimensions Height 40 6 cm 16 in Width 22 cm 8 75 in Depth 55 9 cm 22 in Minimum required clearance behind the EG 5 cm 2 in Weight 18 kg 40 Ib Doc 065031 04 1 08 339 ICS 3000 lon Chromatography System A 10 EluGen Cartridge Concentration 0 10 to 100 mM Range Note The allowable eluent concentration for any particular application depends on several factors For more information refer to Section 4 7 340 Doc 065031 04 1 08 A 11 Electrical Main Power Requirements Fuse Requirements DC Specifications 90 to 265 VAC 47 to 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Typical input power 190 W Maximum line draw 9 2 A at 110 VAC Two IEC 60127 2 slow blow fuses P N 954772 rated at 10 A 250 V A 12 E
53. System 2 22 Injection Valves The TC is available in the following configurations TC Description Part Number TC with one 2 position 6 port high pressure injection valve 064660 TC with two 2 position 6 port high pressure injection valves 064661 TC with one 2 position 6 port high pressure injection valve and 064651 one 2 position 10 port high pressure injection valve The 6 port valve is installed on the left side of the module TC with no injection valves 064659 2 22 1 Injection Valve Operation The 6 port injection valve has two operating positions Load and Inject Liquid flows through either the Load or Inject path depending on the valve position Figure 2 55 shows flow schematics for the 6 port valve LOAD POSITION INJECT POSITION To Waste To Waste Sample In Sample In To Column To Column From Pump From Pump Eluent Sample Figure 2 55 TC Injection Valve Flow Schematics 6 Port Valve e In the Load position sample is loaded into the sample loop where it is held until injection Eluent flows from the pump through the valve and to the column bypassing the sample loop Sample flows from the syringe or autosampler line if installed through the valve and into the sample loop Excess sample flows out to waste 98 Doc 065031 04 1 08 TC Description e In the Inject position sample is swept to the column for analy
54. The EluGen current is automatically turned off to prevent damage to the cartridge This error may also occur if the liquid flow to the cartridge is interrupted To troubleshoot 1 Connect the EluGen cartridge cable connection to the electrical bulkhead see Figure 2 8 2 Refer to Section 8 23 to determine why there is no flow 206 Doc 065031 04 1 08 8 EG Troubleshooting 3 Ifthe error message appears again contact Dionex for assistance The EluGen cartridge control electronics may have malfunctioned NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user Leak sensor wet This error occurs when liquid accumulates in the drip tray in the bottom of the EG To troubleshoot 1 Locate the source of the leak by visually inspecting the tubing fittings and components in the EG 2 Tighten fittings or replace tubing and fittings as required see Section 9 10 Refer to Section 8 22 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray and leak sensor thoroughly to prevent the leak sensor from triggering additional error messages 8 20 EG ALARM LED Is Lighted Leaking fitting Locate the source of the leak Tighten or replace liquid line connections as needed see Section 9 10 Blocked or improperly installed waste line Check the EG waste lines to be sure they are not crimped or otherwise blocked Make sure th
55. The Ship Kit DP Ship Kit P N 062463 SP Ship Kit P N 063342 includes a coil of PharMed tubing The Preventive Maintenance Kit DP P N 061794 SP P N 061795 includes a coil of Tygon tubing 7 Connect the new tubing pieces to the seal wash reservoir and pump heads see Figure 9 8 8 Push the tubing onto the fitting that was removed in Step 4 9 Connect the PharMed tubing to the peristaltic pump as follows a Push the tubing into the lower notch on the pump mounting plate b Lift the lever to the right and hold it in that position with one hand c With your other hand wind the tubing around the rotor d Release the lever e Pull on the fitting slightly to slide the tubing into the upper notch PharMed Tubing Tygon 2075 Tubing Figure 9 8 Piston Seal Wash Tubing Connections f Make sure there is no slack in the tubing If necessary lift the lever again adjust the tubing around the rotor and through the lower notch to remove any slack and release the lever 10 Push the component mounting panel back into the enclosure Close the DP SP door 11 Click Motor on the Control panel to turn on the pump flow Doc 065031 04 1 08 275 ICS 3000 lon Chromatography System 9 8 Replacing the DP SP Priming Valve Knob Seal Replace the seal in the priming valve knob if there is leakage around the valve threads when the valve is open or if the waste port leaks w
56. Voltammetry jnal i Cycle Time 10 00 s y Elapsed Time _Autozero C Number of Cycles o g Signal LEVMode JI cvLowVoitage 1000V allel 5ll ollection Rate Step DC Voltage 0 000 V Figure 2 27 Cyclic Voltammetry Control Panel Integrated Amperometry Waveforms Integrated amperometry waveforms are included in a Program file in Chromeleon or Chromeleon Xpress Integrated amperometry waveforms have the following characteristics e The duration of one waveform period can be between 0 05 and 2 0 s with a step resolution of 10 ms A waveform can have no more than 100 steps 64 Doc 065031 04 1 08 2 DC Description The maximum waveform period is 2 0 s However for 2D data because only one data point is generated per waveform period the effective maximum length of a waveform period depends on the data collection rate the rate at which Chromeleon collects digital data points from the detector The relationship is as follows Data Collection Rate 1 Waveform Period Multiple waveforms can be defined for a single run provided they all have the same cycle duration Up to 15 waveform changes per run are allowed Each waveform can have only one integration interval The integration interval generates one integrated data point per waveform Chromeleon and Chromeleon Xpress provide several pre programmed waveforms see Figure 2 28 Program W
57. air This section describes two procedures e For instructions on using the PUMP PRIME button to prime the pump refer to Section 9 3 1 e For instructions on priming the pump from the Control panel in Chromeleon or Chromeleon Xpress refer to Section 9 3 2 Although a 10 cc syringe P N 054578 can be used with either priming procedure Dionex recommends using a syringe only if eluent lines are 100 empty or if the pump is dry 9 3 1 Priming with the PUMP PRIME Button 1 Gradient pump only Set the channel to be primed A B C or D to 100 on the pump Control panel in Chromeleon or Chromeleon Xpress 2 Disconnect the DP SP from the software by clearing the Connected check box in the upper left corner of the Control panel NOTE When the pump is connected to Chromeleon or Chromeleon Xpress the PUMP PRIME buttons are disabled 3 Open the priming valve on the secondary pump head see Figure 9 1 by turning it one half turn counterclockwise NOTE If the priming valve is opened too much air is drawn through the valve and air bubbles can be seen exiting the waste line Doc 065031 04 1 08 259 ICS 3000 lon Chromatography System 4 Press PUMP PRIME 1 or PUMP PRIME 2 on the front of the DP SP The pump will begin pumping at approximately 6 0 mL min 5 Continue priming the pump until all air and previous eluents are purged and no air bubbles can be seen exiting the waste line Priming Valve Secondary Pump H
58. always wear gloves when handling electrodes Follow the instructions in Section 9 24 2 Step 1 through Step 6 to remove the working electrode from the cell Prepare the polishing pads a Using indelible ink label the plastic side of a pad to designate it for use with the coarse polishing compound b Label another pad for fine polishing compound also designate the working electrode type with which it will be used Doc 065031 04 1 08 317 ICS 3000 lon Chromatography System NOTE Do not use the same fine polishing pad to polish more than one type of working electrode this can contaminate the electrode surface with microparticles from the other working electrodes c Designate a pad that will not be used with polishing compound This pad is for removal of particles after polishing see Step 5 d Moisten the suede side of the polishing pad slightly with water and place the pad on a smooth flat surface with the suede side facing up 3 Polish the electrode e If you are polishing the electrode before initial installation use only the fine polishing compound e Ifyou are polishing the electrode because of degradation of performance such as increased baseline noise or tailing peaks first use the coarse polishing compound Then repeat with the fine compound a Sprinkle about one half gram of polishing compound in the center of the suede side of the polishing pad Add enough ASTM Type I 18 megohm cm f
59. and the cap is securely tightened For an AS40 use the cap insertion tool P N 037987 to prevent contamination and ensure the cap is inserted to the proper depth For an AS with the sample temperature option After loading the vials position tray covers P N 061010 over any empty tray rows Doc 065031 04 1 08 121 ICS 3000 lon Chromatography System 122 Doc 065031 04 1 08 DP SP Startup Set Up the Eluent Reservoirs Rinse the eluent reservoirs with ASTM Type I 18 megohm cm filtered and deionized water NOTE Always use ASTM Type I 18 megohm cm filtered and deionized water to prepare eluent and regenerant or to rinse eluent reservoirs If necessary prepare the eluent for the application For instructions refer to the manual for the column Column manuals are provided on the Dionex Reference Library CD ROM P N 053891 Fill the reservoirs with prepared eluent or deionized water Locate the end line filters P N 045987 provided in the ship kit DP Ship Kit P N 062463 SP Ship Kit P N 063342 Before installation thoroughly rinse the end line filter with ASTM Type I 18 megohm cm filtered and deionized water to remove any loose particles Install an end line filter on the end of each reservoir s eluent line Install the reservoir caps making sure the end of each line extends to the bottom of the reservoir and that each filter is submerged in liquid This prevents air from being drawn through th
60. carbon working electrodes The ED is installed in the upper compartment of the DC ICS 3000 Automation Manager AM The AM consists of a component mounting panel on a base tray The AM provides mounting sites for sample preparation and post column application components high pressure switching valves low pressure solenoid valves reaction coils etc The AM is installed in the upper compartment of the DC above the detector ICS 3000 Thermal Compartment TC The TC provides a temperature controlled environment for ICS 3000 chromatography components The TC is intended for applications that do not require conductivity or electrochemical detection The TC is available in four configurations e With one 2 position 6 port high pressure injection valve e With two 2 position 6 port high pressure injection valves e With one 2 position 6 port high pressure injection valve and one 2 position 10 port high pressure injection valve e With no injection valves An optional temperature stabilizer standard bore P N 064548 microbore P N 064650 can be installed inside the TC if necessary The temperature stabilizer brings the eluent to the column temperature before it enters the column 4 Doc 065031 04 1 08 1 Introduction ICS 3000 Eluent Generator EG The EG generates high purity acid or base eluents online from deionized water The EG can be configured for single or dual channel operation Each channel includes
61. cartouche d EluGen contient un de ce qui suit une base corrosive KOH LiOH ou NaOH un acide corrosif MSA ou une solution concentr e de K CO Porter des lunettes et des gants protectives en manipulant la cartouche Die EluGen Kassette enthalt eine korrodierende Base KOH LiOH oder NaOH eine korrodierende S ure MSA oder eine konzentrierte K CO L sung Tragen Sie daher beim Umgang mit Kassette eine Schutzbrille und Handschuhe 282 Doc 065031 04 1 08 9 EG Service 9 12 1 EG Flow Schematic Refer to Figure 9 12 when performing EG and CR TC service procedures EGC VENT EGC Eluent Degasser x J Regen Regen To Waste E Inlet Outlet EGC IN EGC OUT From pump Regen Out Port To injection valve port P blue label jT fe CR TC Eluent In Port red label 74 Regen In Port orange label a To gas separator waste tube From suppressor REGEN OUT p Figure 9 12 EG Flow Schematic Example Doc 065031 04 1 08 283 ICS 3000 lon Chromatography System 9 12 2 Removing the Old EluGen Cartridge 1 Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow This turns off the power to the EluGen cartridge and the suppressor also Open the front door of the EG Push down on the slide release latch and pull the tray forward until it
62. connect the TC to an external device For details about the pin assignments refer to Table 2 3 Pin Signal Name Signal Level Core Core Label Color 1 Not occupied Pink Analog High 2 Not occupied Gray Analog Low 3 Digital GND OV Green Digital GND 5 Digital Input 0 to 5 V Yellow Digital Input 6 Relay_N O 100 Vpc 0 25 A 3 W Brown Digital Output 8 Relay_Com 100 Vpc 0 25 A 3 W White Dig Out GND Black Shield Table 2 3 Pin Assignments for the TC Mini DIN Signal Cable USB Receptacle The USB Universal Serial Bus receptacle B type connector provides a connection to the PC on which Chromeleon or Chromeleon Xpress is installed Select one of the following methods to establish the connection e Connect the TC directly to the USB receptacle on the PC e Connect the TC to the PC through another USB device in the system for example the pump The TC Ship Kit P N 064789 includes a 1 m 3 ft USB cable P N 063246 Drain Port The drain port provides a connection for the waste line P N 014157 that removes condensing water and liquid leaks from the interior of the TC The tubing should be directed to an appropriate waste container The waste line must remain below the drain port If the waste line is above the drain port liquid may flow back into the TC and cause damage to the instrument Make sure the waste line is not bent or kinked at any point Doc 065031 04 1 08 97 ICS 3000 lon Chromatography
63. e A high precision programmable current source power supply e A high pressure gas removal device that removes electrolysis gases created during eluent generation The following options must be ordered separately for installation inside the EG e A disposable EluGen cartridge to generate eluent Each cartridge contains 900 mL of the appropriate electrolyte concentrate solution e A Continuously Regenerated Trap Column CR TC to remove any extraneous contaminants from the deionized water source The CR TC is electrolytically regenerated which allows it to operate for extended periods without chemical regeneration ICS 3000 Eluent Organizer EO The EO holds eluent reservoirs in a liner that contains spills and leaks Up to two EOs can be installed on top of the DC Each EO accommodates up to four 1 liter or 2 liter reservoirs or up to two 4 liter reservoirs The EO is typically ordered configured with four 2 liter reservoirs P N 062629 All eluent reservoirs available for use with the DP SP can be pressurized If you plan to pressurize the eluent reservoirs the optional EO Regulator Accessory and Stand P N 063493 is required The Regulator Accessory includes a pressure regulator and gauge assembly with four outputs for connections to four eluent reservoirs as well as the tubing and connection fitting required If more reservoirs are required order a second regulator P N 064387 Doc 065031 04 1 08 ICS 3000 lon Chr
64. exiting the waste line Gradient pump only a If all eluent lines have not been primed select another eluent channel and repeat the priming procedure b After priming all eluent lines click the Prime button to stop priming c Close the priming valve by turning it clockwise Do not overtighten the priming valve Do not use any tools to tighten the priming valve Overtightening may IMPORTANT destroy the cap seal Open or close the priming valve only when the system pressure is down T Enter the Flow rate required for your application on the Control panel Gradient pump only Enter the required proportions of eluents A B C and D on the Control panel under Gradient Control Click Motor on the Control panel to turn on the pump flow Doc 065031 04 1 08 261 ICS 3000 lon Chromatography System NOTE After starting the pump wait at least 5 minutes longer for flow rates below 1 0 mL min before beginning an analysis This allows the DP SP Moduleware to stabilize the flow rate 9 4 Replacing the Check Valves A dirty check valve causes erratic flow rates and pressures in addition it may cause the pump to lose prime and or be difficult to reprime If a check valve leaks or is dirty it should be replaced 1 Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Control panel When the system pressure
65. from the front of the DP SP through the interior of the module and to the rear panel Main Power Switch Fuse Holder and Power Receptacle The rear panel power switch is the main power switch for the DP SP Turn on the main power switch before initial operation and leave it on unless instructed to turn it off for example before performing a service procedure NOTE For routine on off control use the POWER button on the front of the DP SP see Figure 2 1 and Figure 2 2 To Doc 065031 04 1 08 25 ICS 3000 lon Chromatography System turn off the pump press and hold the POWER button for 2 seconds The fuse cartridge contains two 2 amp IEC 60127 2 slow blow fuses P N 954773 For instructions on how to change the fuses see Section 9 9 The power cord plugs into the IEC 320 three prong receptacle The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the DC and is easily accessible CAUTION 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 Digital I O Port The digital I O port provides a connection to an AS40 Automated Sampler or o
66. in ID Black 042690 Connections from the EluGen PEEK cartridge to the pump from the EluGen cartridge to the CR TC from the RFIC Eluent Degasser to the injection valve from the RFIC Eluent Degasser to the eluent reservoir 3 mm 0 125 in OD Teflon Clear 014157 Connections from the RFIC tubing Eluent Degasser REGEN IN to the CR TC from the RFIC Eluent Degasser REGEN OUT to waste 1 58 mm 0 062 in ID Clear 047203 EluGen cartridge gas vent line Polyurethane 10 mm 0 39 in ID Clear 055075 Drip tray waste line Polyethylene e Use 1 8 in fittings P N 052267 and ferrules P N 048949 for connections to the suppressor REGEN OUT port and the eluent reservoir e Use double cone 10 32 ferrule fittings P N 043276 and 10 32 bolts P N 043275 for all other tubing connections For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Dionex Reference Library CD ROM P N 053891 Use a tubing cutter to cut tubing to the required length Make sure the cut is at a right angle to the length of the tubing and there are no nicks or burrs on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 062614 dual P N 063408 single Refer to the instructions provided with the cutter Doc 065031 04 1 08 281 ICS 3000 lon Chromatography System 9 11 Isolating a Restriction in the Liquid Lines A restriction in the liquid plumbing w
67. injection valve and the EluGen cartridge OUTLET port For details refer to Section 9 15 34 Doc 065031 04 1 08 2 EG Description Continuously Regenerated Trap Column CR TC The CR TC is a high pressure electrolytically regenerated trap column The CR TC is designed to remove anionic or cationic contaminants in the eluent or deionized water and to reduce drift during gradient separations Two versions of the CR TC can be used with the EG e CR ATC Continuously Regenerated Anion Trap Column P N 060477 e CR CTC Continuously Regenerated Cation Trap Column P N 060478 For more information refer to the CR TC manual The manual is included on the Dionex Reference Library CD ROM P N 053891 NOTE Do not install a CR TC in the same channel as an EGC K CO EluGen Cartridge or an EPM Electrolytic pH Modifier NOTE The IonPac ATC HC Trap Column P N 059604 or IonPac CTC 1 Trap Column P N 040192 may be used with the EG However both IonPac trap columns require off line chemical regeneration Contact Dionex for more information EPM Electrolytic pH Modifier and EGC CO Mixer The EGC II K CO3 EluGen Cartridge can be used with an EPM Electrolytic pH Modifier P N 063175 and an EGC CO3 Mixer P N 061686 to produce a carbonate bicarbonate mixture for use with anion exchange separations on carbonate based JonPac columns After the cartridge generates potassium carbonate eluent the EPM adjusts the eluent concentrat
68. is minimized by velocity modulation of the drive A patented secondary control system automatic compressibility compensation ensures highly constant eluent delivery The flow rate remains constant in relation to the pressure Pressure Transducer The secondary pump head contains a built in pressure transducer to measure the system pressure The DP SP Moduleware the instrument control firmware installed in the pump precisely controls the pump motor speed to ensure flow rate accuracy and to maintain constant flow and constant pressure Flow output from the secondary pump head passes through a static mixer described in Section 2 2 6 before being directed to the remainder of the chromatography system the injection valve columns and detector Proportioning Valves Gradient pump only In the gradient pump eluent flows from the eluent reservoirs through the vacuum degas chambers and into a four way proportioning valve assembly see Figure 2 3 Programmed percentages of each eluent are proportioned by the four valves 20 Doc 065031 04 1 08 2 DP SP Description 2 2 4 Vacuum Degassing Module The DP SP vacuum degassing module provides continuous online eluent degassing Eluent quality significantly affects DP SP performance and vacuum degassing eluents is one way to ensure high eluent quality Degassing helps prevent bubbles caused by eluent outgassing from forming in the eluent proportioning valves gradient p
69. mL min typical 0 1 to 35 MPa 15 to 5000 psi 1 typical Not applicable One Not applicable 0 to 35 MPa 0 to 5000 psi in increments of 0 1 MPa 14 psi trips instantaneously 0 to 34 MPa 0 to 4900 psi in increments of 0 1 MPa 14 psi Built in single channel degas chamber with degassing membranes with internal volume of 670 uL and dual stage diaphragm vacuum pump Gradient Pump Dual piston in series variable speed 80 uL per revolution 0 001 to 10 0 mL min in increments of 0 001 mL min 0 1 at 1 0 mL min typical 0 1 to 35 MPa 15 to 5000 psi 1 typical 0 5 at 2 0 mL min typical Four GM 3 lt 500 uL 3 to 9 mm ID columns GM 4 lt 290 uL 2 mm ID columns 0 to 35 MPa 0 to 5000 psi in increments of 0 1 MPa 14 psi trips instantaneously 0 to 34 MPa 0 to 4900 psi in increments of 0 1 MPa 14 psi Built in four channel degas chamber with degassing membranes with internal volume of 670 uL per channel and dual stage diaphragm vacuum pump 336 Doc 065031 04 1 08 DP SP Specifications A 5 Computer Connections USB Three USB Universal Serial Bus ports provide connections to other ICS 3000 modules One USB receptacle provides a connection to the PC on which Chromeleon or Chromeleon Xpress software is installed A 6 1 O Interfaces and Inputs Outputs Digital I O Four programmable relays Analog output for system pressure Three digital inputs for Start
70. now Pull the piston P N 062082 out of the pump mechanism NOTE A magnet secures the piston in place If the magnetic force makes the piston difficult to remove tilt the piston to one side and then pull it out of the pump mechanism 266 Doc 065031 04 1 08 9 DP SP Service Outlet Check Valve Assembly H P N 045721 includes check J valve body and cartridge Main Piston Seal P N 064946 Primary Pump Head PNA PIN 062083 Piston Seal Wash 5 QS Inlet Check Valve Assembly P N sa ii P N 045722 includes check valve body and cartridge Piston P N 062082 o Ring m 040695 Retainer for Piston Seal Wash Seal P N 062092 Figure 9 4 DP SP Primary Pump Head Assembly Priming Valve P N 062087 Priming Valve Knob Seal PIN 063382 Pressure Transducer Assembly Seal Wash Body P N 062064 Piston Seal Wash Seal Main Piston Seal PIN 063382 AD PIN 064946 O Ring P N 040695 Retainer for Piston Seal Wash Seal P N 062092 Piston P N 062082 Secondary Pump Head Figure 9 5 DP SP Secondary Pump Head Assembly Doc 065031 04 1 08 267 ICS 3000 lon Chromatography System 9 5 2 9 5 3 Cleaning the Piston 1 Place the piston in a beaker containing ASTM Type I 18 megohm cm filtered and deionized water or methanol and sonicate for several minutes After cleaning rinse the piston thoroughly with ASTM Type I 18 meg
71. of the sample Doc 065031 04 1 08 99 ICS 3000 lon Chromatography System loop with it Excess flows out to waste Eluent flows from the pump through the valve and to the separator column bypassing the concentrator column 2 22 2 Injection Valve Plumbing Figure 2 57 shows the injection valve connections for the 6 port valve The injection valve is plumbed at the factory with all tubing and fittings for connection to the pump sample loading port column and waste A 25 uL PEEK sample loop P N 042857 is installed between ports L 1 and L 4 Dionex offers sample loops in various sizes If needed the pre installed 25 uL loop can be replaced with a loop that has a different sample injection volume TO INJECT SAMPLE IN from door inject port or autosampler 25 uL SAMPLE LOOP Orange VALVE P TO INJ Red microbore VALVE C Black standard bore Figure 2 57 Injection Valve Plumbing 6 Port Valve 100 Doc 065031 04 1 08 TC Description 2 23 Column Identification ID System The electronic column ID system stores column specific information on a column ID chip card P N 5710 1500 that is connected to a column for the column life cycle see Figure 2 58 H lt Column ID Chip Card Figure 2 58 Column ID Identification System The columns to be monitored are selected in the TC Properties dialog box in the Server Configuration pro
72. or Chromeleon Xpress installation This error occurs if the file is missing To troubleshoot Select Qualification gt Chromeleon IQ to run the Chromeleon IQ and diagnose the problem When you eliminate the source of the error rerun the Setup program A Can t start acquisition at negative retention times This error occurs if you attempt to execute the AcqOn command while retention times are negative To troubleshoot Wait until the retention time value is positive Can t start acquisition The server configuration does not fulfill the license conditions Operation of the TC requires the appropriate version of Chromeleon or Chromeleon Xpress plus a Timebase Class 1 license This error occurs if you attempt to start data acquisition when these requirements are not met To troubleshoot Contact Dionex to obtain the appropriate software version and license Doc 065031 04 1 08 229 ICS 3000 lon Chromatography System Can t start TC firmware A firmware download may be necessary Or Error finishing download Or TC Firmware download failed Ifthe TC firmware Moduleware cannot be started after a firmware download or if Chromeleon or Chromeleon Xpress is unable to successfully download firmware to the TC the appropriate message shown above is displayed To troubleshoot 1 Press the POWER button on the front of the TC to turn off the power after 30 seconds press the button again to turn on the po
73. panel tabset select the Detector Compartment tab Under Suppressor Settings verify that Mode is set to Off Doc 065031 04 1 08 291 ICS 3000 lon Chromatography System To avoid damaging the suppressor always turn off the suppressor PORTANT before hydrating the CR TC The pump flow is on during conditioning 9 13 3 however no flow reaches the suppressor 5 Select the Pump tab and select the following parameters a Under Flow Control set Flow to the flow rate recommended for your application b Click the Motor switch to start the pump flow c Gradient pump only Under Gradient Control enter 100 for the reservoir containing the ASTM Type I 18 megohm cm filtered and deionized water 6 Allow the pump to run for at least 10 minutes 7 Click Motor to turn off the pump flow 8 Disconnect the hydration tubing assembly from the ELUENT OUT and REGEN IN ports on the CR TC 9 Disconnect the pump outlet line from the ELUENT IN port on the CR TC Completing the New CR TC Plumbing Reinstall the EluGen Cartridge 1 Reconnect the EluGen cartridge inlet and outlet lines 2 Turn the EluGen cartridge right side up and check for bubbles in the eluent generation chamber If necessary shake and tap the cartridge to remove bubbles 3 Reinstall the EluGen cartridge in the holder Remove the 10 32 plug from the vent opening and reinstall the luer adapter and vent line 4 Push the cartridge s electrical cabl
74. parts may impair valve performance and void the product warranty NOTE If you prefer you can replace the high pressure valve pod instead of rebuilding the valve Replacing the pod is easier and faster than rebuilding the valve 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 2 Press the POWER button on the front of the DC to turn off the DC To avoid injury wait for the DC to cool down before opening the door or performing any maintenance or service procedures CAUTION Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hit ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the DC door 4 Disconnect each liquid line connected to the valve 5 Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 300 Doc 065031 04 1 08 9 e DC Service 6 Reconnect all liquid lines to the injection valve see Figure 9 23 SAMPLE IN from door inject port or autosampler L 10 uL ETS SAMPLE LOOP x _ 5s fi Black i c TO INJ Red microbore W s VALVE C Black standard bore 1 2 INP TO INJ VALVE W TO mec VALVE P Green Figure 9 23 Injecti
75. point where it enters the column This includes the mixer transfer tubing and swept volume in the injector or autosampler 22 Doc 065031 04 1 08 2 DP SP Description 2 3 DP SP Flow Schematics 2 3 1 isocratic Pump Flow Schematic Figure 2 4 illustrates the liquid flow path through an isocratic pump J N TO INJECTION VALVE ELUENT V OUTLET pew CHECK VALVE 4 N ZON PUMP PUMP HEAD HEAD D OINLET oe CHECK VALVE DEGAS J w i J TF N ee ELUENT SUPPLY ON OFF VALVE Figure 2 4 Isocratic Pump Flow Schematic e Fluent flows from the reservoir through the vacuum degas chamber if the vacuum degas module is installed through the eluent supply on off valve and into the inlet check valve on the primary pump head e The inlet check valve opens drawing eluent into the primary pump head At the same time the secondary piston pushes forward pushing eluent into the system After completing the intake the primary piston pushes eluent through the outlet check valve and into the secondary pump head e Flow exits the secondary pump head and is directed to the remainder of the chromatography system the injection valve columns and detector Doc 065031 04 1 08 23 ICS 3000 lon Chromatography System 2 3 2 Gradient Pump Flow Schematic Figure 2 5 illustrates the liquid flow path through a gradient pump ELUENT D STATIC LJ TO INJECTIO
76. provides storage of both 2D and 3D pulsed amperometry and integrated amperometry data For 2D data Chromeleon stores the detector s response at each waveform period s integration interval One integrated data point per waveform period is stored This allows you to produce a chromatogram similar to the example shown in Figure 2 31 The retention time in minutes is on the x axis and the detector response in nanoCoulombs is on the y axis Analytical Column CarboPac PA10 4x 250 mm and Guard Eluent 18 mM NaOH Flow Rate 1 5 mL min Detection Pulsed Amperometry Electrode Gold 40 j Waveform Quadruple Potential Peaks 1 L Fucose 1 2 D Galactosamine 3 D Glucosamine 3 4 D Galactose 5 5 D Glucose Response 4 6 D Mannose nC 6 0 J 0 5 10 Retention Time Minutes Figure 2 31 Example Chromatogram for a Pulsed Amperometry Application For 3D integrated amperometry data Chromeleon stores raw data points at a rate of 1 KHz throughout the entire run Each raw 3D data point is defined by the following attributes the detector current 1 recorded at a particular waveform time 2 and at a specific retention time 3 As a result the two dimensional view of an integrated amperometry chromatogram retention time vs integrated current is extended by a third dimension waveform time Thus data for the entire waveform period not just the integration intervals is collected For details about 68 Doc 065031 04 1 0
77. reaches zero do the following e Disconnect the pump from the software by clearing the Connected check box on the Control panel Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the DP SP door to access the mechanical components 4 Use the handles on the component mounting panel to pull the panel forward until it reaches the stop NOTE On newer pumps three red Phillips screws are installed on the component mounting panel before shipment from the factory If the mounting panel does not move freely make sure these screws have been removed 5 To prevent contamination of pump parts wear cleanroom gloves while disassembling the pump head Never disassemble the pump head with bare hands Even minute IMPORTANT Particles of dust dirt etc on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance 262 Doc 065031 04 1 08 9 DP SP Service 6 The check valves are installed in the primary pump head see Figure 9 2 gt UMP rom w y Outlet Check Valve Inlet Check Valve Figure 9 2 DP SP Check Valve Connections 7 Disconnect the tubing connections from the inlet and outlet check valves 8 Using the 1 2 inch wrench P N 062336 provided in the Ship Kit DP Ship Kit P N 062463 SP Ship Kit P N 063342 loosen both check valve assemblies 9 Remove both check valve assemblies from the
78. reference potential of the combination 58 Doc 065031 04 1 08 2 DC Description pH Ag AgCl electrode also shifts by 0 059 V per pH unit pH dependent potential shifts at the working electrode are canceled Correcting for pH Dependence At an eluent pH of 7 the reference potential of the entire electrode is the same as that of the Ag AgCl half cell As the eluent pH is increased the pH half cell potential decreases approximately 0 059 V per pH unit For example at an eluent pH of 12 the reference potential of the pH half cell would be 0 295 V relative to the Ag AgCl half cell Therefore at pH 12 the potentials applied to the working electrode must be raised approximately 0 3 V when switching from the Ag reference to the pH reference In acidic eluents the reference potential of the pH half cell is positive with respect to the Ag AgCl half cell and all applied potentials must be decreased by 0 059 V per pH unit when switching from the Ag reference to the pH reference Do not allow the reference electrode to dry out Make sure that eluent is being pumped continuously through the cell If the cell will not be used for a short time less than 2 days disconnect the tubing from the inlet and outlet fittings and install fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage cap filled with saturated KCI solution See Section 6 4 for detailed storage ins
79. repeat Step 4 268 Doc 065031 04 1 08 9 DP SP Service 9 5 4 Removing the Piston Seal Wash Seal 1 Remove the O ring P N 040695 from the seal wash body 2 Follow these steps to remove the piston seal wash seal P N 063382 from the seal wash body a Using a large flat blade screwdriver remove the retainer P N 062092 for the seal from the seal wash body b Insert the piston into the seal wash body from the O ring side and gently push the seal out of the retainer Do not use a sharp tool such as tweezers to remove the piston seal IMPORTANT wash seal This may scratch the seal and the inside of the pump housing scratches will prevent a proper seal and cause leakage 9 5 5 Installing the Piston Seals 1 Follow these steps to reassemble the seal wash body a Place the seal wash body on a clean work surface b Slide the seal wash seal P N 063382 with the open side of the seal facing upward onto the seal insertion tool P N 063675 see Figure 9 6 Seal Insertion Tool P N 063675 Piston Seal Wash Seal PIN 063382 Figure 9 6 Piston Seal Wash Seal and Seal Insertion Tool c Insert this end of the tool partway into the seal wash body Make sure the tool is centered and does not rock back and forth Then press firmly on the tool and the seal wash body until they snap together d Remove the seal insertion tool from the seal wash body Doc 065031 04 1 08 269 ICS 300
80. response from x 241 Doc 065031 04 1 08 Index 7 ICS 3000 lon Chromatography System Nominal temperature must be set 247 Nominal temperature value out of range 247 Operating columns above 242 Oven not fully operable 248 Parameter x value exceeded 242 Primary column ID property 248 Primary property x already assigned 243 Properties cannot be changed 243 244 Raw data file x cannot be created 244 Raw data file x cannot be written 244 Starting data acquisition manually 245 TC firmware download failed 230 TC is not remote 235 The command can format 245 There was already an AcqOff 250 There was already an AcqOn 250 This function cannot be adjusted 250 This operation may affect 250 Two AcqOn commands for channel 250 Unknown error code 251 Unknown format of card data 251 Upper limit must be higher 249 USB LAN communication error 235 Value for parameter is not within 242 Value x replaced by 242 Warning threshold must be higher 249 Warning threshold must be lower 249 X position error 251 You do not have the privilege 252 External low pressure valves DC 49 External Seal Wash Kit 22 124 350 F Filter end line Bacterial contamination 161 Installation 123 Maintenance 161 Fittings DC Replacing 297 Requirements 297 Fittings DP SP Replacing 257 Requirements 257
81. section describes routine maintenance procedures for the ICS 3000 Detector Chromatography Module DC that users may perform All other maintenance procedures must be performed by Dionex personnel DC Daily Maintenance Check the DC components for leaks or spills Wipe up spills Isolate and repair leaks see Section 8 26 Rinse off any dried eluent with ASTM filtered Type I 18 megohm cm deionized water Check the waste container and empty as needed NOTE If you are using an electrochemical detector also see the special maintenance considerations that are described in Section 4 1 2 DC Weekly Maintenance Check liquid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines Check for excess condensation inside the DC Condensation may build up when the DC is operated in a highly humid environment and the majority of the applications are run at cold temperatures To remove condensation run the DC at its maximum temperature for at least 48 hours for a dual zone DC or 72 hours for a single zone shared DC DC Periodic Maintenance Calibrate the CD cell every 6 months Inspect the door seal for signs of damage A defective seal impairs the performance of the instrument If the seal is defective contact Dionex Technical Support Doc 065031 04 1 08 165 ICS 3000 lon Chromatography System 7 12 DC Annual Maintenance Dionex recommends performing preventive maintenance annually A DC TC
82. slide release latch and pull the tray forward until it reaches the stop Grasp the degasser by the sides and pull it straight off the ball studs that secure it to the component mounting panel Dispose of the degasser Disconnect the four lines connected to the RFIC Eluent Degasser fittings ELUENT OUT REGEN OUT REGEN IN and ELUENT IN Connect the four lines that were disconnected in Step 5 to the new RFIC Eluent Degasser P N 062137 Align the two mounting holes on the back plate of the new RFIC Eluent Degasser with the ball studs on the component mounting panel Push the degasser firmly onto the mounting ball studs The degasser clicks into place when properly installed Push the tray into the module until it locks into place Close the EG door Turn on the power and resume operation 294 Doc 065031 04 1 08 9 EG Service 9 15 Installing a Backpressure Coil The EluGen cartridge requires at least 14 MPa 2000 psi of system backpressure this ensures optimal removal of electrolysis gas from the eluent produced by the cartridge During system equilibration monitor the pressure and verify that it is between 14 and 21 MPa 2000 and 3000 psi A system backpressure of 16 MPa 2300 psi is optimal If the backpressure is too low install a backpressure coil between the injection valve and the OUTLET port on the EluGen cartridge Connect one end of the backpressure coil to Port P 2 on the injection valve connect t
83. the Wellness panel again and click Calibrate After calibration the conductivity reading should be 147 00 2 LS If this is not the case contact Dionex for help To record the new calibration value in the Audit Trail click the Log button for the cell that was calibrated Flush the KCI solution from the system by pumping ASTM Type I 18 megohm cm filtered and deionized water through the cell When the conductivity drops to less than 1 uS cm stop the pump Reconnect the pump to the injection valve and reconnect the line from the suppressor to the cell inlet 9 23 2 Replacing a Suppressor Refer to the suppressor manual for guidance about when to replace a suppressor Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 1 Refer to the suppressor quick start guide shipped with the suppressor for instructions on preparing the suppressor before initial use Press the POWER button on the front of the DP SP to turn off the pump Press the POWER button on the front of the DC to turn off the DC Doc 065031 04 1 08 309 ICS 3000 lon Chromatography System Open the DC upper door Disconnect the two eluent and the two regenerant lines from the suppressor see Figure 9 30 Unplug the suppressor cable from the detector Figure 9 30 Disconnecting the Suppressor Liquid Lines and Cable 7 Remove the suppressor from the detector by sliding it to the left a few millim
84. the main power cord from both its source and from the rear panel of the pump HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the pump HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du pump HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite der Pumpe 278 Doc 065031 04 1 08 9 DP SP Service 5 The fuse cartridge is located next to the main power switch see Figure 9 11 Use a small screwdriver to remove the fuse cartridge 6 Replace the two fuses with new 2 A IEC 60127 2 slow blow fuses P N 954773 Dionex recommends always replacing both fuses Fuse Cartridge 7 Reinstall the fuse cartridge 8 Reconnect the main power cord to its source and to the DP SP Figure 9 11 DP SP Fuse Cartridge 9 Turn on the main power switch 10 Press the POWER button on the front of the DP SP to turn on the pump 11 Select the Connected check box on the Control panel to reconnect the pump to the software 12 Click Motor on the Control panel to turn on the pump flow Doc 065031 04 1 08 279 ICS 3000 lon Chromatography System 280 Doc 065031 04 1 08 EG Service 9 10 Replacing Tubing and Fittings The EG is plumbed with the tubing and fittings listed below Tubing Size and Type Color P N Used For 0 25 mm 0 010
85. the transducer are tight Replace any damaged fittings see Section 9 17 2 Ifthe leak is from behind the valve stator the rotor seal may be scratched Rebuild the injection valve see Section 9 19 e Leaking 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 and cause it to leak If the problem continues contact Dionex for assistance e Leaking suppressor Refer to the suppressor manual for troubleshooting procedures Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 8 27 VALVE Button Not Working The VALVE 1 and VALVE 2 buttons on the front of the DC must be enabled in Chromeleon or Chromeleon Xpress in order to use them to manually switch the inject valves To enable a button open the Commands dialog box and select the ValvelButton or Valve2Button command in the list of commands for the DC 222 Doc 065031 04 1 08 8 DC Troubleshooting 8 28 Amperometry Cell Troubleshooting 8 28 1 Amperometry Cell pH Readout Always 7 0 The pH reading is displayed on the Chromeleon or Chromeleon Xpress EC Detector Control panel e Disconnected reference electrode Verify that the reference electrode cable is securely connected see Figure 8 7
86. the valve to Load and the rising edge switches the valve to Inject Similarly for the detector start stop the falling edge starts the detector and the rising edge stops it For the detector mark and offset functions the falling edge turns on the function and the rising edge has no effect e Inverted Edge The inverted Action On edge mode works identically to ONE R acure the normal edge mode except INVERTED that the positive and negative EDGE 16 y 1 si edges are reversed in function Action Off t No Effect e Normal Pulse In normal pulse operation the negative falling TTL 5 VY edge of the TTL signal is the eee a active edge and the positive rising edge is ignored Action On Action Off A pulse width of 50 ms or more 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 e Inverted Pulse The inverted pulse mode operates identically Action On om Off to the normal pulse mode TTL 5 V except that the positive and INVERTED PULSE 49 y negative edges are reversed in function Doc 065031 04 1 08 89 ICS 3000 lon Chromatography System 90 Doc 065031 04 1 08 TC Description 2 19 TC Front Features A status bar on the front of the ICS 3000 Thermal Compartment TC includes LEDs light emitting diodes that indicate the status of several TC
87. to control injection valve 1 that function is assigned to both timebases You do not need to associate a TTL input with a particular timebase To select TTL input control functions 1 2 Open the Chromeleon Server Configuration program Double click the DC icon under the timebase 86 Doc 065031 04 1 08 2 DC Description 3 Select the TTL Inputs tab see Figure 2 49 Dionex DC Detector Chromatography M TTLInput_1 TTL_Input_2 M TTL_Input_3 TTL_Input_4 M TTLInput_5 M TTL_Input_6 M TTL_Input_ TTL Input 1 TTL Input 2 TTL Input 3 TTL Input 4 TTL Input 5 TTL Input 6 TTL Input 7 Figure 2 49 DC Server Configuration Properties TTL Inputs 4 Select the name of the input and press the F2 key or double click the name Doc 065031 04 1 08 87 ICS 3000 lon Chromatography System The Device Configuration dialog box for the selected input appears Device Configuration x Device Name fT TL_Input_1 Mode Normal edge E Control Functions lt InjectValve_Left position A B K Inject alve_Right position 4 B _ AM_HP_A position A B C AM_HP_B position A B _ AM_LP_A position open closed U AM_LP_B position open closed DC_LP_A position open closed Deactivate check boxes for unused functions Cancel Figure 2 50 Assign TTL Input Control Functions 5 Inthe Control Functions lis
88. whenever they become discolored if bacterial buildup is evident or if eluent flow is blocked NOTE It is especially important to regularly replace end line filters when using aqueous eluents Aqueous eluents may contaminate the filters with bacteria or algae although the contamination may not be visible it can cause flow restrictions to the pump Doc 065031 04 1 08 161 ICS 3000 lon Chromatography System End line filters are provided in the ship kit DP Ship Kit P N 062463 SP Ship Kit P N 063342 Before installation thoroughly rinse the end line filter with ASTM Type I 18 megohm cm filtered and deionized water to remove any loose particles e Replace the seal wash solution ASTM Type I 18 megohm cm filtered and deionized water is appropriate for most applications e Check the tubing connected to the peristaltic pump If the tubing is blocked or crimped replace it see Section 9 7 7 4 DP SP Periodic Maintenance e Make fresh eluent as needed e Replace piston seals every 6 to 12 months see Section 9 5 7 5 DP SP Annual Maintenance e Dionex recommends performing preventive maintenance annually The following kits are available DP Preventive Maintenance Kit P N 061794 SP Preventive Maintenance Kit P N 061795 162 Doc 065031 04 1 08 7 6 7 7 7 8 EG Routine Maintenance This section describes routine maintenance procedures for the ICS 3000 Eluent Generator EG that users may perfor
89. 0 Blocked or improperly installed waste line Check the EG waste lines to be sure they are not crimped or otherwise blocked Make sure the lines are not elevated at any point after they exit the EG 208 Doc 065031 04 1 08 8 EG Troubleshooting e EluGen cartridge leaks Replace the EluGen cartridge see Section 9 12 e RFIC Eluent Degasser leaks Replace the RFIC Eluent Degasser see Section 9 14 8 23 No Flow e DP SP power is off Turning off the DP SP automatically turns off the EG and the suppressor Current to the CR TC is automatically turned on and off when the EG power is turned on and off Check that the power to the DP SP is turned on Prime the pump see Section 9 3 and resume operation e DP SP pressure limit tripped When a system includes an EG the high pressure limit for the DP SP is 21 MPa 3000 psi and the low pressure limit is 1 4 MPa 200 psi Verify that the Current Pressure reading on the Control panel is within this range NOTE The EluGen cartridge requires at least 14 MPa 2000 psi of backpressure for optimal removal of electrolysis gas from the eluent produced by the cartridge A system backpressure of 16 MPa 2300 psi is ideal e RFIC Eluent Degasser tubing is ruptured If flow from the EG waste line is normal but there is no flow through the columns the tubing assembly inside the RFIC Eluent Degasser has ruptured Replace the degasser see Section 9 14 Doc 065031 04 1
90. 0 lon Chromatography System 9 5 6 4 e The seal wash seal is now partially installed To complete the seal installation place the retainer in the seal wash body and use the large flat blade screwdriver to tighten the retainer f Place the new O ring P N 040695 on the seal wash body NOTE When replacing a piston seal always replace the O ring also This will prevent leaks Remove the 10 32 fitting plugs from the pump head Insert the piston through the seal wash assembly and then through the new piston seal P N 064946 Make sure the piston seal is centered If the piston seal is not centered applying pressure to it in Step 7 will damage the seal and make it unusable Rinse the piston seal with isopropyl alcohol IPA or dip it into a container of IPA The seal is easier to install when it is moist Place the front of the pump head flat side down on a clean work surface Make sure the open side of the piston seal faces away from the retainer for the seal wash seal Place the components on the pump head and gently press the housing until the piston seal snaps into place Do not use a sharp tool such as tweezers to install the piston seal This will scratch the seal and the inside of the pump housing these scratches will prevent a proper seal and cause leakage Reinstalling the Piston and Pump Head 1 Slide the piston partway into the pump head approximately 6 mm 1 4 in of the sapphire part of th
91. 042126 049135 043276 0643275 042772 054578 954773 063246 005 9001A 061794 061795 Item Piston Seal Wash System Piston seal wash reservoir PharMed tubing 0 159 cm 0 0625 in ID Note Order 12 in of tubing for replacement of piston seal wash tubing Tygon 2075 tubing 0 15 cm 0 060 in ID Note Order 12 in of tubing for replacement of piston seal wash tubing External Seal Wash Kit Eluent Storage and Delivery ICS 3000 Eluent Organizer with 4 reservoirs ICS 3000 Eluent Organizer with 8 reservoirs Eluent reservoir plastic 1 liter Eluent reservoir plastic 2 liter Eluent reservoir plastic 4 liter EO Regulator Kit TC VWD PDA Regulator Bracket Kit Regulator Filter end line Filter high pressure inline Miscellaneous GM 3 Gradient Mixer GM 4 Gradient Mixer Ferrule fitting 10 32 double cone Fitting bolt 10 32 for double cone ferrule fitting Plug Syringe 10 cc Fuse IEC 60127 2 slow blow rated at 2A 250V USB cable 1 m 3 ft long Cinch connector 2 pin Maintenance Kits DP Annual Preventive Maintenance Kit SP Annual Preventive Maintenance Kit 350 Doc 065031 04 1 08 H EG Reordering Information Part Number 058904 058900 058906 058902 058908 060477 060478 063175 061686 053762 053763 053764 053765 062137 954773 063246 043276 043275 046985 Item Consumables EGC II KCO EluGen Cartridge EGC II KOH EluGen Cartridge EGC II LiOH EluGen Cartridge EGC II MSA EluG
92. 12 4 Installing the New EluGen Cartridge 286 9 12 5 Conditioning the New EluGen Cartridge 288 9 12 6 Completing the EluGen Cartridge Installation 289 9 13 Replacing the CR TE 4 use galerie an Pag ieee Bae Bete 290 9 13 1 Removing the Old CR TC 290 9 13 2 Installing and Hydrating the New CR TC 291 9 13 3 Completing the New CR TC Plumbing 292 9 14 Replacing the RFIC Eluent Degasser 294 9 15 Installing a Backpressure Coil 295 9 16 Changing the EG Main Power Fuses 296 DC Service 9 17 Replacing Tubing and Fittings 297 9 18 Replacing the Leak Sensor 298 9 19 Rebuilding a High Pressure Injection Valve 300 9 20 Replacing a High Pressure Injection Valve Pod 302 9 21 Installing or Replacing an I O Option Board 305 9 22 Changing the DC Main Power Fuses 307 9 23 CD Service Procedures 53 4 0 yi ewagea pou done Robien 308 9 23 1 Calibrating the CD Cell 308 9 23 2 Replacing a Suppressor 309 9 2313 Replacing CD pareren tayo Pa een ne Oa et aaa ees 311 9 23 4 Removing Trapped Air from the Conductivity Cell 312 9 24 ED Service Procedures Ladies alee PEetien a
93. 12 50 1275 13 00 1325 13 50 13 75 13 99 Figure 2 34 3D Amperometry Data in Chromeleon 3D View Baseline Correction Based on the peak recognition algorithm Chromeleon can calculate a baseline I t plot for each data point of a peak Each I t plot measured at a given retention time can be corrected by subtracting the calculated baseline I t plot from the 3D amperometry data By definition if baseline correction is enabled 3D amperometry data is zero unless a peak is present To enable baseline correction select Baseline correction on the General tab page of the 3D Amperometry Decoration dialog box Doc 065031 04 1 08 71 ICS 3000 lon Chromatography System Figure 2 35 is an example of 3D amperometry data before baseline correction is enabled Figure 2 35 3D Amperometry Data Before Baseline Correction Figure 2 36 shows the same data after baseline correction is enabled so 325 0 400 425 40 Figure 2 36 3D Amperometry Data After Baseline Correction 72 Doc 065031 04 1 08 2 DC Description 2 17 Automation Manager The ICS 3000 Automation Manager AM provides a mounting location for various components used for performing matrix elimination large volume pre concentration post column reagent addition and other functions Each AM consists of a tray on which valves and other components are installed see Figure 2 37 The tray is installed in the upper compar
94. 30 Tubing and fittings replacement 327 Shift in reference potential 226 Shutdown DC 155 DP SP 151 EG 153 TC 157 Signal plot 146 Silver electrodes 57 Single Pump SP 2 3 Analog pressure output 27 Digital I O port 26 Dimensions 335 Electrical specifications 335 Flow rate accuracy 336 Flow rate range 336 Fuse replacement procedure 278 Fuses 26 335 Gradient proportioning accuracy 336 High pressure limit 336 Low pressure limit 336 Maintenance annual 162 Maintenance daily 161 Maintenance periodic 162 Maintenance weekly 161 Moduleware 20 Operating humidity 335 Operating pressure 336 Operating temperature 335 Piston replacement procedure 271 Piston seal replacement procedure 265 267 271 Piston seal wash tubing replacement procedure 274 Power requirements 335 Pressure limit tripped 185 209 210 Pressure limits for EG 130 209 210 Pressure ripple 336 Priming procedures 259 261 Priming valve knob seal replacement procedure 276 Product warranty 257 Selecting pressure limits 130 Shutdown procedure 151 Spare parts 349 Start up procedures 123 Static mixer 22 Status bar buttons and LEDs 17 System configurations 105 USB connections 28 Vacuum degassing module 336 Waste lines 28 Weight 335 Sodium hydroxide eluent 34 Solvent compatibility ED 58 Spare parts DC 353 357 DP SP 349 EG 351 TC 357 Doc 065031 04 1 08 Index 15 ICS 3000 lon Chromatog
95. 31 04 1 08 9 EG Service 3 On the panel tabset select the following settings a Detector Compartment tab page Under Suppressor Settings verify that Mode is set to off b Eluent Generator tab page Verify that the CR TC is off IMPORTANT To avoid damaging the suppressor and CR TC always turn them off before conditioning the EluGen cartridge The pump flow is on during conditioning however no flow reaches the suppressor or CR TC c Pump tab page Gradient pump only Under Gradient Control select the correct eluent channel A B C or D All pumps Under Flow Control set Flow to 1 0 mL min This turns on the pump flow also d Eluent Generator tab page Enter 50 mM in the Target Concentration field This turns on the power to the EluGen cartridge also Run at the selected settings 1 0 mL min at 50 mM for 30 minutes On the Pump tab page click the Motor switch to turn off the pump flow This turns off the power to the EluGen cartridge also 9 12 6 Completing the EluGen Cartridge Installation 1 Disconnect the EluGen cartridge electrical cable from the EGC 1 or EGC 2 bulkhead connector Twist the ring on the cable counterclockwise to loosen it and then pull the cable straight out of the connector Remove the backpressure tubing from the waste container and remove the waste container Replace the 10 32 plug in the EluGen cartridge vent opening Lift the EluGen cartridge out of the holder
96. 346 Doc 065031 04 1 08 A 19 Electrical Main Power Requirements Fuse Requirements 8 TC Specifications 90 to 264 VAC 47 to 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Power limit 150 W maximum Two IEC 60127 2 time lag fuses P N 954776 rated at 2 A 250 VAC A 20 Environmental Operating Temperature Ambient Humidity Ambient A 21 Physical Dimensions Weight 10 to 35 C 50 to 90 F 5 to 80 relative humidity noncondensing Height 17 4 cm 6 9 in Width 44 4 cm 17 5 in Depth 50 3 cm 19 8 in 15 4 kg 34 Ib Doc 065031 04 1 08 347 ICS 3000 lon Chromatography System A 22 Thermal Compartment Temperature Control Range Temperature Accuracy Temperature Stability Temperature Precision Column Capacity Heat up Time Cooldown Time Control T O Interfaces Injection Valve Safety Features 5 to 85 C in 0 1 C increments 41 to 185 F in 0 18 F increments thermo electric control 0 5 C 0 9 F 0 1 C 0 18 F 0 1 C 0 18 F Up to 3 columns maximum length of 30 cm 11 8 in lt 20 min from 20 to 50 C 68 to 122 F lt 20 min from 50 to 20 C 122 to 68 F Provided by Chromeleon or Chromeleon Xpress software the TC and the host computer are connected through USB Universal Serial Bus 2 digital inputs 2 programmable relay outputs Electrically activated Rheodyne Tita
97. 36 Button descriptions DC 41 DP SP 17 18 EG 31 TC 91 C Cables Power cord 296 305 307 334 Signal cable 6 pin mini DIN 97 357 USB 28 37 350 351 355 357 Index 2 Doc 065031 04 1 08 Index Calibration CD cell 308 309 Recorder analog output 82 Reference electrode 322 323 Carbonate bicarbonate eluent 34 35 CD cell disconnected error 213 CD cell over safe temperature 214 Check valve cartridges Replacement procedure 262 Chromatogram Amperometry data 69 Dips instead of peaks 82 Monitoring 146 Pulsed amperometry example 68 Water dip in 120 Chromeleon Server Configuration 80 Assigning TTL input functions 86 Configuring a remote inject device 145 Chromeleon Chromeleon Xpress 9 Alarm conditions 213 227 Application Wizard 148 149 Audit Trail 18 31 169 Audit Trail error messages 169 Autosampler control 140 Commands dialog box 54 126 Connected LED 41 Control panel 146 Controlling external valves 49 Controlling high pressure valves 76 Controlling low pressure valves 76 Controlling power relays and TTL outputs 85 Controlling switched AC sockets 48 Creating a program 147 Creating a sequence 148 Home panel 9 Installation manual 10 Panel tabset 9 Programs 140 144 147 Quantification method 147 149 Remote inject commands 145 Sample batch processing 147 Sequence Wizard 148 Troubleshooting communication problems 210 USB connectio
98. 4 Pretreating 119 Saving data 147 See also High pressure valves Injection valves Self Regenerating Suppressor SRS 39 45 Gas separator waste tube 36 55 Hydrating 153 154 Start up procedure 153 154 See also Suppressor Sensor gas 91 102 238 Sensor humidity 91 102 238 348 Sequence Wizard 148 149 Service procedures DC Amperometry cell gasket replacement 314 CD cell air removal 312 CD cell calibration 308 Conductivity detector replacement 311 Electrochemical detector replacement 326 Fuse replacement 307 Index 14 Doc 065031 04 1 08 Index Injection valve Pod replacement 302 Injection valve rebuilding 300 330 Leak sensor replacement 298 Reference electrode O ring replacement 324 Reference electrode replacement 320 Suppressor replacement 309 Tubing and fittings replacement 297 Working electrode polishing 317 Service procedures DP SP Check valve cartridge replacement 262 Eluent reservoir cleaning 258 Fuse replacement 278 Piston replacement 271 Piston seal replacement 265 267 271 Piston seal wash tubing replacement 274 Priming 260 261 Priming valve knob seal replacement 276 Service procedures EG CR TC replacement 290 EluGen cartridge replacement 282 Fuse replacement 296 Tubing and fittings replacement 281 Service procedures TC Column ID system setup 328 329 Fuse replacement 334 Injection valve Pod replacement 331 Injection valve rebuilding 3
99. 453 Doc 065031 04 1 08 37 ICS 3000 lon Chromatography System Fuse Holder Main Power Switch and Power Receptacle The fuse cartridge contains two 2 amp slow blow fuses P N 954773 For instructions on how to change the fuses see Section 9 16 The rear panel power switch is the main power switch for the EG Turn on the main power switch before initial operation and leave it on unless instructed to turn it off for example before performing a service procedure NOTE For routine on off control use the POWER button on the front of the EG see Figure 2 7 To turn off the EG press and hold the POWER button for 2 seconds The power cord plugs into the IEC 320 three prong receptacle The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the EG and is easily accessible CAUTION Le cordon d alimentation principal est utilis comme dispositif principal de d branchement Veillez a 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 Tubing Chase The tubing chase routes tubing from the front of the EG through the interior of the module and to the rear panel Vent Suppressor and Drain Lines e The gas vent line clear tubing discharges the el
100. 55 5V output 79 Analog outputs 79 Connections 80 Power output 84 Relay outputs 79 TTL inputs and outputs 79 IA See Integrated amperometry ICS 3000 Automation Manager AM See Automation Manager AM ICS 3000 Conductivity Detector CD See Conductivity Detector CD ICS 3000 Detector Chromatography Module See Detector Chromatography Module DC ICS 3000 Dual Pump DP See Dual Pump DP ICS 3000 Electrochemical Detector ED See Electrochemical Detector ED ICS 3000 Eluent Generator EG See Eluent Generator EG ICS 3000 Eluent Organizer EO See Eluent Organizer EO ICS 3000 IC System Overview 1 2 9 Software control 9 User manuals 10 11 ICS 3000 Single Pump SP See Single Pump SP ICS 3000 Thermal Compartment TC See Thermal Compartment TC Injecting samples Example commands 144 With a remote inject device 145 Injection ports 43 Loading with a syringe 142 Injection valves DC 50 Flow schematics 10 port valve 51 Flow schematics 6 port valve 50 Leaking 222 Operation 50 51 Plumbing 6 port valve 52 Rebuilding 300 Reordering 353 Replacing mechanical parts Pod 302 Specifications 342 Types available 45 Injection valves TC 98 Flow schematics 10 port valve 99 Flow schematics 6 port valve 98 Leaking 254 Operation 98 99 Plumbing 6 port valve 100 Rebuilding 300 330 Doc 065031 04 1 08 Index 9 ICS 3000 lon Chromatography System Replacing mec
101. 6 Update Wellness Database Press for instructions Instructions Settings to Download Current Download In Progress Service Wellness Close Figure 9 38 Wellness Panel ICS 3000 Conductivity Detector 5 Place the electrode in the pH 7 00 buffer Allow the pH to stabilize about 1 minute until the reading fluctuates no more than 0 05 and then click the Offset Cal button 6 Remove the electrode from the first buffer rinse and then dry it Place the electrode in the second buffer solution Allow the pH to stabilize until the reading fluctuates no more than 0 05 7 On the Wellness panel enter the pH of the second buffer in the pH Slope Buffer Value field and then click the Slope Cal button 8 To avoid any hydraulic pressure buildup when inserting the reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings 9 Verify that the reference electrode O ring is present see Figure 9 39 and then screw the reference electrode into the reference electrode cavity Doc 065031 04 1 08 323 ICS 3000 lon Chromatography System Reference Electrode O Ring 10 11 12 13 14 Figure 9 39 Reference Electrode O Ring Orient the cell assembly with the PEEK yoke knob see Figure 9 34 on the left and push the cell onto its mounting location in the DC compartment Reconnect the cell s inlet and outlet
102. 65031 04 1 08 227 ICS 3000 lon Chromatography System _Allsamples scheduled for run on timebases x need to specify the same value for property nominal Temperature Or A All samples scheduled for run on timebases x need to specify the same value for property TempCtrl Or A All samples scheduled for run on timebases x need to specify the same value for property y When a TC is shared by two timebases the same values must be selected for certain parameters If the Chromeleon Ready Check detects a discrepancy this error occurs and batch processing cannot be started To troubleshoot Find and eliminate any discrepancies in the parameter settings For example all samples must turn on TempCtrl or all samples must turn off TempCtrl O Can t execute Disconnect command during data acquisition Or Can t execute Standby command during data acquisition Selecting the Disconnect or Standby command during data acquisition will stop data transmission and cause data acquisition to stall If you attempt to issue one of these commands during data acquisition this error occurs To troubleshoot Wait until data acquisition is completed before attempting to issue either of these commands 228 Doc 065031 04 1 08 TC Troubleshooting Can t find download image TC3000 HEX TC3000 HEX is the version of the TC firmware Moduleware file that should be available in the Bin directory of your Chromeleon
103. 8 2 DC Description how to acquire 3D amperometry data refer to the 3D Amperometry User 5 Manual Document No 065218 Chromeleon displays and lets you reprocess the 3D data in the 3D Amperometry View window see Figure 2 32 To open the window double click the sample in the Browser to open the chromatogram On the View menu click 3D Amperometry Chromeleon JANDIKDESK2_local 3DAmperometry Jan20_PittconWork 28 mix No6CWE_AcetWash 1 30mix JANDIKDESK2_local 3DAmperometry an20_PittconWork a E X TB fie Edt View Workspace Qualification Window Help Den aS st meld Fi ola neje a gt JERK ES OMe waa Rech E0 Sample Injection Data Ditrae 1 00 amount 1 00 no fS Chromatogram Plot Leoo Mr ee l t Plot current vs waveform time 4004 Waveform Plot HE PO sort 73583 52 7 727 min 210 00 ms 74 nA 0 330 v 3D Amperometry Data Plot 160 Paandk __ Figure 2 32 3D Amperometry View Window in Chromeleon The window is divided into several display areas Sample injection data Chromatogram plot 3D amperometry data plot Waveform I t plot Displays information about the sample Displays a chromatogram of data selected in the 3D amperometry data plot Displays the raw 3D amperometry data Displays an I t plot current vs waveform time of selected data and optionally a waveform plot
104. 8 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 9 47 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Splines Figure 9 47 Injection Valve Pod and Pod Holder 9 Push the pod into the holder until it clicks into place Replace the black locking ring 10 Reconnect all liquid lines to the valve 11 Turn on the pump flow Check for leaks from the valve Tighten fittings as required see Section 9 25 12 Close the TC door Doc 065031 04 1 08 333 ICS 3000 lon Chromatography System 9 29 Changing the Main Power Fuses 1 Press the POWER button on the front of the TC for 2 seconds to turn off the power 2 Disconnect the main power cord from both its source and from the TC rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the TC DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du TC DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des TC ACHTUNG 3 The fuse cartridge is located next to the main power switch see Figure 9 48 Use a small screwdriver to remove the fuse cartridge Fuse Cartridge Figure 9 48 TC Fuse Cartridge 4 Replace the two fuses with new 2 A IEC 60127 2 time lag fuses P
105. 8 Chromatogram example 68 Data storage 68 Integration interval 61 Waveform example 61 See also Integrated amperometry Pump See Dual Pump DP Single Pump SP Q Quantification method 147 149 R Raw data 68 RCH 1 Reaction Coil Heater 78 Controlling 78 Installed in AM 73 Open circuit error 219 Over safe temperature 219 Reordering 354 Specifications 343 Temperature control range 46 343 Reagent Free IC RFIC 1 System configurations 105 112 Rear panel DC AC sockets 48 Analog outputs 49 Description 47 Fuses 48 T O option 49 355 Power switch 48 TTL and relay connectors 49 USB connections 48 Rear panel DP SP Analog pressure output 27 Digital I O port 26 Fuses 26 Power receptacle 26 Power switch 25 USB connections 28 Waste lines 28 Rear panel EG 37 Exhaust fan 37 Fuse cartridge 38 Gas vent line 38 Power switch 38 USB connections 37 Waste lines 36 38 Rear panel TC Description 95 Digital I O connectors 96 Fuses 95 Power switch 95 USB connections 97 Waste line 97 Rear seal wash See Piston seal wash system Recorder Analog output setting 82 Calibrating 82 Redox reactions 58 Reference electrode 57 58 Contaminated 224 Faulty 226 Leaking 225 O ring replacement procedure 324 Preventing from drying out 59 Doc 065031 04 1 08 Index 13 ICS 3000 lon Chromatography System Reordering informa
106. 8 and select the ValvelButton or Valve2Button command in the list of commands for the DC 42 Doc 065031 04 1 08 2 DC Description Sample Loading Ports The front of the DC has two sample loading ports see Figure 2 12 that can be connected to injection valves installed inside the DC A syringe is used to manually load sample through the ports For automated sample injection the DC can be connected to an autosampler For more information about sample injection see Section 5 1 Sample Loading Ports Figure 2 12 DC Sample Loading Ports Doc 065031 04 1 08 43 ICS 3000 lon Chromatography System 2 12 DC Interior Components Figure 2 13 illustrates the interior compartments of the DC Upper Compartment 1 Automation Manager Components amp 5 3 O Electrochemical Gi je f Detector and Cell uioxex Y ps wa f Conductivity a Detector and ii Suppressor Lower Compartment Columns and Injection Valves Figure 2 13 DC Interior View Example Upper Compartment The upper compartment consists of two sections The top section houses an optional ICS 3000 Automation Manager AM The AM contains various components required for performing matrix elimination large volume pre concentration post column reagent addition and other functions See Section 2 17 for details about the AM The section below the AM section houses one or two detectors The detector
107. A2 2001 e TC EN 61326 1997 including A1 1998 A2 2001 and A3 2003 Safety e DC EG DP SP EN 61010 1 2001 UL 61010 1 2004 CAN CSA C22 2 61010 1 2004 e TC EN 61010 1 2001 UL 61010A 2002 CAN CSA C22 2 61010 1 2004 NOTE The TC does not carry the TUV GS Mark safety label 14 Doc 065031 04 1 08 1 Introduction These symbols appear on the ICS 3000 modules or on labels affixed to the modules rw Alternating current D Protective conductor terminal Power supply is on Power supply is off Indicates a potential hazard Refer to this operator s manual for an explanation of the hazard and how to proceed m Doc 065031 04 1 08 15 ICS 3000 lon Chromatography System 16 Doc 065031 04 1 08 mover sam 2 1 2 Description DP SP Description DP SP Front Features A status bar on the front of the ICS 3000 Dual Pump DP and ICS 3000 Single Pump SP includes buttons for controlling certain pump functions as well as LEDs light emitting diodes that indicate the status of several pump functions see Figure 2 1 and Figure 2 2 FLOW PRIME FLOW PRIME e o e o 0 e CONNECTED ALARM YV PUMP 1 A PUMP 2 Figure 2 1 DP Status Bar FLOW PRIME ee CONNECTED ALARM Y PUMP 1 Figure 2 2 SP Status Bar Doc 065031 04 1 08 17 ICS 3000 lon Chromatography System Button LED Label If the L
108. Check the cable connection Figure 8 7 Amperometry Cell Electrical Connections e Reference electrode short circuit Replace the reference electrode see Section 9 24 4 e Reference electrode glass membrane broken or cracked Replace the reference electrode see Section 9 24 4 Doc 065031 04 1 08 223 ICS 3000 lon Chromatography System 8 28 2 Cannot Set Amperometry Cell pH Readout to 7 0 The pH reading is displayed on the Chromeleon or Chromeleon Xpress EC Detector Control panel 8 28 3 Inaccurate calibration buffer Use a pH meter to check the pH of the buffer Dry reference electrode Soak the reference electrode in a solution containing 1 M KCI and 1 M HCI long enough to restore the electrode potential to lt 30 mV when compared to an unexposed Ag AgCl reference electrode To test the reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 226 Replace the reference electrode see Section 9 24 4 To prevent a reference electrode from drying out make sure that eluent is being pumped continuously through the cell If the cell will not be used for a short time less than 2 days disconnect the tubing from the inlet and outlet fittings and install fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage bottle filled with saturated KC solution See Section 4 1 2 for detailed instructions Shift
109. D cell 2 option disconnected CD cell 1 over safe temperature Abort page 214 CD cell 2 over safe temperature Column open circuit Abort page 214 Column over safe temperature Abort page 214 Compartment open circuit Abort page 215 Compartment over safe temperature Abort page 215 ED cell 1 option disconnected Abort page 215 ED cell 2 option disconnected ED cell 1 working electrode disconnected Abort page 216 ED cell 2 working electrode disconnected High pressure valve 1 error Abort page 217 High pressure valve 2 error High pressure valve 3 error High pressure valve 4 error Lower door opened Warning page 218 Lower leak sensor wet Warning page 218 Reaction coil open circuit Abort page 219 Reaction coil over safe temperature Abort page 219 Suppressor 1 over current Abort page 219 Suppressor 2 over current Suppressor 1 over power Abort page 220 Suppressor 2 over power Suppressor 1 over voltage Abort page 220 Suppressor 2 over voltage 172 Doc 065031 04 1 08 8 Troubleshooting DC Related Audit Trail Error Message Default Severity See Level Suppressor 1 open circuit Abort page 221 Suppressor 2 open circuit Upper door opened Warning page 221 8 1 4 TC Error Messages The table below lists the TC related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in th
110. DC_LP1 DC_LP2 DC_LP3 DC_LP4 DC_LP5 nd DC_LP6 InjectValve_1 LoadPositic gt Figure 2 48 DC Control Panel ov DC_Relay_1 Closed gt DC_Relay 2 open x DC_ACRelay 1 Closed x DC_ACRelay 2 z E elay 2 Open Input TTLs TTL_Input_1 TTL_Input_2 TTL_Input_3 TTL_Input_4 TTL_Input_5 TTL_Input_6 TTL_Input_ TTL_Input_8 NOTE It is possible to change the settings for the power relays and TTL outputs while a Chromeleon or Chromeleon Xpress program is running Doc 065031 04 1 08 85 ICS 3000 lon Chromatography System 2 18 4 TTL Inputs When connected to a controlling device the TTL inputs can be programmed to perform the following DC functions Injection valves left and right load inject AM high pressure valves A and B A B AM low pressure valves A and B open closed DC low pressure valves A through F on the rear panel open closed ED detectors 1 and 2 on off CD ED detectors 1 and 2 auto offset CD ED detectors 1 and 2 mark Suppressors and 2 on off Reaction coil heater on off A C relays 1 and 2 open closed Assigning TTL Input Functions TTL input control functions are assigned in the Chromeleon Server Configuration program You can assign one or more functions to each input NOTE If two timebases are sharing the DC the TTL input functions are shared between the timebases For example if TTL input one is assigned
111. Detector Compartment Cond Detector EC Detector 4 gt EluentGenerator M Connected Show Audit Trail EGC_1 Control Bor Target Concentration 0 00 mM Applied Concentration 0 00 mM Status NOR ACT CR TC orf EGC_1 Information Serial Number _123456789012 Expiration Date Remaining lon Count 100 ce Figure 4 4 EG Control Panel 2 Under EGC Control enter a value in the Target Concentration field The allowable eluent concentration depends on several factors the flow rate suppressor type EluGen cartridge type and cartridge configuration For details refer to Table 4 1 and Table 4 2 Doc 065031 04 1 08 131 ICS 3000 lon Chromatography System Single Cartridge or Independent Dual Cartridge Configuration In the single cartridge configuration the EG contains one EluGen cartridge In the independent dual cartridge configuration the EG contains two EluGen cartridges operating mdependently on separate systems each cartridge is linked to a different DP SP For details refer to the EluGen cartridge manual Cartridge manuals are included on the Dionex Reference Library CD ROM P N 053891 EluGen Cartridge Eluent Concentration Range K CO 0 1 to 15 mM at 0 1to 1 0 mL min flow 0 1 to X mM at 1 0 to 2 0 mL min flow where X 15 flow KOH 0 1 to 100 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 3 0 mL min flow where X 100 f
112. ED Is On If the LED Is Flashing CONNECTED The DP SP is connected to a Does not flash Chromeleon or Chromeleon Xpress timebase ALARM A DP SP related problem has Does not flash occurred for example a pressure limit was activated Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause PUMP 1 FLOW PUMP 2 FLOW The DP SP is on and is delivering flow Does not flash PUMP 1 PRIME PUMP 2 PRIME Use the PRIME button to prime the pump The LED indicates whether the pump is being primed The pump is being primed POWER Use this POWER button for routine on off control of the DP SP When the power is on this LED is lighted To turn off the DP SP press and hold this POWER button for 2 seconds Note The main power switch is on the rear panel Does not flash Pump is always installed in the lower half of the DP SP enclosure SP only This button is not present 18 Doc 065031 04 1 08 2 DP SP Description 2 2 DP SP Interior Components The pump s mechanical components are located directly behind the front door of the module Figure 2 3 shows the mechanical components of a DP that contains both a gradient pump pump 1 and an isocratic pump pump 2 For servicing components the component mounting panel slides out about 5 cm 2 in for easy access to components To pull the panel out use the handles on the top and bottom of the
113. Fittings EG Replacing 281 Requirements 281 Fittings TC Replacing 327 Requirements 327 Flow restrictions 161 Front description DC Buttons and LEDs 41 Sample loading ports 43 Front description DP SP Buttons and LEDs 17 18 Front description EG Buttons and LEDs 31 Front description TC LEDs 91 Full scale analog output 82 Response range 81 Voltage output ranges 81 Fuses DC 48 Replacement procedure 307 Fuses DP SP 25 Replacement procedure 278 Fuses EG 38 339 Replacement procedure 296 Fuses TC 95 Replacement procedure 334 G Gas leak in TC 91 102 238 Gas sensor 102 238 Gas separator waste tube 36 55 Installation 114 Reordering 354 Gas vent line EG 38 Glassy carbon electrodes 57 GM 3 Gradient Mixer 22 182 350 GM 4 Gradient Mixer 22 182 350 Gold electrodes 57 Index 8 Doc 065031 04 1 08 Index Gradient proportioning valves 20 21 H Half cells 58 Heater Conductivity cell 53 Reaction coil 78 Heater DC 46 See also Temperature control DC High pressure limit Limit is tripped 198 Selecting 130 High pressure valve error 216 High pressure valves AM Controlling 76 Flow schematics 74 Installed in AM 73 Rebuilding 300 Reordering 353 Replacing 302 High pressure valves TC 93 98 Reordering 357 Humidity leak in TC 91 102 238 Humidity limits DC 341 TC 347 Humidity sensor 102 238 348 I T O option DC 49 79 3
114. I can be kept on hand for this purpose Using a Digital Voltmeter to Determine Reference Potential Shift 1 Using the reference electrode adapter cable connect the voltmeter s test probes to the center sockets of the unexposed electrode and the reference electrode being tested Immerse both reference electrodes in a solution of 0 1 M KCl Read the potential difference in mV between the unexposed electrode and the electrode being tested If it is greater than 50 mV try regenerating the electrode by soaking it in a solution containing 1 M KCl and 1 M HCL If this does not reduce the potential shift replace the electrode see Section 9 24 6 226 Doc 065031 04 1 08 TC Troubleshooting 8 29 Troubleshooting TC Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail A AcqOff without previous AcqOn This error occurs if the Chromeleon or Chromeleon Xpress program contains an AcqOff command but no AcqOn command To troubleshoot Every program should include one AcqOn command Enter the AcqOn command after the first injection A Acquisition is still on at program end This error occurs if a Chromeleon or Chromeleon Xpress program does not include a command that ends data acquisition To troubleshoot The AcqOn command must be paired with an AcqOff command Enter the AcqOff command at the appropriate point in the program Doc 0
115. IC Eluent Degasser tubing is ruptured If flow from the EG waste line is normal but there is no flow through the columns the tubing assembly inside the RFIC Eluent Degasser has ruptured Replace the degasser see Section 9 14 e Internal EluGen cartridge leak from membrane barrier Leakage from the membrane barrier may trip the DP SP low pressure limit and shut down the pump If all other causes of the low system pressure have been eliminated replace the EluGen cartridge see Section 9 12 Doc 065031 04 1 08 185 ICS 3000 lon Chromatography System NOTE The EG leak sensor cannot immediately detect leakage from the membrane barrier because these leaks exit the EG through the vent line 8 9 High System Backpressure e Restriction in the system plumbing 1 Begin pumping eluent through the system including the columns at the flow rate normally used 2 Work backward through the system beginning at the flow cell exit One at a time loosen each fitting and observe the pressure The connection at which the pressure drops abnormally indicates the point of restriction If the EluGen cartridge is the source of the high backpressure replace the outlet frit as instructed in the EluGen cartridge manual The manual is on the Dionex Reference Library CD ROM P N 053891 3 Ifthe restriction has caused such high pressure that the system cannot be operated you must work forward through the system adding parts one at a time until a
116. N C Conversely when the valve is on port 1 is open and port 0 is closed N C normally closed N O normally open COM common flow Figure 2 40 Three Way Low Pressure Valve Flow Schematics Doc 065031 04 1 08 75 ICS 3000 lon Chromatography System 2 17 3 High and Low Pressure Valve Control Chromeleon or Chromeleon Xpress is used to control the high and low pressure valves Commands for valve control can be included in a program see Figure 2 41 for automated control or the valves can be controlled manually from a Control panel see Figure 2 42 Program Wizard Relay and State Devices Options x Retention Time 2 min Duration 0 01 0 01 59999 90 s AM_HP1 State Qa 4 Qi B AM_HP2 AM_LP1 State Q Closed 9 Open AM_LP2 DC_ACRelay_1 DC_ACRelay_2 DC_LP1 e DC_LP2 f DC LP3 1 000 AM_HP1 A 0 01 2 000 AM_LP1 Open 0 01 a Help treat the selected device into the list lt Back Next gt Cancel Help Figure 2 41 Program Wizard Relay and State Devices Options Page 76 Doc 065031 04 1 08 2 DC Description ICS 3000 2 gt Home Sequence Control Status Autosampler Gradient Pumps Eluent Generator Detector Compartment Cond Detector EC Detector 3D Amp Plot Valves Detector Compartment Compartment_TC njectValve_1 LoadPosition
117. N VALVE ELUENT ELUENT ELUENT Cc B A OUTLET O O CHECK VALVE PUMP PUMP HEAD HEAD INLET CHECK VALVE VACUUM DEGAS Lo E PROPORTIONING l VALVE Figure 2 5 Gradient Pump Flow Schematic e Fluent flows from the reservoirs and through the vacuum degas chambers The selected proportions of eluent flow out of the proportioning valve assembly and into the inlet check valve on the primary pump head e The inlet check valve opens drawing eluent into the primary pump head At the same time the secondary piston pushes forward pushing eluent into the system After completing the intake the primary piston pushes eluent through the outlet check valve and into the secondary pump head e Flow exits the secondary pump head continues through the static mixer and is then directed to the remainder of the chromatography system the injection valve columns and detector 24 Doc 065031 04 1 08 2 DP SP Description 2 4 DP SP Rear Panel Figure 2 6 illustrates the rear panel of the DP SP 6 0 660006 Tubing Chase 2 Main Power Switch Fuse Holder and Power Receptacle Analog Pressure Output Digital I O Port USB Receptacle B Connectors USB Ports 3 A Connectors Exhaust Port from Vacuum Degas Module Waste Line from Drip Tray Figure 2 6 DP SP Rear Panel Tubing Chases The tubing chases route tubing
118. Pac MicroMembrane MMS Reagent Free and RFIC are trademarks of Dionex Corporation Adobe Adobe Reader and Acrobat are registered trademarks of Adobe Systems Incorporated Kel F is a registered trademark of 3M Corporation FastLock and MSQ Plus are trademarks of Thermo Electron Corporation PEEK is a trademark of Victrex PLC PharMed and Tygon are registered trademarks of Saint Gobain Performance Plastics Teflon is a registered trademark of E I duPont de Nemours amp Company TitanHP is a trademark of Rheodyne LLC Ultem is a registered trademark of General Electric Company PRINTING HISTORY Revision 01 May 2005 Revision 02 July 2006 Revision 03 September 2006 Revision 04 January 2008 Contents 1 Introduction 1 1 1 2 1 3 1 4 ICS 3000 System Overview 1 1 1 1 ICS 3000 System Components 2 1 1 2 ICS 3000 System Control 9 ICS 3000 System Documentation 10 The ICS 3000 System Operator s Manual 11 13 1 Overview LS Re Ve ONS PR R PR de 11 1 3 2 Safety Messages and Notes 12 Safety and Regulatory Information 14 14 1 Safety Labels si0c 000800e ememenmmadneniet 14 2 Description DP SP Description 2 1 2 2 DP SP Front Features 17 DP SP Interior Components
119. S lt 0 28 MPa 40 psi Table 9 3 Suppressor Operating Pressure Ranges To verify that the required amount of backpressure is being generated follow the instructions in the flier Backpressure Coil Pressure Test for Dionex Suppressors Document No 031759 which is shipped with the suppressor The instructions are also in the suppressor manual on the Dionex Reference Library CD ROM P N 053891 312 Doc 065031 04 1 08 9 e DC Service 3 Ifa bubble is still trapped in the cell try these techniques to remove it e Loosen and then tighten the cell outlet fitting e Temporarily disconnect the backpressure coil from the suppressor REGEN IN port and then plug and unplug the end of the tubing with your fingertip 2 or 3 times to create a pressure difference 9 24 ED Service Procedures 9 24 1 Disconnecting the Amperometry Cell Before performing an amperometry cell service procedure follow these instructions to disconnect the cell 1 Turn off the cell voltage from the Control panel in Chromeleon or Chromeleon Xpress 2 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 3 Disconnect the inlet and outlet lines from the amperometry cell and disconnect the two electrical cables see Figure 9 32 4 Grasp the cell by the cell body and pull straight out to remove it from the detector Disconnect cables Disconnect inlet li
120. Sample Tray 120 DP SP Startup 4 4 Set Up the Eluent Reservoirs 123 4 5 Set Up the Piston Seal Wash System 124 4 6 Start the Pump praspar ata sga wns rats ae ale dd glad ie 127 EG Startup 4 7 Setting the Eluent Concentration 131 Doc 065031 04 1 08 Contents DC Startup 4 8 Startthe D S SES tt Rte wna canteen total dons lesa stark waa Raa trpo ah len ata 135 4 9 E quilibrate the System and Verify Operational Readiness 136 TC Startup 4 10 Start the TO asta hada SLs ancy tena tel ane Wanted ant en thane Sn es 137 4 11 Equilibrate the System and Verify Operational Readiness 138 5 Operation S OVERVIEW seston esn ne pe aon lens ne nn ds 139 5 2 Loading Samples with an Autosampler 140 5 3 Loading Samples with a Syringe 140 5 3 1 Loading Samples with a Syringe Push Method 141 5 3 2 Loading Samples with a Vacuum Syringe Pull Method 143 5 4 Example Commands for Loading and Injecting Samples 144 5 4 1 Commands for an AS Autosampler 144 5 4 2 Commands for an AS40 Autosampler 144 5 4 3 Commands for a Remote Inject Device 145 5 5 Manual Sample Processing 146 5 5 1 Saving Manual Data 147 5 6 Automatic Ba
121. TC 347 Dionex Technical Support 169 Index 4 Doc 065031 04 1 08 Index Disposable working electrodes 57 Reordering 353 Drain port TC 97 Drifting baseline 178 Dual Pump DP 2 3 Analog pressure output 27 Delay volume 336 Digital I O port 26 Dimensions 335 Electrical specifications 335 Flow rate accuracy 336 Flow rate range 336 Fuse replacement 278 Fuses 26 335 Gradient proportioning accuracy 336 High pressure limit 336 Low pressure limit 336 Maintenance annual 162 Maintenance daily 161 Maintenance periodic 162 Maintenance weekly 161 Moduleware 20 Operating humidity 335 Operating pressure 336 Operating temperature 335 Piston replacement procedure 271 Piston seal replacement procedure 265 267 271 Piston seal wash tubing replacement procedure 274 Power requirements 335 Pressure limit tripped 185 209 210 Pressure limits for EG 130 209 210 Pressure ripple 336 Priming procedures 259 261 Priming valve knob seal replacement 276 Product warranty 257 Selecting pressure limits 130 Shutdown procedure 151 Spare parts 349 Start up procedures 123 Static mixer 22 Status bar buttons and LEDs 17 System configurations 105 USB connections 28 Vacuum degassing module 336 Waste lines 28 Weight 335 Dual system configuration 108 109 E EC cell See Amperometry cell ED cell See Amperometry cell ED cell disconnected error 215 216 Electric
122. TC tubing and fittings 327 Plumbing configuration drawings 105 112 Polarity Analog output 82 Polishing kit ED Reordering 354 Polishing working electrodes 317 Post column reagent addition 44 73 112 Potassium carbonate eluent 34 35 Potassium hydroxide eluent 34 Potential shifting 58 226 Power cord 296 305 307 334 Power LED DC 42 Power LED DP SP 18 Power LED EG 32 Power LED TC 92 Power output DC T O option 49 79 84 Power receptacle DC 48 DP SP 25 EG 38 TC 95 Power requirements DC 341 DP SP 335 EG 339 TC 347 Power switch rear panel DC 48 DP SP 25 EG 38 TC 95 Pre concentration 44 73 Predictive Performance 104 Pressure limit settings 130 Pressure limits tripped 185 Pressure ripple 336 Pressure transducer 20 Pressurizable eluent reservoirs Installation 30 Priming procedures DP SP 259 From the Control panel 261 With the Prime button 260 261 Priming valve Leakage from knob 200 Index 12 Doc 065031 04 1 08 Index Seal knob replacement procedure 276 Problems See Troubleshooting Processing samples 139 147 Automatically batch 147 Manually 146 Product warranty voiding 257 Program Wizard Waveforms 65 Programs Chromeleon Chromeleon Xpress Autosampler control 140 144 Creating programs 147 Remote inject device control 145 Proportioning valves 20 21 Leaks 200 Malfunction 182 183 Pulsed amperometry 61 3D data 6
123. TTE Inputs nier sate saga dee eee eee bs ee bone EE 86 TC Description 2 19 TC Front Features 91 2 20 TC Interior Components 93 2 219 TE Rear PANNE Sn she men se LI Rues 95 2 22 Injection Valves 3 144 ea wa ihe vba lunaire 98 2 22 1 Injection Valve Operation 98 2 22 2 Injection Valve Plumbing 100 2 23 Column Identification ID System 101 Doc 065031 04 1 08 iii ICS 3000 lon Chromatography System 2 24 Gas and Humidity Sensors 102 2 25 Theory of Operation 103 2 25 1 Predictive Performance 104 3 Configurations 349 Overview fected oy ev acecsthag tan eh deste Regge tau Re Wade Neh ES 105 4 Startup 4 1 Operating Precautions 113 4 1 1 EG Operating Precautions 113 4 1 2 ED Amperometry Cell Operating Precautions 115 4 2 System Startup Checklist 118 43 Preparing Samples 119 4 3 1 Collecting and Storing Samples 119 4 3 2 Pretreating Samples 119 43 3 Diluting Samples 120 4 3 4 Fill the Autosampler Vials and Load the
124. This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the ICS 3000 system when properly followed Safety messages appear in bold type and are accompanied by icons as shown below Indicates an imminently hazardous situation which if not avoided will result in death or serious injury Indicates a potentially hazardous situation which if not avoided could result in death or serious injury Indicates a potentially hazardous situation which if not avoided may result in minor or moderate injury Also used to identify a situation or practice that may seriously damage the instrument but will not cause injury Indicates that the function or process of the instrument may be impaired Operation does not constitute a hazard 12 Doc 065031 04 1 08 1 Introduction gt DANGER gt AVERTISSEMENT gt MISE EN GARDE gt ACHTUNG gt WARNUNG gt VORSICHT Messages d avertissement en fran ais Signale une situation de danger imm diat qui si elle n est pas vit e entrainera des blessures graves a mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves a mortelles Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entra ner des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrai
125. a degradation in performance baseline noise tailing peaks etc polish the electrode as instructed in Section 9 24 3 Over the lifetime of the conventional working electrode the surface may gradually become pitted or receded Receded electrodes can be repaired by sanding with 600 grit sandpaper Continue sanding until the metal surface is again flush with the Kel F electrode block surface Then polish the electrode with coarse and fine polishing compounds as instructed in Section 9 24 3 Doc 065031 04 1 08 115 ICS 3000 lon Chromatography System e To help determine when the reference electrode needs regenerating or replacing monitor the pH value displayed on the Control panel in Chromeleon or Chromeleon Xpress e To have an alarm displayed in the Audit Trail if the pH exceeds certain values set pH limits in Chromeleon or Chromeleon Xpress To monitor the cell pH 1 At installation calibrate the pH electrode see Section 9 24 5 When you run your first chromatographic program note the pH value displayed on the Chromeleon or Chromeleon Xpress Control panel Thereafter monitor the pH value to determine whether there is a shift in the pH A shift in the pH reading indicates a change in the Ag AgCl reference potential If the pH value shifts by 0 5 pH unit from the value first observed check the reference electrode see Section 8 28 6 Electrochemical Detector Settings Signal i M
126. a read only parameter To troubleshoot Do not attempt to reset read only parameters This operation may affect the oven s operation on timebase x Which is currently running a batch If batch processing is in progress when you attempt to change a property such as Temperature or TempCtrl that affects the entire TC this error occurs To troubleshoot To avoid disrupting operation cancel the command 250 Doc 065031 04 1 08 TC Troubleshooting O Unknown error code This error occurs if Chromeleon or Chromeleon Xpress does not recognize error code sent by the TC firmware Moduleware To troubleshoot The firmware cannot be serviced by the user Contact Dionex for assistance A Unknown format of the card data This error occurs if Chromeleon or Chromeleon Xpress does not recognize the format of data stored on the column ID chip card To troubleshoot 1 Inthe Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to display the items underneath 2 Click the plus sign beside the column name 3 Select FormatChipCard and click Execute 4 Ifthe error occurs again insert a new column ID chip card see Section 9 26 _ Xposition error This error occurs if a TC injection valve fails to switch position within the time allotted To troubleshoot 1 Ifa sequence is being executed terminate the sequence by clicking Abort Batch on the Sequence Control panel 2 Press
127. ad see Figure 4 3 NOTE The drop sensor cap is not installed on current pump models Drop Sensor Cap included only on early pump models Seal Wash Reservoir Inlet Line Figure 4 3 Optional Drop Sensor Reservoir Cap Connections 6 Follow these steps to activate the piston seal wash function a In Chromeleon or Chromeleon Xpress select Command on the Control menu or press the F8 key 126 Doc 065031 04 1 08 4 DP SP Startup b In the Commands dialog box select the pump name c Select the RearSealWashSystem command and select an option e Select Internal if the standard seal wash reservoir is installed e Select Automatic if the drop sensor cap reservoir is installed d Click Execute 4 6 Start the Pump 1 Press the POWER button on the front of the DP SP 2 Ifany of the following conditions applies prime the pump see Section 9 3 before proceeding e The eluent has been changed e The eluent line is new empty e The eluent line contains air 3 To display the ICS 3000 panel tabset follow one of the steps below e If Chromeleon is installed launch the application and click the Default Panel Tabset toolbar button e IfChromeleon Xpress is installed launch the application this automatically displays the ICS 3000 panel tabset 4 The panel tabset opens to the Home panel by default This panel displays basic status information for each instrument in the system In addition a
128. ages If any of the following alarm conditions occurs a message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail CR TC1 over current Or CR TC2 over current This error occurs when the current applied to the CR TC exceeds the maximum current allowed The CR TC current is automatically turned off to prevent damage to the CR TC This error may also occur if liquid flow to the CR TC is interrupted To troubleshoot 1 Check the CR TC cable connection to the electrical bulkhead see Figure 2 8 2 Refer to Section 8 23 to determine why liquid flow stopped 3 Ifthe error message appears again contact Dionex for assistance The CR TC control electronics may have malfunctioned NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user CR TC1 stopped due to zero flow Or CR TC2 stopped due to zero flow This message appears if you turn off the pump flow while the EluGen cartridge current and CR TC are on The CR TC current is automatically turned off to prevent damage to the CR TC Doc 065031 04 1 08 203 ICS 3000 lon Chromatography System To troubleshoot If the pump stopped unexpectedly follow the troubleshooting steps in Section 8 23 EG1 cartridge disconnected Or EG2 cartridge disconnected This error occurs if Chromeleon or Chromeleon Xpress sends a command to set an EG parameter when the EluGen cartridge is disconnect
129. al separation is performed at the nominal temperature This minimizes fronting and tailing of peaks as well as retention time variations Column ID Chip Card Slots The TC column ID identification system lets you store column specific information on a memory card and read the information at any time Up to four column ID chip cards can be installed at the same time The TC is shipped with two column ID chip cards P N 5710 1500 An optional Column ID Kit P N 066353 containing five chip cards is available See Section 2 23 for details about the column ID system 94 Doc 065031 04 1 08 TC Description 2 21 TC Rear Panel Figure 2 53 illustrates the rear panel of the TC Main Power Switch Digital 1 0 USE Receptacle Drain Port Fuse Holder and Connectors 2 B Connector Power Receptacle Figure 2 53 TC Rear Panel Main Power Switch Fuse Holder and Power Receptacle The rear panel power switch is the main power switch for the TC Turn on the main power switch before initial operation and leave the switch on unless instructed to turn it off for example before performing a service procedure NOTE For routine on off control of the TC use the POWER button on the front of the module To turn off the TC press and hold the POWER button for 2 seconds The fuse holder contains two 2 amp fuses P N 954776 For instructions on how to change the fuses see Section 9 29 The power cord
130. al specifications DC 341 DP SP 335 EG 339 TC 347 Electrochemical detection DC amperometry 60 Integrated amperometry 61 Pulsed amperometry 61 Electrochemical Detector ED 2 4 57 3D data 68 71 Amperometry cell description 57 Data storage 68 Description 44 57 Detection modes 57 Reference electrode 58 Reordering information 353 Replacement procedure 326 Shutdown procedure 155 Specifications 345 See also Amperometry cell Electrodes 58 Reference 57 Working 57 Electrolysis gases Purging from eluent 34 113 Venting from system 38 Eluent concentration 131 133 Doc 065031 04 1 08 Index 5 ICS 3000 lon Chromatography System Eluent generation Electrolysis gases 34 Eluent Generator EG 2 5 Alarm LED is lighted 35 207 210 Backpressure 34 Backpressure coil 178 Component description 33 35 Concentration range 340 Dimensions 339 Electrical connections consumables 36 Eluent concentration ranges 131 133 EluGen cartridges 5 Fuse cartridge 38 Fuses 38 Gas vent line 38 Leak sensor 35 207 Liquid flow path 39 Liquid leaks 207 209 Main power switch 38 Maintenance 163 Operating humidity 339 Operating precautions 113 Operating temperature 339 Power LED does not light 208 Power requirements 339 Pump pressure limits 210 Rear panel description 37 38 Selecting the eluent concentration 131 Shutdown procedures 153 Spare parts 351 Status bar buttons a
131. and acetonitrile Pressurizable reservoirs allow eluents to be stored under a specific atmosphere Never pressurize eluent reservoirs above 0 07 MPa 10 psi Pressurizing reservoirs above this limit can cause the reservoir to explode CAUTION Ne mettez jamais les r servoirs d luants sous une pression sup rieure 0 07 MPa 10 psi MISE EN GARDE Doc 065031 04 1 08 29 ICS 3000 lon Chromatography System Setzen Sie den Eluentbeh lter auf keinen Fall einem Druck ber 0 07 MPa aus VORSICHT 2 6 EO Optional The ICS 3000 Eluent Organizer EO holds eluent reservoirs in a liner that contains spills and leaks Up to two EOs can be installed on top of the DC Each EO accommodates up to four 1 liter or 2 liter reservoirs or up to two 4 liter reservoirs The EO is typically ordered configured with four 2 liter reservoirs P N 062629 All eluent reservoirs available for use with the DP SP can be pressurized If you plan to pressurize the eluent reservoirs an optional regulator kit is required The kit is available in two versions e When the DC is installed as the topmost module in the system the EO Regulator Kit P N 063493 is required The kit includes a pressure regulator and gauge assembly with four outputs for connections to four eluent reservoirs as well as the tubing and connection fitting required e When the TC ICS Series Variable Wavelength Detector or ICS Series Photodiode Array Detector is install
132. andard bore systems Connections between other system components e Use 1 8 in fittings P N 052267 and ferrules P N 048949 for connections to the suppressor REGEN OUT port and the eluent reservoir e Use double cone 10 32 ferrule fittings P N 043276 and 10 32 bolts P N 043275 for all other tubing connections For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Dionex Reference Library CD ROM P N 053891 Doc 065031 04 1 08 297 ICS 3000 lon Chromatography System Use a tubing cutter to cut tubing to the required length Make sure the cut is at a right angle to the length of the tubing and there are no nicks or burrs on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 062614 dual P N 063408 single Refer to the instructions provided with the cutter 9 18 Replacing the Leak Sensor 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 2 Press the POWER button on the front of the DC to turn off the DC To avoid injury wait for the DC to cool down before opening the door or performing any maintenance or service procedures CAUTION Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hi
133. anging a secondary column property For a list of primary and secondary properties refer to the Chromeleon or Chromeleon Xpress Help Properties cannot be changed A chip card has not been A inserted properly Check the CardState property for all cards and reinsert those indicating BusBlocked This error occurs if you attempt to change column ID properties when at least one column ID chip card is inserted incorrectly To troubleshoot 1 Inthe Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to display the items underneath 2 One ata time click the plus sign beside each column name and select the CardState command If the status is BusBlocked remove the card from the card slot and reinsert it When the card is properly installed the Dionex logo on the card faces up and the LED on the memory slot is green Doc 065031 04 1 08 243 ICS 3000 lon Chromatography System gt gt gt P Properties cannot be changed if the compartment door is open This error occurs if you attempt to change column ID properties when the TC door is open or is not fully closed To troubleshoot 1 Verify that the door is fully closed 2 Ifthe door is not fully closed check for and remove any obstruction 3 Ifthe door is fully closed but the error persists contact Dionex for assistance Properties cannot be changed there is no card in the card reader This error occurs if yo
134. are no liquid leaks in the flow system 3 Make sure the priming valve is closed see Figure 2 3 To close the valve turn the knob clockwise until closed Tighten no more than fingertight Do not use any tools to tighten the priming valve Overtightening may destroy the cap seal Open or close the priming valve only when the system pressure is down Doc 065031 04 1 08 197 ICS 3000 lon Chromatography System 8 14 DP SP Stops e Program or other remote input instructed the pump to stop If no error message is displayed in the Audit Trail the DP SP was probably instructed to stop by the Chromeleon or Chromeleon Xpress program the computer or other remote signal source If you do not want the pump to stop take the appropriate preventive action edit the program etc e Low pressure limit was tripped 1 Verify that the Minimum Pressure setting is several hundred psi below the Current Pressure reading on the Chromeleon or Chromeleon Xpress Control panel Make sure there are no liquid leaks in the flow system Check the Eluent Level Display on the Chromeleon or Chromeleon Xpress Control panel to verify that eluent is present in the selected channel If the eluent reservoir is empty refill it or select a channel that does have eluent Prime the pump before resuming operation see Section 9 3 Make sure the priming valve is closed see Figure 2 3 To close the valve turn the knob clockwise until closed Tighten n
135. ash solution detected by the sensor while the peristaltic pump is idle 55 minutes per hour exceeds the leak detection threshold To troubleshoot 1 Inspect the piston seals for leakage Replace the piston seals and O rings as needed see Section 9 5 Increase the value for the rear seal leak threshold a In Chromeleon or Chromeleon Xpress select Command on the Control menu or press the F8 key b In the Commands dialog box select the pump name c Select the RearSealLeakCounter command d Enter a new value and click Execute Doc 065031 04 1 08 195 ICS 3000 lon Chromatography System The rear seal leak sensor is malfunctioning This error occurs only when the cap on the seal wash reservoir is equipped with a drop sensor and the sensor is very dirty To troubleshoot 1 Clean the sensor electrodes with water or solvent 2 Ifthe message appears again the leak sensor may be defective Contact Dionex for assistance This function cannot be adjusted by the user This error occurs if you attempt to change a parameter that users are not allowed to adjust To troubleshoot Only Dionex Service Representatives can change this parameter Upper pressure limit exceeded This error occurs if the upper pressure limit specified in the program is exceeded The running batch is aborted default and this message appears To troubleshoot 1 Check all tubing connections for signs of blockage replace a
136. ay the items underneath 2 Click the plus sign beside the column name 3 Select FormatChipCard and click Execute to reinitialize the chip card 246 Doc 065031 04 1 08 TC Troubleshooting CD The injections limit for the column has been exceeded Or O The injections limit will be exceeded for the column x Chromeleon and Chromeleon Xpress monitor the number of injections done with each column and display an appropriate message shown above at the following times when the injections limit is about to be exceeded or has been exceeded To troubleshoot Replace the column The nominal temperature must be set within the current limits This error occurs if the selected TC temperature setting is outside the range specified by the Temperature LowerLimit and Temperature UpperLimit commands To troubleshoot Select a valid temperature setting The nominal temperature value is out of range defined by the active column ID This error occurs if the selected TC temperature setting is outside the range specified by the Column_x Temp_LowerLimit and Column_x Temp_ UpperLimit commands To troubleshoot Select a valid temperature setting Doc 065031 04 1 08 247 ICS 3000 lon Chromatography System The oven is not fully operable yet Check the values of Standby Ready Door and CardState Each time the TC power is turned on the firmware Moduleware runs a series of s
137. be lower than the Limit Error page 249 threshold There was already an AcqOff command for this channel Warning page 250 before There was already an AcqOn command for this channel Warning page 250 before This function cannot be adjusted by the user Abort page 250 This operation may affect the oven s operation on Warning page 250 timebase x which is currently running a batch Two AcqOn commands for the same channel The Error page 250 second chromatogram will overwrite the first Unknown error code Warning page 251 Unknown format of the card data Error page 251 USB LAN communication error Please check Abort page 235 communication cable and instrument s power Value for name parameter is not within valid range Warning page 242 Value passed x will be substituted by y Value x replaced by valid table entry y Warning page 242 X position error Abort page 251 You do not have the privilege to approve the module s Error page 252 qualification You do not have the privilege to change the performance Error page 252 limits You do not have the privilege to change the qualification Error page 252 intervals Doc 065031 04 1 08 177 ICS 3000 lon Chromatography System 8 2 Noisy Baseline Eluent is contaminated 1 Clean all eluent reservoirs thoroughly inside and out with ASTM Type I 18 megohm cm filtered and deionized water and dry with clean particulate free air If a reservoir still app
138. cessing 146 Overview 139 Sample preparation 119 Organic solvent 58 Oven DC 46 See also Temperature control DC Oven TC 92 See also Temperature control TC Oven LED TC LED is flashing 92 253 LED is lighted 92 Oven LEDs DC LED is flashing 41 LED is lighted 41 P PAD See Pulsed amperometry Panel tabset 9 Home panel 9 127 How to display 127 Panels Chromeleon Chromeleon Xpress Control panel 146 Parameters Chromeleon Chromeleon Xpress commands 147 Doc 065031 04 1 08 Index 11 ICS 3000 lon Chromatography System Peak height Reproducibility 53 Peaks Fronting 94 Reversed 82 Tailing 94 185 Periodic maintenance DC 165 DP SP 162 TC 168 pH gradient 58 pH half cell 58 pH limits 117 pH reading Adjusting potentials for 59 Always 7 0 223 Cannot be set to 7 0 224 Effect on potentials 58 Monitoring 59 Nonexistent 225 pH Ag AgCl reference electrode 57 See also Reference electrode Photodiode Array Detector 2 7 Regulator Bracket Kit 30 Piston seal wash solution 22 151 Piston seal wash system 22 124 Activation 22 Dual pump seal wash option 22 124 350 Replumbing the DP connections 124 Setup 125 Piston seals Replacement procedure 265 Pistons Replacement procedure 271 Platinum electrodes 57 Plot I t 69 Plot signal 146 Plumbing Replacing DC tubing and fittings 297 Replacing DP SP tubing and fittings 257 Replacing EG tubing and fittings 281 Replacing
139. ch wrench to tighten an additional one quarter to one half turn Overtightening may damage the pump head and check valve housing IMPORTANT and crush the check valve seats 14 Push the component mounting panel back into the enclosure Close the DP SP door 15 Press the POWER button on the front of the DP SP to turn on the pump 264 Doc 065031 04 1 08 9 DP SP Service 16 Select the Connected check box on the Control panel to reconnect the pump to the software 17 Click Motor on the Control panel to start the pump flow 9 5 Replacing a Piston Seal A defective piston seal allows leakage past the piston This may cause unstable flow rates and baseline noise in addition it may make it difficult to prime the pump The piston seal replacement procedure consists of 9 5 1 Removing the pump head and piston see Section 9 5 1 Cleaning the piston see Section 9 5 2 Removing the main piston seal see Section 9 5 3 Removing the piston seal wash seal see Section 9 5 4 Installing new seals see Section 9 5 5 Reinstalling the piston and pump head see Section 9 5 6 Removing the Pump Head and Piston 1 Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Control panel When the system pressure reaches zero do the following e Disconnect the pump from the software by clearing the Connected check box on th
140. cludes five chip cards These are the main steps required to implement the column ID system e Specify the column you want to monitor e Install a column ID chip card for the column e Close the TC door and select the column properties to be monitored To select the column to be monitored 1 Launch the Chromeleon Server Configuration program 2 In the timebase right click the TC and select Properties on the context menu 3 Inthe TC Properties dialog box select the Components tab to display the Components tab page see Figure 9 42 Dionex TC Thermal Compartment General Components Configuration Relays Inputs Error Levels Installed components Left Valve controlled by AS Right Valve HOpots x D controlled by AS M Column fColumn_A N ICS 3000 Le D Column B F Column C I Column D Figure 9 42 TC Properties Dialog Box Components Tab Page 4 Select the check box for the column to be monitored A B C or D and click OK 328 Doc 065031 04 1 08 TC Service To install a column ID chip card 1 To attach a column ID chip card to the column wrap the strap around the column insert the rivet into one of the holes on the strap and press to secure the strap to the column see Figure 9 43 Figure 9 43 Attaching the Column ID System to the Column 2 Insert the chip card with the Dionex logo facing up into the appropriate card reader A B C or D along the top of the compartment see Figure 9 44
141. components and functions see Figure 2 51 CONNECTED LOAD INJECT LOAD e e VALVE 1 VALVE 2 INJECT Figure 2 51 TC Status Bar of a gas or humidity leak inside the TC or a valve or oven error was detected Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause LED Label If the LED Is On If the LED Is Flashing CONNECTED The TC is connected to a Does not flash Chromeleon or Chromeleon Xpress timebase ALARM A sensor detected the presence Does not flash VALVE 1 LOAD VALVE 2 LOAD VALVE 1 INJECT VALVE 2 INJECT Indicates whether the injection valve is in the Load or Inject position Valve error See Section 8 30 for troubleshooting Doc 065031 04 1 08 91 ICS 3000 lon Chromatography System LED Label If the LED Is On If the LED Is Flashing OVEN The TC is at its set temperature The TC is transitioning to the set temperature The TC is not ready for operation If the LED is flashing and the ALARM LED is lighted an oven error has been detected See Section 8 30 for troubleshooting POWER When the power is on this LED Does not flash is lighted Use the POWER button on the front of the TC for routine on off control To turn on the TC press the POWER button To turn off the TC press and hold the POWER button for 2 seconds NOTE The main power switch is on the TC rear panel see Figure 2 53
142. connect the TC to the Chromeleon server Check the Audit Trail for messages indicating whether the module was successfully connected Device not found on the USB Or USB LAN communication error Please check communication cable and instrument s power This error occurs if there is a problem with the connection between the TC and the Chromeleon server or with the power supply To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 If you cannot identify the cause of the error contact Dionex for assistance Doc 065031 04 1 08 235 ICS 3000 lon Chromatography System Either the current date is later than the expiration date for x or the program or batch will end later than 24 hours before the expiration time for x Chromeleon and Chromeleon Xpress compare the current date with the column expiration date during injection or before beginning batch processing This error occurs if the expiration date has already passed or if batch processing is scheduled to start less than 24 hours before the expiration date To troubleshoot Replace the column Error deleting flash memory This error occurs if during a firmware Moduleware download the existing firmware cannot be erased from memory To troubleshoot Flash memory cannot be serviced by the user Contact Dionex for assistance Error during storing of the card data to the chip card This error occu
143. ction 5 3 1 for connection instructions Disconnect the waste line from port W 6 on the injection valve see Figure 5 5 and attach a shorter line 25 to 30 cm 10 to 12 in of PEEK or Teflon tubing Place the free end of the line into the sample Verify that the injection valve is in the Load position If it is not switch the valve by clicking the valve control on the Control panel or pressing the VALVE button on the front of the DC Insert a 5 cc syringe into the sample loading port on the DC front door and pull out the plunger to draw the sample into the injection valve Switch the injection valve to the Inject position by clicking the valve control on the Control panel or pressing the VALVE button on the front of the DC Figure 5 5 Loading Sample with a Vacuum Syringe Pull Method Doc 065031 04 1 08 143 ICS 3000 lon Chromatography System 5 4 Example Commands for Loading and Injecting Samples The following examples show Chromeleon or Chromeleon Xpress program commands for loading and injecting samples 5 4 1 Commands for an AS Autosampler 0 000 Load Switch the valve to Load Wait CycleTimeState Wait for cycle time if any Inject Switch the valve to Inject Wait InjectState Wait for injection to finish CDetl Autozero Zero the baseline CD 1 AcqOn Start data acquisition 14 000 CD 1 AcqOff Stop data acquisition 5 4 2 Commands for an AS40 Autosampler A rela
144. ctrolyte concentrate solution for eluent generation EluGen Cartridge Part Number Function EGC I KCO 058904 Generates potassium carbonate eluent EluGen Cartridge for anion exchange separations Note Produces a carbonate bicarbonate mixture when installed with the EPM Electrolytic pH Modifier P N 063175 and EGC CO Mixer P N 061686 EGC II KOH 058900 Generates potassium hydroxide eluent EluGen Cartridge for anion exchange separations EGC II LiOH 058906 Generates lithium hydroxide eluent for EluGen Cartridge anion exchange separations EGC I MSA 058902 Generates methanesulfonic acid eluent EluGen Cartridge for cation exchange separations EGC II NaOH 058908 Generates sodium hydroxide eluent for EluGen Cartridge anion exchange separations For more information refer to the EluGen cartridge manual The manual is included on the Dionex Reference Library CD ROM P N 053891 RFIC Eluent Degasser The RFIC Eluent Degasser P N 062137 contains a tubing assembly that purges the electrolysis gas from the freshly generated eluent before it is directed to the separator column Backpressure Coil Optional The EluGen cartridge requires at least 14 MPa 2000 psi of system backpressure for removal of electrolysis gas from the eluent produced by the cartridge A system backpressure of 16 MPa 2300 psi is ideal If necessary increase the system backpressure by installing a backpressure coil between the
145. d on an AM Two models are available 6 port P N 061961 and 10 port P N 061962 Both models are electrically activated two position valves Figure 2 38 and Figure 2 39 show the liquid flow path through the valve ports at each valve position POSITION A POSITION B 5 4 6 3 1 2 Figure 2 38 High Pressure Switching Valve Flow Schematics 6 Port Valve POSITION A POSITION B 6 Figure 2 39 High Pressure Switching Valve Flow Schematics 10 Port Valve 74 Doc 065031 04 1 08 2 DC Description Valve port connections to chromatography components vary depending on the application Refer to Chapter 3 for the configuration schematic for your application Valves are controlled by Chromeleon or Chromeleon Xpress see Section 2 17 3 2 17 2 Low Pressure Valves Up to two low pressure valves can be mounted on an AM The valves are either two way or three way valves The two way valves provide on off control of liquid flow in one direction while the three way valves provide on off control in two directions see Figure 2 40 Valve port connections to chromatography components vary depending on the application Refer to Chapter 3 for the system flow schematic for your application Valves are controlled by Chromeleon or Chromeleon Xpress see Section 2 17 3 OFF POSITION ON POSITION Note When the valve is off i e it is not energized port 0 is open N O and port 1 is closed
146. dary pump head e One waste line exits the drip tray and is routed to the rear panel Place the free ends of the waste lines into one waste container To maintain a positive siphon position the waste container below the level of the pump NOTE To ensure proper drainage the waste lines must remain above the liquid level in the waste container 28 Doc 065031 04 1 08 2 DP SP Description 2 5 Eluent Reservoirs The following reservoirs are available for use with the DP SP e liter plastic reservoir P N 063291 e 2 liter plastic reservoir P N 062510 e 4 liter plastic reservoir P N 063292 Do not use the 2 liter plastic reservoir P N 062510 for offline vacuum degassing of eluents The reservoir was not designed for this purpose CAUTION N utilisez pas le r servoir en plastique de 2 litres N P 062510 pour le d gazage vide hors ligne d luants Le r servoir n a pas t con u a cette fin MISE EN GARDE Verwenden Sie den 2 Liter Plastikbeh lter Bestell Nr 062510 nicht zum Offline Vakkum Entgasen von Eluenten Der Beh lter ist daf r nicht ausgelegt VORSICHT All eluent reservoirs listed above are pressurizable Although the DP SP does not require pressurized reservoirs Dionex recommends pressurizing reservoirs with helium or nitrogen under the following circumstances e When using eluents that are sensitive to contamination e When combining aqueous and nonaqueous components for example water
147. display an appropriate message shown above at the following times when the due date for the next service is approaching and when the due date is overdue The Service WarningPeriod property determines the number of days before the due date that the warning is first displayed To troubleshoot Contact Dionex for information about performing annual preventive maintenance The DC TC Preventive Maintenance Kit P N 061796 contains all required replacement parts 240 Doc 065031 04 1 08 TC Troubleshooting A No chip card in the reader for the column x This error occurs if a column ID chip card is not installed for the column identified in the message To troubleshoot Install a column ID chip card for the column see Section 9 26 Or if you do not want to store information about this column follow the steps below to disable this option 1 Inthe Server Configuration program right click the TC and select Properties on the context menu 2 Select the Components tab in the Properties dialog box Clear the check mark beside the column name and click OK No response from x for x seconds Or No response from x for x seconds Device disconnected This error occurs if there is a communication failure between the TC and the PC on which Chromeleon or Chromeleon Xpress is installed To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 If you cannot identify the cau
148. ds Device disconnected Abort page 241 Operating columns above 70 C could affect column Warning page 242 performance Verify recommended column operating conditions before setting temperature above 70 C Parameter x value exceeded its allowed range Set to Warning page 242 closest valid value y Primary property x is already assigned and cannot be Error page 243 changed Properties cannot be changed A chip card has not been Error page 243 inserted properly Check the CardState property for all cards and reinsert those indicating BusBlocked Properties cannot be changed if the compartment door is Error page 244 open Doc 065031 04 1 08 175 ICS 3000 lon Chromatography System TC Related Audit Trail Error Message Default Severity See Level Properties cannot be changed there is no card in the Error page 244 card reader Raw data file x cannot be created Warning page 244 Raw data file x cannot be created Continuing with Warning page 244 network failure protection Raw data file x cannot be written Warning page 244 Raw data file x cannot be written Continuing with Warning page 244 network failure protection Starting data acquisition manually will overwrite any data Warning page 245 which has been acquired so far TC Firmware download failed Abort page 230 TC is not remote Abort page 235 The command can format only chip ca
149. dual products for instructions These manuals are provided on the Dionex Reference Library CD ROM P N 053891 6 4 Amperometry Cell Storage 6 4 1 Short term Storage of the Amperometry Cell If the cell will not be used for a short period of time less than 2 days disconnect the tubing from the inlet and outlet fittings and install fitting plugs NOTE If the reference electrode remains in the cell but eluent is not being pumped through the cell the reference electrode frit may partially dry out If this occurs regenerate the electrode by soaking it in a solution containing 1 M KCI and 1 M HCI 6 4 2 Long term Storage of the Amperometry Cell If the cell will not be used for 2 days or more remove the pH reference electrode and store it in a solution of saturated KCl as instructed in the procedure below 1 Prepare a saturated solution of KCI in ASTM filtered Type I 18 megohm cm deionized water 2 Locate the cap in which the electrode was shipped and fill it two thirds full with the prepared KCI solution 3 Remove the pH reference electrode from the cell Doc 065031 04 1 08 155 ICS 3000 lon Chromatography System 4 Insert the electrode into the cap and screw on the cap see Figure 6 2 5 Make sure there is no air bubble in the cap Add more KCI solution if needed weg Storage Cap J Figure 6 2 Reference Electrode in Storage Cap 156 Doc 065031 04 1 08 6 6 6 7 TC Shutdown Co
150. e When the injection valve is switched to inject the remote inject device signals Chromeleon or Chromeleon Xpress that injection occurred A Got inject response message appears in the Audit Trail and program execution resumes Suppressorl Type ASRS 4mm Commands before the hurrentsar 75 mA Inject command are executed Flow 1 000 ml min 0 000 Inject The program pauses and waits for the inject signal CDetl Autozero When the inject signal is CD 1 AcqOn received program execution resumes 14 000 CD 1 AcqOff Notes e When configuring the properties of the remote inject device in the Chromeleon Server Configuration program select the name of the DC injection valve InjectValve_Left or InjectValve_Right in the Inject Port list on the General tab page e The VALVE 1 and VALVE 2 buttons on the front of the DC must be enabled in Chromeleon or Chromeleon Xpress in order to use them to manually switch the injection valves To enable a button open the Commands dialog box press F8 and select the Valve1 Button or Valve2Button command in the list of commands for the DC device Doc 065031 04 1 08 145 ICS 3000 lon Chromatography System 5 5 Manual Sample Processing To process samples manually select operating parameters and commands from the panel tabset Commands are executed as soon as they are entered 1 Load and inject the sample using a syringe see Section 5 3 1 vacuum syringe
151. e 2 43 for automated control or the heater can be controlled manually from the DC Control panel see Figure 2 42 Program Wizard DC Options Ea r Column M Us e On Temperature 35 00 i000 80 00 V Wait Ready Off Compartment M Use G On a Temperature 35 00 1000 40 00 MF Wait Ready Off m Reaction Coil Heater M Use A On Temperature 35 00 15 00 80 00 FR wait Ready C or lt Back Next gt Cancel Figure 2 43 Program Wizard DC Options Page Doc 065031 04 1 08 2 DC Description 2 18 I O Option When the I O option P N 062201 is installed two 12 pin connector strips are on the DC rear panel Figure 2 44 describes the functions assigned to each connector pin Connector Position Pin Function Description 1 O Analog 2 lol mas Det 1 H 16 bit analog output from detector 1 3 IO Analog 4 O Det 2 16 bit analog output from detector 2 5 O 5V 5 V 200 mA 6 lol Gnd Ground 7 LO N O H Relay contacts output 8 ILOJI COM Rly 1 Connect for either normally open N O 9 IOl INC or normally closed N C 10 LO N O L Solid state relay contacts output 11 O COM Rly 2 Connect for either normally open N O 12 O INC or normally closed N C Note Relays are capable of switc
152. e Control panel e Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the DP SP door to access the mechanical components Doc 065031 04 1 08 265 ICS 3000 lon Chromatography System 4 5 Use the handles on the component mounting panel to pull the panel forward until it reaches the stop NOTE On newer pumps three red Phillips screws are installed on the component mounting panel before shipment from the factory If the mounting panel does not move freely make sure these screws have been removed To prevent contamination of pump parts wear cleanroom gloves while disassembling the pump head Never disassemble the pump head with bare hands Even minute IMPORTANT particles of dust dirt etc on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance 6 Disconnect all tubing connections to the pump head with the defective piston seal Using a 3 0 mm hex key P N 062338 loosen the two screws on the pump head with the defective seal Remove the screws and then carefully remove the head and place it on a clean surface Refer to Figure 9 4 or Figure 9 5 when disassembling and reassembling the primary pump head or secondary pump head respectively Remove the seal wash body P N 062064 from the pump head Or if the seal wash body was not removed with the pump head in Step 7 pull it straight out of the pump mechanism
153. e Figure 9 24 and remove the ring Figure 9 24 Unscrew the Locking Ring 5 Grasp the front of the valve pod and pull out firmly to remove it from the DC or AM 6 Align the slots in the new pod with the runner in the valve holder on the DC or AM see Figure 9 25 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 Doc 065031 04 1 08 303 ICS 3000 lon Chromatography System 7 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 9 25 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Splines Figure 9 25 High Pressure Valve Pod and Pod Holder 8 Push the Pod into the holder until it clicks into place Replace the black locking ring 9 Reconnect all liquid lines to the valve 10 Turn on the pump flow Check for leaks from the valve Tighten fittings as required see Section 9 17 11 Close the door 304 Doc 065031 04 1 08 9 e DC Service 9 21 Installing or Replacing an I O Option Board 1 Press the POWER button on the front of the DC to turn off the power 2 Turn off the main power switch on the DC rear panel see Figure 2 15 3 Disconnect the main power cord from both its source and from the DC rear panel HIGH VOLTAGE Disconnect the main power cord from its
154. e TC lights red and remains red as long as the sensor is exposed to gases or humidity The error is logged in the Chromeleon or Chromeleon Xpress Audit Trail A beep sounds What to do when an alarm occurs 1 2 3 Find and eliminate the leak On the TC Control panel click the Clear Alarm button Ventilate the interior of the TC thoroughly before closing the door and resuming operation Adjusting the Sensor Sensitivity Follow these steps to change the sensitivity setting of the gas or humidity sensor or to turn off a sensor 1 In the Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to display the items underneath Under TC_Temp select the GasLeakSensor or HumidityLeakSensor command Select the new sensitivity setting and click Execute To disable the sensor select Off and click Execute 102 Doc 065031 04 1 08 TC Description 2 25 Theory of Operation The fundamental requirement for a thermal compartment intended for chromatography applications is the ability to maintain the preset temperature as precisely as possible The TC contains advanced electronic circuitry that maintains the selected temperature with a precision of 0 1 C The TC can be heated from 5 to 85 C in 0 1 C increments An increase in temperature from 20 to 50 C or a decrease from 50 to 20 C is typically realized in less than 20 minutes Columns can be warmed up to 85 C If
155. e connector onto the EGC 1 or EGC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 5 Refer to Figure 9 19 to plumb the four ports on the new CR TC 292 Doc 065031 04 1 08 9 EG Service Connect to EGC OUTLET Port Connect to Suppressor REGEN OUT Port Preplumbed to RFIC Eluent Degasser REGEN IN Port Preplumbed to RFIC Eluent Degasser ELUENT IN Port TO CR TC REGEN OUT blue label Ps Figure 9 19 CR TC Plumbing Diagram Installation Completed 6 Check that no liquid lines are caught under the CR TC Align the two mounting holes on the CR TC back plate with the ball studs on the mounting plate and then push the CR TC firmly onto the mounting ball studs The CR TC clicks into place when properly installed 7 Connect the CR TC electrical cable to the CR TC 1 or CR TC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 8 Push the tray into the module until it locks into place Close the EG door 9 Turn on the power and resume operation Doc 065031 04 1 08 293 ICS 3000 lon Chromatography System 9 14 Replacing the RFIC Eluent Degasser The RFIC Eluent Degasser contains a tubing assembly that may rupture if subjected to excessive pressure 1 2 3 Press the POWER button on the front of the EG to turn off the power Open the front door of the EG Push down on the
156. e eluent lines Hand tighten the caps NOTE A Dionex High Pressure Inline Filter P N 044105 can be used to remove particulates down to 0 45 micron from eluent Connect the inline filter between the pump outlet and the eluent inlet port on the injection valve For details see the instructions provided with the inline filter Doc 065031 04 1 08 123 ICS 3000 lon Chromatography System 4 5 Set Up the Piston Seal Wash System Replumbing the Seal Wash System DP only Optional The standard piston seal wash system is designed for use with only one of the two pumps in a DP module When the DP is shipped from Dionex the seal wash system is connected to pump 1 the bottom pump If you want to connect the seal wash system to pump 2 the top pump follow the instructions in this section NOTE Dionex offers an External Seal Wash Kit P N 063518 for users who need to operate a piston seal wash system for both pumps in the DP Installation instructions are provided in the kit Note the tubing connected from the peristaltic pump to the seal wash tube on the secondary pump head on pump 1 see Figure 4 1 Disconnect this tubing from the pump head and connect it to the seal wash tube on the secondary pump head on pump 2 Disconnect the seal wash reservoir inlet line from the primary pump head on pump 1 see Figure 4 1 Connect the inlet line to the primary pump head on pump 2 Disconnect the short piece of tubing between the prima
157. e lines are not elevated at any point after they exit the EG EluGen cartridge leaks Replace the EluGen cartridge see Section 9 12 RFIC Eluent Degasser leaks Replace the RFIC Eluent Degasser see Section 9 14 Doc 065031 04 1 08 207 ICS 3000 lon Chromatography System EluGen cartridge electrical connection is open 1 Tug gently on the EluGen cartridge electrical cable the locking connector should hold the cable in place see Figure 2 8 2 Ifthe electrical cable is fully seated but the problem persists the cartridge is defective and must be replaced see Section 9 12 EluGen cartridge input electrical connection has shorted out Replace the EluGen cartridge see Section 9 12 Electrical error The EG current and or voltage may have become unstable Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user 8 21 EG POWER LED Fails to Light No power Check that the POWER button on the front of the EG is turned on Check that the EG main power switch on the rear panel is turned on Check that the main power cord is plugged into both the EG rear panel connector and the power source Check that the wall outlet has power If the POWER LED still fails to light contact Dionex for assistance 8 22 Liquid Leaks in the EG Leaking fitting Locate the source of the leak Tighten or replace liquid line connections as needed see Section 9 1
158. e piston should extend from the head Place the pump head back on the pump Reinstall the screws in the pump head Using the 3 0 mm hex key P N 062338 tighten the screws just until they come into contact 270 Doc 065031 04 1 08 9 DP SP Service with the pump head Then tighten the screws another one quarter to one half turn one eighth of a turn at a time Reconnect all tubing connections to the pump head Tighten connections fingertight and then tighten an additional one quarter turn only Push the component mounting panel back into the enclosure Close the DP SP door Press the POWER button on the front of the DP SP to turn on the pump Select the Connected check box on the Control panel to reconnect the pump to the software Click Motor on the Control panel to turn on the pump flow 9 6 Replacing the Piston If a new piston seal leaks assuming that the pump head is tight it indicates that the piston is dirty scratched or broken and should be replaced The piston replacement procedure consists of e Removing the pump head and the old piston see Section 9 6 1 e Installing a new piston see Section 9 6 2 e Reinstalling the pump head see Section 9 6 3 9 6 1 Removing the Pump Head and Piston Refer to Figure 9 4 or Figure 9 5 when disassembling and reassembling the primary pump head or secondary pump head respectively 1 Click Motor on the pump Control panel in Chromeleon or Chromel
159. e table TC Related Audit Trail Error Message Default Severity See Level AcqOff without previous AcqOn Error page 227 Acquisition is still on at program end Error page 227 All samples scheduled for run on timebases x need to Error page 228 specify the same value for property nominal Temperature All samples scheduled for run on timebases x need to Error page 228 specify the same value for property TempCtrl All samples scheduled for run on timebases x need to Error page 228 specify the same value for property y Can t execute Disconnect command during data Warning page 228 acquisition Can t execute Standby command during data Warning page 228 acquisition Can t find download image TC3000 HEX Abort page 229 Can t start acquisition at negative retention times Error page 229 Can t start acquisition The server configuration does not Abort page 229 fulfill the license conditions Can t start TC firmware A firmware download may be Abort page 230 necessary Can t use device x as a source of the column pressure Error page 231 Please check the property SystemPressure for a valid device name The device must have the Pressure property available Doc 065031 04 1 08 173 ICS 3000 lon Chromatography System TC Related Audit Trail Error Message Defaul
160. ead Figure 9 1 DP SP Priming Valve 6 Gradient pump only a Ifall eluent lines have not been primed select another eluent channel and repeat the priming procedure b After priming all eluent lines press PUMP PRIME 1 or PUMP PRIME 2 to stop priming and return to the flow rate last selected 7 Close the priming valve by turning it clockwise Do not overtighten the priming valve Do not use any tools to tighten the priming valve Overtightening may IMPORTANT destroy the cap seal Open or close the priming valve only when the system pressure is down 8 Click the Connected check box on the Control panel to reconnect the pump to Chromeleon or Chromeleon Xpress 260 Doc 065031 04 1 08 9 DP SP Service 9 3 2 Priming from the Control Panel 1 Gradient pump only Set the channel to be primed A B C or D to 100 on the pump Control panel in Chromeleon or Chromeleon Xpress Under Prime Control on the Control panel a Set the Duration to 300 sec b Set the Prime Rate to 6 0 mL min Open the priming valve on the secondary pump head see Figure 9 1 by turning it one half turn counterclockwise NOTE If the priming valve is opened too much air is drawn through the valve and air bubbles can be seen exiting the waste line To enable priming click the Prime button on the Control panel Continue priming the pump until all air and previous eluents are purged and no air bubbles can be seen
161. eak 2 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Failure of a mechanical component Ifa VALVE LED is flashing a mechanical component in the TC injection valve has failed Replace the injection valve pod see Section 9 28 and then click the Clear Alarm button on the TC Control panel If the OVEN LED is flashing a mechanical component in the TC has failed These parts are not user serviceable Contact Dionex for assistance 8 31 Liquid Leaks from TC Components e Leaking fitting Locate the source of the leak Tighten or if necessary replace the liquid line connection see Section 9 25 e Broken liquid line Replace the line with tubing of the same length and internal diameter see Section 9 25 Doc 065031 04 1 08 253 ICS 3000 lon Chromatography System Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked Also make sure the waste line is not elevated at any point after it exits the TC If a line is blocked replace it see Section 9 25 Leaking injection valve 1 Make sure the liquid line connections to the valve are tight Replace any damaged fittings see Section 9 25 2 Liquid leaks from behind the valve stator may indicate a scratched rotor seal Rebuild the injection valve see Section 9 27 Leaking temperature stabilizer 1 Tighten the
162. ears dirty or if there is a slimy film on the interior follow the cleaning instructions in Section 9 2 2 Flush the system with ASTM Type I 18 megohm cm filtered and deionized water 3 Replace all end line filters P N 045987 See Section 4 4 for instructions 4 Prepare new stock solution 5 Prepare fresh eluent To ensure eluent purity prepare all eluents with spectro grade eluents reagent grade chemicals and ASTM Type I 18 megohm cm filtered and deionized water DP SP not properly primed Prime the pump see Section 9 3 Piston seal is damaged If the piston seal is damaged it allows liquid leaks Leaks are usually visible and thus easily detected If necessary replace the piston seal see Section 9 5 Inadequate system or cell backpressure Add backpressure tubing to the cell outlet see Section 9 23 4 or to the pump if no column is installed EG Only System backpressure is below 14 MPa 2000 psi When the EG is installed the optimal system backpressure is 16 MPa 2300 psi Low system backpressure may cause high baseline noise as the eluent concentration increases in the gradient To correct this install a backpressure coil in the EG after the RFIC Eluent Degasser see Section 9 15 Flow system leak ahead of cell Check all fittings and liquid lines for leaks Tighten or if necessary replace all liquid line connections see Section 9 17 178 Doc 065031 04 1 08 8 Troubleshooting
163. ectrode disconnected This error occurs when the cable on the working electrode is disconnected from the cell electronics To troubleshoot Check the cable connection Verify that the signal cable from the working electrode is connected to the detector block see Figure 8 4 216 Doc 065031 04 1 08 8 DC Troubleshooting High pressure valve 1 error or High pressure valve 2 error or High pressure valve 3 error or High pressure valve 4 error This error occurs if a high pressure valve fails to switch position within 1 second of being toggled The high pressure valves are the 6 or 10 port valves installed in either the DC lower see Figure 8 5 or upper compartment see Figure 8 6 High Pressure Valve 2 High Pressure Valve 1 High Pressure High Pressure Valve 3 Valve 4 Figure 8 6 High Pressure Valves 3 and 4 Doc 065031 04 1 08 217 ICS 3000 lon Chromatography System To troubleshoot 1 If a sequence is being executed terminate the sequence by selecting Stop on the Chromeleon or Chromeleon Xpress Control panel Turn off the ICS 3000 Ion Chromatography System power briefly by pressing the POWER button on the front of each module Then press each button again to restart the system Try to toggle the valve from Load to Inject by pressing the Load and Inject buttons on the front of the DC If the problem persists contact Dionex for assistance L
164. ectrolysis gas H or O2 that is vented from the electrolyte reservoir of the EluGen cartridge e The lines exiting the tubing chase white tubing are for connecting the REGEN IN port on the CR TC or EPM Electrolytic pH Modifier to the REGEN OUT port on the suppressor e The drip tray drain port removes any liquid that collects in the drip tray in the bottom of the EG A clear corrugated tubing line is connected to this port during installation 38 Doc 065031 04 1 08 2 EG Description 2 10 Place the free ends of the vent and drain lines into a waste container To maintain a positive siphon position the waste container below the level of the EG NOTE To ensure proper drainage each waste line must remain above the liquid level in the waste container EG Flow Schematic Figure 2 10 illustrates the liquid flow path through the EG Deionized water is delivered by the DP SP to the EluGen cartridge DC current is applied to the cartridge to produce eluent The electrolytically generated eluent flows through the Continuously Regenerated Trap Column CR TC into the RFIC Eluent Degasser through the backpressure coil if installed through the injection valve to the separator column and finally to the detector cell The detector cell effluent is directed through the Atlas or SRS suppressor regenerant chamber to the CR TC regenerant chamber through the RFIC Eluent Degasser inside the EG and finally to waste NOTE Ref
165. ed To troubleshoot 1 Refill the reservoir with wash solution if necessary ASTM Type I 18 megohm cm filtered and deionized water is usually appropriate Verify that the tubing is engaged in the peristaltic pump see Section 4 5 The tubing should not be plugged or crimped Replace the tubing as needed see Section 9 1 Clean the sensor on the reservoir with water or solvent Check for leaks at connections throughout the pump module tighten or replace any leaking fittings Replace any tubing that is plugged or damaged Doc 065031 04 1 08 193 ICS 3000 lon Chromatography System Relay 4 is configured for inject synchronization Please change pump configuration This error occurs if you attempt to use relay 4 as a standard relay in a Chromeleon or Chromeleon Xpress program although the relay has been set to synchronize the gradient with the autosampler sample injection To troubleshoot Define the relay as a standard relay or specify a different relay for use in the program The maximum purge pressure was exceeded Ifthe DP SP pressure exceeds 5 MPa 725 psi during priming this error occurs and the priming process is aborted To troubleshoot 1 Verify that the priming valve is open and then reprime the pump To open the valve turn the knob one half turn counterclockwise 2 Check fittings for overtightening Check tubing for crimping and replace it as necessary Be careful not to overtighten f
166. ed To troubleshoot 1 Connect the EluGen cartridge cable connection to the electrical bulkhead see Figure 2 8 2 Ifthe error message appears again contact Dionex for assistance The EluGen cartridge control electronics may have malfunctioned NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user EG1 invalid concentration Or EG2 invalid concentration This error occurs if the eluent concentration is outside 0 10 to 100 mM the range allowed by the EG This may indicate corrupted memory or a problem in the EG Moduleware the instrument control firmware installed in the EG To troubleshoot Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components and Moduleware cannot be serviced by the user 204 Doc 065031 04 1 08 8 EG Troubleshooting EG invalid flow Or Ee invalid flow This error occurs if the flow rate is set to a value the EG does not support The DP SP flow rate range is 0 001 to 10 0 mL min however when an EG is installed the allowed range is 0 01 to 3 00 mL min The recommended operating range is 0 4 to 2 00 mL min To troubleshoot Set the flow rate to a value within the allowed range EG1 invalid flow rate concentration Of EG2 invalid flow rate concentration This error occurs if the selected concentration is too high for the current flow rate To troubleshoot Set the flo
167. ed as the topmost module in the system the TC VWD PDA Regulator Bracket Kit P N 064792 is required The kit includes the EO Regulator Kit described above as well as a right angle regulator bracket and mounting hardware After attaching the bracket to the TC or detector you will mount the gas regulator assembly on the bracket If more reservoirs are required order a second regulator P N 062345 30 Doc 065031 04 1 08 EG Description 2 7 EG Front Features The status bar on the front of the ICS 3000 Eluent Generator EG includes buttons that provide control of certain EG functions as well as LEDs that indicate the status of several EG functions see Figure 2 7 e CONNECTED ALARM Figure 2 7 EG Status Bar Button LED If the LED Is On Comment Label CONNECTED The EG is connected to a Chromeleon or Chromeleon Xpress timebase ALARM An EG related problem has occurred Check the Chromeleon or for example the EluGen cartridge Chromeleon Xpress Audit was disconnected Trail for the cause EGC 1 The EluGen cartridge is on and is EGC 1 is always installed in EGC 2 generating eluent the left section of the component compartment EGC 2 if present is installed in the right section of the compartment CR TC 1 The CR TC is on CR TC 1 is always installed in CR TC 2 the left section of the component compartment CR TC 2 if present is installed in the right section of the compa
168. ed on the Dionex Reference Library CD ROM P N 053891 which is included in the ship kit of each ICS 3000 system module In addition the software manuals are provided as PDF files on the Chromeleon or Chromeleon Xpress CD ROM A printed copy of the software installation instructions is provided in the software ship kit Consumables documentation For complete information about Dionex columns suppressors EluGen cartridges etc refer to the appropriate product manual These manuals are provided on the Reference Library CD ROM 10 Doc 065031 04 1 08 1 Introduction 1 3 The ICS 3000 System Operator s Manual 1 3 1 Overview The electronic version i e PDF file of the ICS 3000 system 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 Chapter 1 Introduction Chapter 2 Description Chapter 3 System Configurations Chapter 4 Getting Started Chapter 5 Operation Chapter 6 Shutdown Chapter 7 Maintenance An overview of the ICS 3000 system includes a brief description of the ICS 3000 modules the software required for ICS 3000 operation and the ICS 3000 user manua
169. elf diagnostics in which the status of the main components is checked This error occurs if a component is not ready for operation To troubleshoot 1 Inthe Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to display the items underneath 2 Check the status of each command listed in the error message The table below indicates the status required for operation Command Status CardState OK Door Closed Ready Ready Standby NoStandby 3 When you identify the component that is not ready for operation find and eliminate the cause of the problem The primary column ID property x will be changed The property can t be changed in the future This error occurs when you modify a primary column property batch or lot number date of manufacture etc To prevent any unintended changes Chromeleon or Chromeleon Xpress requests confirmation before saving the new property To troubleshoot If you are sure that the proposed change is correct go ahead and save it 248 Doc 065031 04 1 08 TC Troubleshooting A The upper limit must be higher than the lower limit This error occurs if the value entered for a parameter s upper limit for example TC_Temp Signal UpperLimit is less than the lower limit for the parameter To troubleshoot Increase the value of the upper limit setting A The Warning threshold must be higher than the Limit threshold This error occurs if the Wa
170. eluent composition can be delivered as isocratic isocratic proportioned linear ramp step curved or any combination of these With a DP the second pump can be operated as a second channel chromatography pump an auxiliary dependent pump or an auxiliary independent pump ICS 3000 Detector Chromatography Module DC The DC provides a temperature controlled environment for ICS 3000 chromatography components The DC can accommodate components for two channels plumbed either serially or in parallel The following components may be installed in the DC e Conductivity detector e Electrochemical detector e Injection valves e Switching valves e Guard and separator columns e Suppressors e ICS 3000 Automation Manager Doc 065031 04 1 08 ICS 3000 lon Chromatography System ICS 3000 Conductivity Detector CD The CD is a modular detector with integrated cell providing dual detection capabilities series or parallel The CD has a signal range up to 15 000 uS and supports high background nonsuppressed applications The CD is installed in the upper compartment of the DC ICS 3000 Electrochemical Detector ED The ED is a modular detector and cell with dual detection capabilities series or parallel The ED supports multiple waveforms multiple integration times and post analysis data manipulation The ED is also capable of providing 3D amperometry data The ED cell can be configured with gold silver platinum or glassy
171. en Cartridge EGC II NaOH EluGen Cartridge CR ATC Anion Continuously Regenerated Trap Column CR CTC Cation Continuously Regenerated Trap Column EPM Electrolytic pH Modifier EGC CO3 Mixer Backpressure Coils Backpressure coil 2 0 mL min 500 psi 4 mm Backpressure coil 2 0 mL min 1000 psi 4 mm Backpressure coil 0 5 mL min 500 psi 2 mm Backpressure coil 0 5 mL min 1000 psi 2 mm Miscellaneous RFIC Eluent Degasser Fuse IEC 60127 2 slow blow rated at 2A 250V USB cable 1 m 3 ft long Ferrule fitting 10 32 double cone Fitting bolt 10 32 for double cone ferrule fitting Mini screwdriver Doc 065031 04 1 08 351 ICS 3000 lon Chromatography System 352 Doc 065031 04 1 08 H om Part Number 061961 061962 061971 061745 042949 042857 044105 024305 016388 057896 061759 061718 061756 061879 014067 061749 061751 061753 061755 063722 060082 060140 060139 060216 DC Reordering Information Item Valves and Accessories High pressure injection or switching valve 6 port High pressure injection or switching valve 10 port Low pressure valve 3 way Low pressure valve 2 way Sample loop 10 uL Sample loop 25 uL Filter high pressure inline for sample filtering Luer adapter fitting 1 4 28 for manual injections Syringe cc for manual injections Valve rebuild kit 6 port Valve rebuild kit 10 port Electrochemical Detector and Accessories ICS 3000 Electroc
172. ent Maximum temperature 70 C above ambient For example if the ambient air temperature in the lab is 30 C and you set the temperature to 5 C the actual temperature achieved will be about 12 C Doc 065031 04 1 08 103 ICS 3000 lon Chromatography System CAUTION MISE EN GARDE VORSICHT 2 25 1 Do not touch any metal parts inside the TC while it is heating up or after it reaches the set point temperature Wait for the compartment to cool down before servicing any parts Ne touchez aucune des pi ces m talliques l int rieur du TC pendant qu il chauffe ou apr s qu il ait atteint la temp rature de consigne Attendez que le compartiment soit refroidi avant de r parer les pi ces Ber hren Sie im TC keine metallischen Teile w hrend dieses aufgeheizt wird oder nachdem die Solltemperatur erreicht ist Warten Sie bis die Kammer abgek hit ist ehe Sie Wartungsarbeiten durchf hren Predictive Performance The Predictive Performance feature of the TC provides various functions for estimating the lifetime of replaceable parts and for planning and recording service and qualification procedures A partial list of the TC Predictive Performance functions is provided below Refer to the Chromeleon or Chromeleon Xpress Help for details Monitoring of the total cooling and heating workload performed by the compartment and the total operating hours since initial operation Monitoring of the injecti
173. ential Volts 0 10 gt 0 60 Integration i 0 0 0 2 0 4 0 6 0 8 z Time Seconds El E2 Analytical Potentials E3 Cleaning Potential E1 E2 E3 E4 E4 Reconditioning Potential Figure 2 25 Example Integrated Amperometry Waveform With the example waveform shown in Figure 2 25 the current is integrated both while the potential is swept across the metal oxide formation wave and also during the reverse sweep across the oxide reduction wave This technique minimizes baseline shift and the peak dips that can occur when an eluting analyte s effect on oxide suppression is greater than the detector response from the analyte As with pulsed amperometric detection the waveform period repeats until the end of data acquisition or until another waveform is specified 62 Doc 065031 04 1 08 2 DC Description 2 16 5 2 16 6 Cyclic Voltammetry Detection The determination of the optimum potentials to use in amperometry begins with an electrochemical technique called voltammetry in which the current that results from oxidation or reduction reactions is measured against the voltage applied to the system The applied voltage is changed scanned within preset limits In cyclic voltammetry the voltage is first scanned in one direction and then reversed so that the voltage at the end of the scan is the same as at the beginning This results in a triangular waveform see Section 2 16 6 In the c
174. eon Xpress to turn off the pump flow Begin monitoring the Current Pressure reading on the Control panel When the system pressure reaches zero do the following e Disconnect the pump from the software by clearing the Connected check box on the Control panel Doc 065031 04 1 08 271 ICS 3000 lon Chromatography System important e Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump Open the DP SP door to access the mechanical components Use the handles on the component mounting panel to pull the panel forward until it reaches the stop NOTE On newer pumps three red Phillips screws are installed on the component mounting panel before shipment from the factory If the mounting panel does not move freely make sure these screws have been removed To prevent contamination of pump parts wear cleanroom gloves while disassembling the pump head Never disassemble the pump head with bare hands Even minute particles of dust dirt etc on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance 6 Disconnect all tubing connections to the pump head with the damaged piston Using a 3 0 mm hex key P N 062338 loosen the Allen screws on the pump head with the damaged piston Remove the Allen screws and then carefully remove the head and place it on a clean surface If the piston was not removed with the pump head in Step 7 remove
175. er to the EGC CO Mixer manual for a flow schematic showing the components required to generate a carbonate bicarbonate mixture The manual is included on the Dionex Reference Library CD ROM P N 053891 Doc 065031 04 1 08 39 ICS 3000 lon Chromatography System EGC VENT H LGG RFIC Eluent Degasser J Regen Regen To Waste Inlet Outlet EGC IN EGC OUT From pump Regen Out Port blue label CR TC To injection valve port P lt To gas separator waste tube Eluent In Port red label L Regen In Port orange label From suppressor REGEN OUT p Figure 2 10 EG Flow Schematic Example Doc 065031 04 1 08 DC Description 2 11 DC Front Features A status bar on the front of the ICS 3000 Detector Chromatography Module DC see Figure 2 12 includes buttons for controlling certain DC functions as well as LEDs that indicate the status of several DC components and functions e e CONNECTED ALARM 2 UPPER LOWER LOAD INJECT OM Qi ee SUPPRESSOR OVEN VALVE 1 VALVE 2 LOAD INJECT Figure 2 11 DC Status Bar Button LED Label If the LED Is On If the LED Is Flashing valve or suppressor error Check the Chromeleon or Chromeleon Xpress Audit Trail for the cause CONNECTED The DC is connected to a Does not flash Chromeleon or Chromeleon Xpress timebase
176. essure command 3 Enter the name of the pump currently delivering flow for this column and click Execute A Card data checksum error This error indicates that the column ID chip card memory is corrupted To troubleshoot Replace the column ID chip card see Section 9 26 Doc 065031 04 1 08 231 ICS 3000 lon Chromatography System Command is not available in demo mode This error occurs if you attempt to issue a command that is not available when the TC is in demo or virtual mode To troubleshoot Ifa TC is present and connected disable the demo mode 1 Start the Server Configuration program 2 Inthe timebase right click the TC and select Properties on the context menu 3 On the General tab page in the Properties dialog box clear the Demo Mode check box and click OK Communication error x This error occurs if there is a communication failure between the TC and the PC on which Chromeleon or Chromeleon Xpress is installed To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 If you cannot identify the cause of the error contact Dionex for assistance Communication time out This error occurs if a TC firmware Moduleware command is not executed within the time allotted for its completion To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 Ifyou cannot identify the cause of the er
177. eters to detach it from the mounting tabs on the detector Then pull the suppressor toward you Orient the new suppressor with the ELUENT IN fitting on the bottom see Figure 9 30 Press the suppressor against the back of the detector and then slide it to the right to secure it onto the mounting tabs Pull out slightly on the center of the suppressor to verify that it is securely fastened Connect the two eluent and the two regenerant lines to the new suppressor Plug in the cable Close the DC door Turn on the DC power and restart the pump flow 310 Doc 065031 04 1 08 9 e DC Service 9 23 3 Replacing a CD 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump Press the POWER button on the front of the DC to turn off the DC Open the DC upper door and disconnect the tubing from the conductivity detector CELL IN and CELL OUT fittings see Figure 9 31 Disconnect Figure 9 31 Disconnecting the Conductivity Detector Liquid Lines 4 5 Remove the suppressor from the detector see Section 9 23 2 Press the release lever located below the detector The detector pops out slightly from the DC compartment Grasp the top of the detector and pull outward to remove the detector from the compartment Do not pull from the CELL IN and CELL OUT fittings Note the electrical plug on the back of the detector and the receptacle
178. f valve Variable Wavelength Detector 2 7 Regulator Bracket Kit 30 Vials 118 120 Filling 118 120 Virtual Column Separation Simulator 149 Voltammetry 63 See also Cyclic voltammetry W Waste container EG Preventing gas buildup 114 Waste disposal 167 Waste lines CD Gas separator waste tube 36 55 Waste lines DC Blocked 221 Waste lines DP SP 28 Waste lines EG 36 38 Blocked or incorrectly installed 207 208 Waste lines TC Blocked 254 Water dip 120 Water samples 119 Waveform Editor 66 Waveforms 63 Cyclic voltammetry 63 Defining 66 Integrated amperometry 64 Integrated amperometry example 62 Maximum length 65 Pre programmed 65 Pulsed amperometry example 61 Weekly maintenance DC 165 DP SP 161 EG 163 TC 167 Weight DC 341 DP SP 335 EG 339 TC 347 Wellness 104 Wireframe plot 70 Working electrodes 57 Maintenance 115 Materials 57 Polishing 317 Z Zero position analog out 82 Index 18 Doc 065031 04 1 08
179. fittings on the temperature stabilizer inlet and outlet 2 If tightening the fittings does not eliminate the leak excessive system backpressure may be the source of the problem Follow the troubleshooting steps in Section 8 9 to reduce the backpressure 8 32 TC Temperature Does Not Increase If the temperature fails to increase as expected although the temperature set point has not been reached follow the troubleshooting steps below Front door not closed Verify that the TC door is fully closed If it is check the door seal for signs of damage If the seal is damaged contact Dionex for assistance Column tubing connections incorrectly oriented Column tubing connections that are incorrectly oriented can open a small path for ambient air into the TC Check that the tubing connections are at a 90 degree angle in relation to the door seal Ventilation slots on TC are obstructed Make sure the ventilation slots are not obstructed in any way Allow at least 6 cm 2 4 in behind the TC for ventilation Ambient temperature is too high Reduce the ambient temperature for example ventilate the lab in which the TC is installed 254 Doc 065031 04 1 08 TC Troubleshooting 8 33 TC Temperature Stabilizer Not Operating Properly e Temperature stabilizer installed incorrectly Remove the temperature stabilizer and reinstall it correctly Make sure there is good thermal contact between the temperature stabilizer and the the
180. for the ICS 3000 Dual Pump DP or ICS 3000 Single Pump SP that users may perform All other maintenance procedures must be performed by Dionex personnel 7 2 DP SP Daily Maintenance e Check for leaks at the following locations the eluent proportioning valves gradient pump only vacuum degas chambers and eluent reservoirs Tighten or replace any leaking fittings e Wipe up liquid spills and rinse dried reagents off pump components with deionized water Dry the leak sensor thoroughly if the sensor is not dry it will remain activated and continue to report a leak to the Audit Trail e Check the liquid level in each eluent reservoir and refill as required e Check the liquid level in the seal wash reservoir The liquid level should remain between the Min and Max markers on the reservoir label e Rinse each eluent reservoir thoroughly inside and out with ASTM filtered Type I 18 megohm cm deionized water and dry with clean particulate free air If a reservoir still appears dirty or if there is a slimy film on the interior clean the reservoir as instructed in Section 9 2 7 3 DP SP Weekly Maintenance e The end line filters P N 045987 on the eluent lines may need to be replaced weekly depending on water quality and eluent conditions For example replace the filters weekly when using an EluGen cartridge to generate carbonate bicarbonate eluent When the end line filters are new they are pure white Replace the filters
181. fthe program and quantification method have already been created use the Sequence Wizard e Ifyou want to create a new program and quantification method in addition to the sequence use the Application Wizard Using the Sequence Wizard 1 Click Create Sequence on the Sequence Control panel see Figure 5 7 ICS 3000_2 gt k Home Sequence Control Status Gradient Pump Detector Compart Cond Detector 1 System Log Audit Trail 2 55 11 PM 0 000 CD_1 AcqOn 2 55 11 PM 0 000 CD_1_TotalAcqOn H Pump_1_Pressure 60 2 55 41 PM 0 500 Pump_1 Log Pressure 0 0 psi CD_1_Total 02 55 41 PM 0 500 CDet1 Log Background 0 0 uS CD 1 3 06 11 PM 10 987 System AcqOft E 306 11 PM The sample state was Single and has been setto Finished Preparing a new sample for the next time v Vs Run Time Elapsed an ols wy wey 1 Create Application 2 Prepare System 3 Execute Application System Maintenance Create Program Application Wizard Hold Continue Daily Audit Trail Create Sequence Acq On Acq Off Start Batch Consumable Change Edit Program Load Sequence Abort Batch Eluent Change Sequence No Po Inj Vol Program Status Inj Date Time Sequence Finishe 2 28 2005 2 23 2 Unknow ICS 3000 2 test Finishe 2 28 2005 2 53 3 Unknow ICS 3000 2 test Finishe 2 28 2005 3 23 5 Unknow ICS 3000 2 test Figure 5 7 Sequence Control Panel 2 Complete the steps in the Sequence Wi
182. glich ist VORSICHT USB Connections The USB Universal Serial Bus receptacle B type connector allows connection to the PC on which Chromeleon or Chromeleon Xpress software is installed The two USB ports A type connectors allow connection to other USB devices in the system for example the pump and eluent generator A 1 8 m 6 ft USB cable P N 960777 is included in the DC Ship Kit P N 062614 dual P N 063408 single 48 Doc 065031 04 1 08 2 DC Description External Low Pressure Valve Outputs Six outputs allow connection to externally installed low pressure solenoid valves Low pressure valves can be used for on off control of liquid flow for example to turn flow on and off from a reagent reservoir You control the outputs with Chromeleon or Chromeleon Xpress Two low pressure valves can be installed on a regulator stand and four valves can be installed on the rear of the DC Analog Output TTL and Relay Connectors Optional If the I O option P N 062201 is installed the following connections are provided e Two analog outputs one for each detector e One 5V power output e Two relay outputs e Two TTL outputs e Eight programmable TTL inputs See Section 2 18 for details about the I O option Doc 065031 04 1 08 49 ICS 3000 lon Chromatography System 2 14 Injection Valves One or two injection valves can be installed in the lower compartment of the DC The fo
183. gram Use the TC Control panel or the Commands dialog box in Chromeleon or Chromeleon Xpress to select column properties see below for storage and to review the stored information at any time Information on the column ID chip card is continuously updated as long as the column and the chip card are installed in the TC Column Properties Two types of information can be stored on the column ID chip card e Primary column properties are entered once by the column manufacturer or the user and are never changed during the lifetime of the column The primary properties are the product ID serial number batch lot number date of manufacture and custom information e Secondary column properties are entered by the user and can be changed whenever required by any Chromeleon or Chromeleon Xpress user with Expert privileges Secondary properties include the column manufacturer diameter length particle size maximum number of injections pH limits and upper pressure limit For a complete list of secondary properties refer to the Chromeleon or Chromeleon Xpress Help Doc 065031 04 1 08 101 ICS 3000 lon Chromatography System 2 24 Gas and Humidity Sensors The TC contains two sensors to detect any gas or humidity that may accumulate inside the TC When a certain concentration of gas or humidity is reached while the door is closed the following events occur The corresponding sensor is activated The ALARM LED on the front of th
184. hanical parts Pod 331 Specifications 348 Types available 93 Integrated amperometry 61 3D data 68 Data storage 68 Integration interval 62 65 Waveform characteristics 64 Waveform example 62 Interior components DC 44 Conductivity Detector CD 44 Electrochemical Detector ED 44 Lower compartment description 45 Suppressor types 45 Upper compartment description 44 Inverted edge TTL input control DC 89 Inverted pulse TTL input control DC 89 IonPac ATC HC Trap Column 35 IonPac CTC 1 Trap Column 35 IPAD See Integrated amperometry I t plot 69 L Leak sensor EG 35 207 Leak sensors DC Lower leak sensor wet alarm 218 Replacement 298 Upper leak sensor wet alarm 221 Leak sensors TC Gas 102 238 Humidity 102 238 348 Leaks Conductivity cell 222 DC 221 EG 35 207 Gas 91 102 238 253 Humidity 91 102 238 253 Injection valve DC 222 Injection valve TC 254 Reference electrode 225 Suppressor 222 Temperature stabilizer TC 254 LED descriptions DC 41 91 LED descriptions DP SP 17 18 LED descriptions EG 31 LED descriptions TC 91 Lithium hydroxide eluent 34 Loading samples 140 Example program 144 With a syringe 141 With a vacuum syringe 143 With an autosampler 140 Loading the autosampler tray 118 120 Low detector output 186 Low pressure limit Selecting 130 Lower compartment DC Description 45 Specifications 342 348 Temperature control 46 Tem
185. hat replaces and combines the module front panels into one centralized system control panel A convenient Home panel see Figure 1 2 shows the overall system status Individual tabs provide quick access to module functions as well as detailed status and diagnostics 0000000000 0000000000 0000000000 Figure 1 2 ICS 3000 Panel Tabset Home Panel Shown Doc 065031 04 1 08 9 ICS 3000 lon Chromatography System 1 2 ICS 3000 System Documentation Every effort has been made to provide complete and accurate user documentation for the ICS 3000 system The table below lists the primary sources of product information and the formats in which information is available Source Part PDF Printed Number File Manual ICS 3000 Ion Chromatography System 065031 Yes No Operator s Manual Installing the ICS 3000 Ion Chromatography 065032 Yes Yes System AS Autosampler Operator s Manual 065051 Yes No ICS Series Photodiode Array Detector 065147 Yes No Operator s Manual ICS Series Variable Wavelength Detector 065141 Yes No Operator s Manual Chromeleon Xpress Quick Reference Guide 065070 Yes No Chromeleon Xpress online Help N A N A N A Chromeleon Software User 5 Guide 4829 5060 Yes No Installing the Chromeleon Chromatography 031883 Yes Yes Management System with a Dionex Ion Chromatograph IC Chromeleon online Help N A N A N A All Adobe PDF files listed above are shipp
186. he Control panel to turn on the pump flow Doc 065031 04 1 08 273 ICS 3000 lon Chromatography System 9 7 Replacing the Piston Seal Wash Tubing Check the piston seal wash tubing weekly for crimping or blockage and replace as needed 1 Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow 2 Open the DP SP door to access the mechanical components 3 Remove the old tubing from the peristaltic pump see Figure 9 7 as follows a Lift the lever up and to the right and hold it in that position with one hand b With your other hand pull the PharMed tubing away from the rotor and out of the lower notch on the left side of the mounting plate c Release the lever d Pull on the fitting slightly to remove the PharMed tubing from the upper notch on the pump mounting plate Tygon 2075 Tubing PharMed Tubing P N 063268 Rotor Lever Fitting Mounting Plate P N 064079 Figure 9 7 Peristaltic Pump for Seal Wash System Pull off the PharMed and Tygon 2075 tubing from the fitting Save the fitting Pull off all seal wash tubing from the seal wash reservoir and the primary and secondary pump heads Cut three new pieces of Tygon 2075 tubing 0 15 cm 0 060 in ID P N 064079 and one piece of PharMed tubing 0 159 cm 0 0625 in ID P N 063268 to the same lengths as the tubing just removed 274 Doc 065031 04 1 08 9 DP SP Service
187. he DC 1 Press the POWER button on the front of the DC 2 To display the DC Control panel select the Detector Compartment tab see Figure 4 5 ICS 3000 5 gt Home Sequence Control Status Autosampler Gradient Pumps Eluent Generator Detector Compartment Cond Detector EC Detector 3D Amp Plot Valves Detector Compartment Compartment_TC injectValve_1 LoadPosition gt ee al Connected Audit Trail Set Point 35 00 C 4 InjectValve 2 LoadPosition pe m 2 Serial Number 123456789012 Mode On AM_HP1 lt eee DC_Relay_1 Open Upper Door is Closed Temperature 35 00 C AMEN DC_Relay_2 Open 7 AM_LP1 Closed d Lower Door is Closed Status Ready DC_ACRelay_1 Open AM_LP2 Closed DC _ACRelay 2 Open x Suppressor Settings Column TC DC_LP1 Closed dAnput TTLs Type ASRS_2mm SetPoint 35 00 C DONPA Closed E ane Mode Off 7 Mode On K DC_LP3 Closed TTL Input 2 TTL_Input_3 NS DC LP4 Closed x Current 0 mA Bj Temperature TTL_Input_4 DC_LP5 Closed TTL_Input_5 Calculate Current Status Calculate Curent eiii DC_LP6 Closed ETES TTL_Input_ TTL_Input_8 Suppressor2 Settings Type None Set Point Mode Off M Mode Current 0 mA El Temperature Status Figure 4 5 DC Control Panel 3 Turn on all temperature control devices ins
188. he manual is included on the Dionex Reference Library CD ROM P N 053891 e Wrong eluent Check that you are using the correct eluent for your application For ED detectors verify that the pH readout is correct for your eluent e Background signal not offset from detector signal Before injecting sample allow the background signal to equilibrate and then press Autozero on the Control panel in Chromeleon or Chromeleon Xpress CD Only e Background not suppressed by suppressor Verify that the suppressor is turned on and the current is set to the correct value Refer to the suppressor manual for additional troubleshooting guidance Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 e Regenerant fails to suppress background Use a higher regenerant flow rate Refer to the suppressor manual for the suggested regenerant flow rate for your application Doc 065031 04 1 08 187 ICS 3000 lon Chromatography System ED Only Integrated Amperometry mode Excessive number or length of integration intervals and or incorrect potential for the integration Verify that the length and potential of the integration interval is correct refer to the column manual for the settings required for your application Column manuals are included on the Dionex Reference Library CD ROM P N 053891 DC Amperometry and Integrated Amperometry modes Amperometry cell working electrode shorted to counter electrode C
189. he other end to the TO INJ VALVE IN P line The EG Ship Kit P N 062453 includes four backpressure coils see Table 9 1 Part Number Backpressure Flow Rate Approximate Coil Description Backpressure Added 053762 4 mm ID 2 0 mL min 3 5 MPa 500 psi 1 0 mL min 1 75 MPa 250 psi 053763 4 mm ID 2 0 mL min 7 MPa 1000 psi 1 0 mL min 3 5 MPa 500 psi 053764 2 mm ID 0 50 mL min 3 5 MPa 500 psi 0 25 mL min 1 75 MPa 250 psi 053765 2 mm ID 0 50 mL min 7 MPa 1000 psi 0 25 mL min 3 5 MPa 500 psi Table 9 1 Backpressure Coils Doc 065031 04 1 08 295 ICS 3000 lon Chromatography System 9 16 Changing the EG Main Power Fuses DANGER DANGER ACHTUNG 1 4 Press the POWER button on the front of the EG for 2 seconds to turn off the power Turn off the main power switch on the EG rear panel see Figure 2 9 Disconnect the main power cord from both its source and from the EG rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the EG HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du EG HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des EG The fuse drawer is located above the main power switch see Figure 9 20 A small tab Fuse locks the fuse drawer in place Using a small Drawer screwdriver pres
190. hemical Detector ED without cell ED titanium cell with reference electrode no working electrode pH Ag AgCl reference electrode pH Ag AgCl reference electrode O ring ED gold working electrode with gasket and polishing kit ED platinum working electrode with gasket and polishing kit ED glassy carbon working electrode with gasket and polishing kit ED silver working electrode with gasket and polishing kit ED AAA gold working electrode with gasket and polishing kit AAA Direct disposable gold working electrodes 6 electrodes with 2 gaskets AAA Direct disposable gold working electrodes 4 packages of 6 electrodes with 8 gaskets Carbohydrate disposable gold working electrodes 6 electrodes with 2 gaskets Carbohydrate disposable gold working electrodes 4 packages of 6 electrodes with 8 gaskets Doc 065031 04 1 08 353 ICS 3000 lon Chromatography System Part Number 064440 063003 060141 045972 062158 036313 036319 036318 036321 061716 056116 056118 064555 064556 064557 045460 045877 045878 061738 061736 061740 061734 061746 062561 062562 Item Disposable platinum working electrodes 6 electrodes with 2 gaskets Disposable silver working electrodes 6 electrodes with 2 gaskets Gaskets for disposable working electrodes 4 gaskets Gasket for non disposable working electrode ED cell polypropylene support block for use with disposable electrodes Polishing
191. hen the valve is closed 1 Click Motor on the pump Control panel in Chromeleon or Chromeleon Xpress to turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Control panel When the system pressure reaches zero do the following e Disconnect the pump from the software by clearing the Connected check box on the Control panel Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the front door of the DP SP to access the mechanical components 4 Use the handles on the component mounting panel to pull the panel forward until it reaches the stop NOTE On newer pumps three red Phillips screws are installed on the component mounting panel before shipment from the factory If the mounting panel does not move freely make sure these screws have been removed 276 Doc 065031 04 1 08 9 DP SP Service 5 The priming valve knob is located on the secondary pump head see Figure 9 9 To remove the knob turn it counterclockwise all the way and then pull it straight off the pump head Priming Valve Secondary Pump Head Figure 9 9 DP SP Priming Valve 6 Pull the old seal off the end of the priming valve knob 7 When correctly installed the groove in the priming valve knob seal faces away from the knob see Figure 9 10 Hold the new seal P N 063382 carefully to avoid scratching or nicking the sides and then slide the seal onto the knob
192. hing 2 A at 24 VDC 1 O ITTL Out TTL Output 1 332 pull up to 5 V 100 mA sink 2 O Gnd Ground 3 O TTLOut2 TTL Output 1 332 pull up to 5 V 100 mA sink 4 lOl Gnd Ground 5 O TTL In1 TTL Input 1 Note TTL input functions are assigned 6 oll TTL In2 TTL Input 2 in software 7 OJ TIL In3 TTL Input 3 8 O TTL In4 TTL Input 4 9 O TTL Ins TTL Input 5 10 O TTL In6 TTL Input 6 11 OJ TTL In7 TTL Input 7 12 O ITTL In8 TTL Input 8 Figure 2 44 Optional Rear Panel 1 0 Connector Strips Doc 065031 04 1 08 79 ICS 3000 lon Chromatography System 2 18 1 CAUTION 1 0 Option Connections 1 Locate the twisted pair of wires P N 043598 and 12 Position 1 position connector plugs P N 923686 see Figure 2 45 provided with the I O Position 12 option board 2 For each I O function 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 2 44 or the label on the DC rear panel for the connector pin assignments Locking Screws Figure 2 45 12 Position Connector Plug 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 ground pin When attaching wires to the connector plug be caref
193. ight position with the electrolyte reservoir at top at 4 to 40 C 39 to 104 F until its next use Cap both ends of the CR TC securely using the plugs supplied with the column To restart the EG 1 5 Select the parameters for the analysis on the EG Control panel in Chromeleon or Chromeleon Xpress Condition the EluGen cartridge see Conditioning the New EluGen Cartridge on page 288 Hydrate the CR TC see Installing and Hydrating the New CR TC on page 291 Hydrate the suppressor as instructed in the product manual Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 Let the system equilibrate for 30 to 45 minutes before collecting data Before shipping the EG Follow the instructions in Section 9 12 Step 4 through Step 9 to disconnect the EluGen cartridge cable cap the EluGen cartridge vent opening remove the EluGen cartridge from the holder and disconnect the inlet and outlet tubing IMPORTANT Make sure the EluGen cartridge packaging conforms to hazardous material shipping requirements Refer to the Material Safety Data Sheet MSDS shipped with the EluGen cartridge for the chemical description 154 Doc 065031 04 1 08 J D C S h u td own 6 3 Consumables Storage The columns suppressors and other consumable items used with an ICS 3000 system have various short and long term storage requirements Refer to the manuals for the indivi
194. ill cause excessive system backpressure 1 Begin pumping eluent through the system including the columns at the flow rate normally used Work backward through the system beginning at the flow cell exit One at a time loosen each fitting and observe the pressure The connection at which the pressure drops abnormally indicates the point of restriction If the EluGen cartridge is the source of the high backpressure replace the outlet frit as instructed in the EluGen cartridge manual The manual is included on the Dionex Reference Library CD ROM P N 053891 If the restriction has caused such high pressure that the system cannot be operated you must work forward through the system adding parts one at a time until an abnormal pressure increase and hence the restriction is found 9 12 Replacing the EluGen Cartridge Replace the EluGen cartridge when the cartridge is expended or when it leaks The CAUTION MISE EN GARDE VORSICHT EluGen cartridge replacement procedure consists of Removing the old EluGen cartridge see Section 9 12 2 Disposing of the old EluGen cartridge see Section 9 12 3 Installing the new EluGen cartridge see Section 9 12 4 Conditioning the new EluGen cartridge see Section 9 12 5 The EluGen cartridge contains one of the following a corrosive base KOH LiOH or NaOH a corrosive acid MSA or a concentrated K CO solution Wear protective eyewear and gloves when handling the cartridge La
195. iltered and deionized water to make a thick paste b Using the working electrode block spread the paste evenly over the pad Then applying firm pressure in a figure eight motion polish the surface of the electrode block for about one minute If the pad dries out while polishing add water sparingly However never allow the polishing compound to dry on the cell body c Use ASTM Type I 18 megohm cm filtered and deionized water to rinse off all traces of polishing compound from the electrode block An ultrasonic cleaner is effective for thoroughly cleaning the electrode block Carefully rinse the surface of the block with ASTM Type I 18 megohm cm filtered and deionized water 4 If you used the coarse polishing compound in Step 3 repeat the step with the fine compound 318 Doc 065031 04 1 08 9 e DC Service 10 11 12 13 Using a moist piece of polishing cloth with no polishing compound added rub the polished surface free of residual polishing compound particles Inspect the surface of the working electrode to make sure that it is clean Repeat Step 5 if necessary NOTE The polishing pads are reusable Do not rinse the polishing compound from the pads After initial use add only enough polishing compound to maintain the coating on the pad Replace the working electrode block and PEEK yoke knob Fingertighten the knob by turning it a full 360 degrees NOTE It is not possible to overtighten the PEEK yoke
196. in ID PharMed Color Black Orange Yellow P N 042690 042855 054410 063268 Used For Connection between pump heads connection from vacuum degassing assembly to proportioning valve or eluent valve Microbore systems only Connection from proportioning valve or eluent valve to inlet check valve Standard bore systems only Connection from proportioning valve or eluent valve to inlet check valve Connection from peristaltic pump to primary pump head Doc 065031 04 1 08 257 ICS 3000 lon Chromatography System 9 2 Tubing Size and Type Color P N Used For 0 15 cm 0 060 in ID Colorless 064079 Connection from peristaltic Tygon 2075 tubing pump to seal wash reservoir connection between pump heads for seal wash 1 58 mm 0 062 in ID Colorless 014157 Connection to eluent reservoirs Teflon or vacuum degassing assembly 1 58 mm 0 062 in ID Colorless 047203 Connection from secondary Polyurethane pump head to waste 10 mm 0 39 in ID Colorless 055075 Drip tray waste line Polyethylene Use 1 16 in fittings P N 052230 and ferrules P N 062511 for connections between the vacuum degassing assembly and the injection valve Use 1 8 in fittings P N 052267 and ferrules P N 048949 for connections to eluent reservoirs Use double cone 10 32 ferrule fittings P N 043276 and 10 32 bolts P N 043275 for all other tubing connections For tightening requirements refer to Installation of Dionex Liq
197. in Amperometry Cell pH Readout The pH readout is considered to have shifted if it is 0 5 pH units or more different from the value observed when the reference electrode was new 1 2 Faulty reference electrode Check the electrode by following the instructions in Section 8 28 6 Regenerate the electrode by soaking in a solution containing 1 M KCI and 1 M HCI long enough to restore the electrode potential to lt 30 mV when compared to an unexposed Ag AgCl reference electrode To test the reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 226 224 Doc 065031 04 1 08 8 DC Troubleshooting 3 If soaking does not fix the problem replace the electrode see Section 9 24 4 8 28 4 No Amperometry Cell pH Readout or Intermittent Readout The pH reading is displayed on the Chromeleon or Chromeleon Xpress EC Detector Control panel Disconnected reference electrode Verify that the reference electrode cable is securely connected see Figure 8 7 Uncalibrated reference electrode Calibrate the reference electrode see Section 9 24 5 Dry reference electrode Soak the reference electrode in a solution containing 1 M KCI and 1 M HCI long enough to restore the electrode potential to lt 30 mV when compared to an unexposed Ag AgCl reference electrode To test the electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift
198. ion to produce the carbonate bicarbonate mixture The EGC CO Mixer provides mixing necessary to produce a homogenous solution of electrolytically generated K CO3 and KHCO eluent For more information about these products refer to the EluGen cartridge manual Cartridge manuals are included on the Dionex Reference Library CD ROM P N 053891 Leak Sensor If liquid collects in the drip tray in the bottom of the EG a leak sensor reports the leak to Chromeleon or Chromeleon Xpress and an error message is displayed in the Audit Trail In addition the Alarm LED on the EG front panel lights Doc 065031 04 1 08 35 ICS 3000 lon Chromatography System Electrical Connections Electrical connectors provide a connection from the components installed in the EG to the EG power supplies There are two sets of electrical connectors one per channel Connections for the following components are provided e Two EluGen cartridges or one cartridge and one EPM Electrolytic pH Modifier and e Two Continuously Regenerated Trap Columns CR TC When operating with an EGC II K CO3 EluGen Cartridge and the EPM the cartridge is connected to the EGC power supply for one channel and the EPM is connected to the EGC power supply for the second channel Thus the EG can accommodate only one such configuration Waste Line The module waste line white tubing discharges liquid and gas waste from the RFIC Eluent Degasser This line is marked WASTE GAS
199. ion will increase in proportion to the decrease in the flow rate In extreme cases excessive heat buildup can occur and damage the EluGen cartridge For a complete list of operating precautions for EluGen cartridges and CR TC trap columns refer to the product manuals The manuals are provided on the Dionex Reference Library CD ROM P N 053891 114 Doc 065031 04 1 08 4 Startup 4 1 2 ED Amperometry Cell Operating Precautions To prevent electrode contamination e Run only clean filtered samples e Prepare all eluents with high purity ASTM Type I 18 megohm cm filtered and deionized water e Avoid contamination of the cell with incompatible eluents Never apply potential to the electrode unless a stream of eluent or water is flowing through the cell Do not allow the reference electrode to dry out Make sure that eluent is pumped continuously through the cell If the cell will not be used for a short time less than 2 days disconnect the tubing from the inlet and outlet fittings and install fitting plugs For longer shutdowns see Section 6 4 Be careful to keep the polished surface of the amperometry cell body clean and dry when not in use The gold spring loaded pogo contact must also remain clean and dry If a salt bridge forms it can cause an electrical short between the working electrode contact and the cell body If the conventional nondisposable working electrode becomes discolored or if you notice
200. it is defective Replace both check valve cartridges see Section 9 4 Eluent proportioning valve leaks gradient pump only Tighten loose fittings If there are no loose fittings the proportioning valve assembly should be replaced Contact Dionex for assistance Priming valve knob leaks If leaks occur when the priming valve knob is open close the knob completely and then open it one half to three quarters turn If this does not stop the leakage replace the seal in the priming valve knob see Section 9 8 If leaks occurs when the priming valve knob is closed either the pump head or the knob is damaged and should be replaced Contact Dionex for assistance Excessive system backpressure If system backpressure is substantially higher than the normal operating backpressure for the currently configured system including the column tubing may be plugged or overtightened Follow the procedure below to isolate segments of the flow path and determine the sources of the high backpressure 1 Remove the pump outlet tubing at the injection valve 2 Press the POWER button on the front of the DP SP to turn on the pump 3 Set the Flow rate to 1 0 mL min on the Chromeleon or Chromeleon Xpress Control panel and record the backpressure 4 One at a time reconnect each component tubing fittings etc of the flow path If reconnecting a component causes an abnormal increase in 200 Doc 065031 04 1 08 8 DP SP Troubleshooting
201. ittings The pressure in the left hand working cylinder exceeded the safety limit Or The pressure in the right hand working cylinder exceeded the safety limit Or The system pressure exceeded the safety limit This error may be caused by a blockage in the system or by a problem with the column Right hand refers to the bottom pump left hand refers to the top pump in a dual pump module 194 Doc 065031 04 1 08 8 DP SP Troubleshooting To troubleshoot 1 Check all tubing connections for signs of blockage and replace it as needed Be careful not to overtighten fittings As columns age their backpressure increases It may be necessary to compensate for this by increasing the high pressure limit If the column is the source of the high backpressure clean the column Refer to the column manual provided on the Dionex Reference Library CD ROM P N 053891 for instructions If this does not eliminate the problem replace the column Observe a run to see whether the high pressure limit is triggered when injection occurs if it is the injection valve may be the source of the blockage i e the rotor seal or stator may need to be replaced Contact Dionex for assistance O The rear seal leak count is x x counted drops and has exceeded the limit of y y leak detection threshold This error occurs when the cap on the seal wash reservoir is equipped with a drop sensor and the number of drops of w
202. ity See Level This function cannot be adjusted by the user Abort page 196 Upper pressure limit exceeded Abort page 196 8 1 2 EG Error Messages The table below lists the EG related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table EG Related Audit Trail Error Message Default Severity See Level CR TC1 over current Abort page 203 CR TC2 over current CR TC1 stopped due to zero flow Abort page 203 CR TC2 stopped due to zero flow EG1 cartridge disconnected Abort page 204 EG2 cartridge disconnected EG1 invalid concentration Abort page 204 EG2 invalid concentration EG1 invalid flow Abort page 205 EG2 invalid flow EG1 invalid flow rate concentration Abort page 205 EG2 invalid flow rate concentration EG1 over current Abort page 205 EG2 over current EG1 over power Abort page 206 EG2 over power EG1 over voltage Abort page 206 EG2 over voltage Leak sensor wet Warning page 207 Doc 065031 04 1 08 171 ICS 3000 lon Chromatography System 8 1 3 DC Error Messages The table below lists the DC related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table DC Related Audit Trail Error Message Default Severity See Level CD cell 1 option disconnected Abort page 213 C
203. izard EDet1 Options x Amperometry Cell Channels Data Collection Rate utozero On M 3D_Amp 1 0 7 Hz C Yes C of F EDA No M ED_1_Total m Waveform Selector ET Insert CELA ES Y Amino Acids pHiAgi Alcohols Formic AlcoholsWave Amino Acids Ag 4 Amino Acids pH amp aus Reference Electrode Mode asci Upper Limit fi 3 0 pH Lower Limit fio o lt Back Next gt Cancel Help Figure 2 28 Pre Programmed Waveforms Doc 065031 04 1 08 65 ICS 3000 lon Chromatography System You can use a pre programmed waveform without modification or modify it for your application You can also define a new waveform Waveforms are defined and modified in the Waveform Editor see Figure 2 29 Click the Edit button on the Program Wizard ED Options page to view the Waveform Editor Waveform Editor x Waveform Alcohals Formic acid Glycols 7 Save Delete Description Alcohols Formic acid Glycols Append No Time s Votage V GainRegion Ramp integration 4 ra 0 2000 off off 0 2000 on ra on Insert 0 4000 0 2000 off ra off 4 0 4100 1 2500 off ra off Delete 5 0 5000 1 2500 off ra off x EER Figure 2 29 Waveform Editor 66 Doc 065031 04 1 08 2 DC Description Analytical vs Scanning Waveforms The pre programmed analytical waveforms supplied with Chromeleo
204. kit Coarse polishing compound Fine polishing compound Polishing pads Conductivity Detector and Accessories ICS 3000 Conductivity Detector AAES Anion Atlas Electrolytic Suppressor CAES Cation Atlas Electrolytic Suppressor ASRS 300 2 mm Anion Self Regenerating Suppressor CSRS 300 4 mm Cation Self Regenerating Suppressor CSRS 300 2 mm Cation Self Regenerating Suppressor Suppressor gas separator waste tube Backpressure coil for 4 mm suppressor Backpressure coil for 2 mm suppressor Automation Manager ICS 3000 Automation Manager two 10 port high pressure valves two low pressure 3 way valves ICS 3000 Automation Manager one 10 port high pressure valve one low pressure 3 way valve ICS 3000 Automation Manager one 6 port high pressure valve one low pressure 3 way valve ICS 3000 Automation Manager tray with no valves RCH 1 Reaction Coil Heater Temperature stabilizer standard bore 0 25 mm 0 010 in ID Temperature stabilizer microbore 0 125 mm 0 005 in ID 354 Doc 065031 04 1 08 B DC Reordering Information Part Number 062201 923686 043598 954772 960777 062437 043276 043275 044105 061796 Item Analog Output Relay TTL T O option Connector plug 12 position Twisted pair of wires Miscellaneous Fuse IEC 60127 2 slow blow rated at 10A 250V USB cable 1 8 m 6 ft long Leak sensor Ferrule fitting 10 32 double cone Fitting bolt 10 32 for double cone ferrule fitting Filter high pressure i
205. le Processing Overview With either manual or batch sample processing you can load samples into the sample loop with either an autosampler see Section 5 2 or with a syringe through the sample loading ports on the DC front door see Section 5 3 Doc 065031 04 1 08 139 ICS 3000 lon Chromatography System 5 2 5 3 Loading Samples with an Autosampler 1 Verify that the autosampler output line is connected to port S 5 on the DC or TC injection valve Direct the waste line as required for this autosampler model Prepare and fill the sample vials and place them in the autosampler tray or cassette Refer to the autosampler manual for detailed instructions Autosampler manuals are provided on the Dionex Reference Library CD ROM P N 053891 Use one of the following methods to load sample into the injection valve sample loop e Manually Click the Load Inject button on the Autosampler Control panel in Chromeleon or Chromeleon Xpress see Figure 5 2 e Automatically Include the Load command in a Chromeleon or Chromeleon Xpress program See the examples in Section 5 4 Sample Control Sample Position 1 Injector Position LoadPosition Sample Volume 20 0 pl Injector 2 Position Load Inject Home Tray Temp Figure 5 2 Control Panel Load Inject Button Loading Samples with a Syringe This section describes two methods for using a syringe to load sample into the DC injection valve
206. lean the working electrode with water and dry with pressurized air or nitrogen Remove any precipitate on the counter electrode by cleaning the spot directly opposite the working electrode with a lint free tissue DC Amperometry and Integrated Amperometry modes Leak between gasket and electrode or between gasket and cell body Remove any precipitate with water and a lint free tissue and then install a new gasket see Section 9 24 2 Turn the PEEK yoke knob see Figure 9 33 a full 360 degrees to completely engage the knob 188 Doc 065031 04 1 08 DP SP Troubleshooting 8 12 Troubleshooting DP SP Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail A program with this name already exists This error occurs if you attempt to save a modified Chromeleon or Chromeleon Xpress program under the name of an existing program To troubleshoot Enter a new name for the modified program or select Save to save your changes under the existing program name Abnormal drive current for x x seconds If this error occurs the tubing between the pump heads may be blocked or the fitting may be overtightened To troubleshoot Inspect the tubing for blockage or crimping and replace if needed Be careful to not overtighten the fitting If the message appears again contact Dionex for assistance Camshaft index too early Of Camshaft i
207. leon Xpress or on the panel tabset in Chromeleon 2 Click the Calibration button under Conductivity Detector Settings The Wellness panel opens see Figure 9 29 zx External Conductivity Cell Calibration Update Wellness Database Press for instructions Instructions Press for instructions Instructions Cond Cell Calibration Calibrate Settings to Download Current gt Log Cell 1 Cal Value Log RAS FES Log Cell 2 Cal Value Log Cell Serial Number Current Calibration Date 4 19 2006 Last Calibration Date 4 19 2006 Dummy Cell Control Cell Control Normal H Service Wellness Close Figure 9 29 Wellness Panel ICS 3000 Conductivity Detector 308 Doc 065031 04 1 08 9 DC Service On the Wellness panel under External Conductivity Cell Calibration click Instructions for a summary of the procedure described in detail in this section Disconnect the pump output line from the injection valve Disconnect the line from the suppressor ELUENT OUT port to the cell inlet and connect the pump output line directly to the cell mlet Verify that there is a minimum of 7 MPa 1000 psi of backpressure Set the cell heater to 35 C Allow the cell to reach this temperature and then wait an additional 5 minutes to let it stabilize Begin pumping 1 0 mM KCI through the cell at 1 0 mL min Wait until the total conductivity reading stabilizes in about 15 minutes Open
208. leshooting 8 25 Troubleshooting DC Error Messages 213 8 26 Liquid Leaks from DC Components 221 8 27 VALVE Button Not Working 222 8 28 Amperometry Cell Troubleshooting 223 8 28 1 Amperometry Cell pH Readout Always 7 0 223 8 28 2 Cannot Set Amperometry Cell pH Readout to 7 0 224 8 28 3 Shift in Amperometry Cell pH Readout 224 8 28 4 No Amperometry Cell pH Readout or Intermittent Readout 225 8 28 5 Leak in pH Reference Electrode Compartment 225 8 28 6 Shift in Ag AgCl Reference Potential 226 TC Troubleshooting 8 29 Troubleshooting TC Error Messages 227 8 30 TC ALARM LED Is Lighted i002 yeh o wie eerie ita ea 253 8 31 Liquid Leaks from TC Components 253 8 32 TC Temperature Does Not Increase 254 8 33 TC Temperature Stabilizer Not Operating Properly 255 9 Service DP SP Service 9 1 Replacing Tubing and Fittings 257 9 2 Cleaning Eluent Reservoirs 258 Doc 065031 04 1 08 ix ICS 3000 lon Chromatography System 9 3 Priming the DP SP 259 9 3 1 Priming with the PUMP PRIME Button 259 9 3 2 Priming from the Control Panel
209. lines Start the pump flow Turn on the DC power Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 9 24 6 Replacing the Reference Electrode O Ring 1 Turn off the cell voltage from the Control panel in Chromeleon or Chromeleon Xpress Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump Disconnect the cell see Section 9 24 1 Unscrew the reference electrode and remove it from the cell body see Figure 9 40 324 Doc 065031 04 1 08 9 e DC Service Unscrew the reference electrode Figure 9 40 Removing the Reference Electrode 5 To remove any particulate matter such as salt crystals rinse and dry the reference electrode cavity 6 Remove the O ring from the bottom of the reference electrode see Figure 9 41 Reference Electrode O Ring Figure 9 41 Removing the Reference Electrode O Ring 7 Slide the new O ring P N 014067 onto the electrode 8 To avoid any hydraulic pressure buildup when inserting the reference electrode make sure that fitting plugs are not installed on the cell inlet and outlet fittings 9 Screw the reference electrode into the cell body and tighten firmly with your fingers Doc 065031 04 1 08 325 ICS 3000 lon Chromatography System 10 11 12 13 Orient the cell assembly with the PEEK yoke knob see Fig
210. llowing models are available 6 port P N 061961 and 10 port P N 061962 2 14 1 Injection Valve Operation Each ICS 3000 Ion Chromatography System injection valve has two operating positions Load and Inject Liquid flows through either the Load or Inject path depending on the valve position Figure 2 16 shows flow schematics for the 6 port valve LOAD POSITION Sample In INJECT POSITION Sample In To Column Sample Loop P76 To Waste From Pump To Waste Sample Eluent To Column From Pump Figure 2 16 Injection Valve Flow Schematics 6 Port Valve e In the Load position sample is loaded into the sample loop where it is held until injection Eluent flows from the pump through the valve and to the column bypassing the sample loop Sample flows from the syringe or autosampler 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 5 3 describes how to inject samples manually and Section 5 2 describes how to inject samples with an autosampler 50 Doc 065031 04 1 08 2 DC Description Figure 2 17 shows example flow schematics for the 10 port valve when it is connected for an a
211. low LiOH 0 1 to 80 mM at 0 1 to lt 1 0 mL min flow 0 1 to X mM at 1 0 to lt 3 0 mL min flow where X 80 flow MSA 0 1 to 100 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 3 0 mL min flow where X 100 flow NaOH 0 1 to 100 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 3 0 mL min flow where X 100 flow Table 4 1 Eluent Concentration Ranges for Single Cartridge and Independent Dual Cartridge Configurations 132 Doc 065031 04 1 08 4 EG Startup Linked Dual Cartridge Configuration In the linked dual cartridge configuration the EG contains two EluGen cartridges linked to a single pump that perform as one cartridge Note that the allowable eluent concentration for a linked cartridge is less than when the cartridge is defined as independent For details refer to the EluGen cartridge manual Cartridge manuals are included on the Dionex Reference Library CD ROM P N 053891 EluGen Eluent Concentration Range Comment Cartridges K CO EPM 0 1 to 15 mM at 0 1 to 1 0 ml min flow The total of the eluent Electrolytic pH 0 1 to X mM at 1 0 to 2 0 ml min flow concentrations from Modifier where X 15 flow both cartridges K CO3 and EPM must not exceed the specified range The EPM concentration must not exceed 10 mM See the notes below for additional information KOH KOH 0 1 to 50 mM at 0 1 to 1 0 mL min flow The eluent concentration KOH MSA 0 1 to X mM at 1 0 to 3 0 mL min f
212. low range for each cartridge KOH NaOH where X 50 flow is 50 of the range for a MSA MSA single cartridge or MSA NaOH independent dual NaOH NaOH cartridge configuration LiOH LiOH 0 1 to 40 mM at 0 1 to 1 0 mL min flow The eluent concentration 0 1 to X mM at 1 0 to 3 0 mL min flow range for each cartridge where X 40 flow is 50 of the range for a single cartridge or independent dual cartridge configuration Table 4 2 Eluent Concentration Ranges for Linked Dual Cartridge Configurations Notes for Generating Carbonate Bicarbonate Eluent Ifa K CO3 EluGen cartridge and an EPM Electrolytic pH Modifier are installed EGC_1 and EGC 2 respectively set EGC_1 Target Concentration to the concentration of K CO3 required for your application and set EGC_2 Target Concentration to the concentration of KHCO3 required In order to achieve the Doc 065031 04 1 08 133 ICS 3000 lon Chromatography System desired K CO KHCO eluent mixture the K CO3 cartridge must generate the total of the two target concentrations For example for a 3 50 mM K CO3 1 00 mM KHCO eluent set EGC_1 to 3 50 mM and EGC 2 to 1 00 mM When eluent is being generated the K CO3 cartridge generates 4 50 mM K CO This is indicated in the Applied Concentration field for the K CO EluGen cartridge The EPM modifies the 4 50 mM K CO eluent to achieve the desired 3 50 mM K CO3 1 00 mM KHCO mixture 134 Doc 065031 04 1 08 4 8 Start t
213. low IMPORTANT can severely damage the cartridge 3 Store the EluGen cartridge in the EG during the shutdown To restart the EG 1 Select the parameters for the analysis on the EG Control panel in Chromeleon or Chromeleon Xpress 2 Ifthe EG has been shut down for more than 3 to 4 days hydrate the suppressor as instructed in the product manual Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 3 Let the system equilibrate for 30 to 45 minutes before collecting data 6 2 Long term Shutdown If the shutdown is for 3 months or more follow the instructions below To prepare the EG for the shutdown 1 Turn off the EG including all consumables installed in the EG the CR TC suppressor etc 2 Verify that the current to the EluGen cartridge and the suppressor is off Supplying power to the EluGen cartridge when there is no eluent flow IMPORTANT can severely damage the cartridge Doc 065031 04 1 08 153 ICS 3000 lon Chromatography System If you plan to store the EluGen cartridge in the EG no further action is required If you plan to store the cartridge outside the EG for example in the original shipping container follow the instructions in Section 9 12 Step 4 through Step 9 to disconnect the EluGen cartridge cable cap the EluGen cartridge vent opening remove the EluGen cartridge from the holder and disconnect the inlet and outlet tubing Store the cartridge in an upr
214. ls Detailed descriptions of ICS 3000 system components and important operating features includes an introduction to Chromeleon and Chromeleon Xpress software Detailed illustrations of component plumbing for several different ICS 3000 system configurations Tasks to be performed before beginning operation of the ICS 3000 system Instructions for routine operation of the ICS 3000 system with Chromeleon or Chromeleon Xpress software Short term and long term shutdown procedures for the ICS 3000 system Routine preventive maintenance procedures for the ICS 3000 system Doc 065031 04 1 08 11 ICS 3000 lon Chromatography System 1 3 2 gt DANGER gt WARNING gt CAUTION IMPORTANT Chapter 8 Troubleshooting Chapter 9 Service Appendix A Specifications Appendix B Reordering Information Minor problems that may occur during operation of the ICS 3000 system with step by step procedures for how to isolate and eliminate the cause of each problem Includes a list of Chromeleon and Chromeleon Xpress Audit Trail error messages with an explanation of the possible cause of each message and the corrective action to take Step by step instructions for routine service and parts replacement procedures the user can perform for the ICS 3000 system Specifications and installation site requirements for the ICS 3000 modules Spare parts for the ICS 3000 modules Safety Messages and Notes
215. m All other maintenance procedures must be performed by Dionex personnel For information about maintenance procedures for the EluGen cartridge CR TC trap column or suppressor refer to the appropriate product manual These manuals are included on the Dionex Reference Library CD ROM P N 053891 EG Daily Maintenance Locate and repair leaks inside the EG see Section 9 11 and wipe up liquid Rinse dried eluents off components with deionized water Rinse the EG drip tray with deionized water to prevent formation of salt crystals and dry the drip tray thoroughly Rinse and dry the leak sensor also if the sensor is not dry it will remain activated and continue to report a leak to the Audit Trail Check the waste container and empty as needed EG Weekly Maintenance Check all air and liquid lines for crimping Move or reroute pinched lines and replace damaged lines see Section 9 10 For help in isolating the cause of a tubing restriction see Section 9 11 Monitor the system backpressure A gradual increase in backpressure can indicate clogging of the EluGen cartridge inlet frit from particulates in the eluent water EG Annual Maintenance Check the expiration date and remaining lifetime of the EluGen cartridge on the EG Control panel in Chromeleon or Chromeleon Xpress Doc 065031 04 1 08 163 ICS 3000 lon Chromatography System 164 Doc 065031 04 1 08 7 9 7 10 7 11 DC Routine Maintenance This
216. m consists of a peristaltic pump a reservoir containing wash solution and the connecting tubing The wash solution is usually ASTM Type I 18 megohm cm filtered and deionized water When seal washing is activated the back of the main piston seal is rinsed with wash solution this prolongs seal lifetime by preventing eluent crystallization on the seal surfaces Notes About the DP Piston Seal Wash System The piston seal wash system is designed for use with only one of the two pumps in a DP module When the DP is shipped from Dionex the seal wash system is connected to pump 1 the bottom pump If necessary connect the seal wash system to pump 2 the top pump instead For instructions on how to replumb the system refer to Section 4 5 NOTE Dionex offers an External Seal Wash Kit P N 063518 for users who need to operate a piston seal wash system for both pumps in the DP Installation instructions are provided in the kit Static Mixer A GM 3 or GM 4 static mixer is installed after the secondary pump head see Figure 2 3 In the gradient pump the mixer helps to ensure that proportioned eluents are mixed thoroughly In the isocratic pump the mixer is optional but can function as a pulse damper The DP SP gradient delay volume is 600 uL when a GM 3 is installed and 380 uL when a GM 4 is installed The gradient delay volume or dwell volume is the volume of liquid in the system between the point where the gradient is formed and the
217. mperometry includes pulsed amperometry see Section 2 16 4 e Cyclic voltammetry see Section 2 16 5 2 16 1 Amperometry Cell The ED amperometry cell is a three electrode voltammetric cell It is a miniature flow through cell with a titanium cell body the counter electrode a working electrode and a combination pH Ag AgCl reference electrode see Figure 2 22 The type of working electrode used depends on the application Four conventional non disposable working electrode types are available gold platinum silver and glassy carbon Three disposable working electrodes types are available gold silver and platinum A Working Electrode Cell Body H nemical b 1 counter electrode Reference Electrode Figure 2 22 Amperometry Cell Titanium Cell Shown Doc 065031 04 1 08 57 ICS 3000 lon Chromatography System 2 16 2 Cell Design The ED amperometry cell is a thin layer design Eluent flows in a thin channel parallel to the surface of a flat disk electrode The resulting smooth flow minimizes noise The low volume 0 25 uL of the channel also allows operation with high efficiency narrow bore columns The cell design minimizes the electrical resistance between the working electrode and the counter electrode by positioning the counter electrode the cell body directly across the thin layer channel from the working electrode This results in a wide linear dynamic range The inlet t
218. mperometry modes Dirty or pitted conventional nondisposable working electrode Polish the working electrode see Section 9 24 3 If you are using a disposable electrode replace it Integrated Amperometry mode Regular baseline oscillations 1 Check the pump pressure plot to verify that the pump is working properly 180 Doc 065031 04 1 08 8 Troubleshooting 2 Air bubbles may be trapped inside the cell While wearing gloves and eye protection generate a slight temporary backpressure by putting your finger over the end of the cell outlet tubing for 2 to 3 seconds Repeat 2 or 3 times If the baseline does not improve check the other causes of baseline instability described in this section Do not block the end of the cell outlet tubing for longer than the recommended 2 to 3 seconds Doing so creates high backpressure which can break the reference electrode glass membrane NOTE To prevent air from becoming trapped in the cell in the future increase the backpressure on the cell by connecting backpressure tubing to the cell outlet The backpressure limit for the ED cell is 690 kPa 100 psi Do not exceed this limit 3 The water used to prepare the eluent contains trace contaminants Remake the eluent using ASTM Type I 18 megohm cm filtered and deionized water containing no contaminants 8 3 Poor Retention Time Reproducibility e Liquid leaks 1 Check for leaks from the piston seals Replace the piston seal
219. mproved performance when dealing with dirty matrices The MS detector is equipped with FastLockTM probes for two complementary ionization techniques atmospheric pressure chemical ionization APCD and electrospray ionization ESI Both ionization techniques can be run in either the positive or negative ion polarity mode The design of the interchangeable probes enables rapid switching of ionization modes During a scan ions of selected mass to charge ratios are sequentially transmitted through a quadrupole mass filter analyzer The MS detector has fully automatic mass scale calibration 15 to 2000 m z and tuning that makes optimization simple and direct The MS detector can perform both full range scans and selected ion monitoring SIM scans When operating in conjunction with Chromeleon the MSQ Plus can be set up to vary the scan type the ionization technique and the ion polarity mode 8 Doc 065031 04 1 08 1 Introduction 1 1 2 ICS 3000 System Control The ICS 3000 system is controlled by a PC configured with Chromeleon Chromatography Management System version 6 7 or later or Chromeleon Xpress The Chromeleon Chromatography Management System provides complete instrument control data acquisition and data management Chromeleon Xpress provides real time control and monitoring of Dionex chromatography instruments but does not include data management capabilities Chromeleon and Chromeleon Xpress provide a panel tabset t
220. mum temperature gt ambient 50 C CD cell 15 to 60 C Minimum temperature gt upper compartment temperature 5 C RCH 1 15 to 80 C Minimum temperature gt upper compartment temperature 5 C For example if the ambient air temperature in your lab is 30 C and you set the upper compartment temperature to 15 C the actual temperature achieved in the upper compartment will be about 20 C 46 Doc 065031 04 1 08 2 DC Description NOTE A DC Temperature Calibration Kit P N 063782 is available The kit includes the parts and instructions required to verify the temperature calibration of the DC upper and lower compartments and to recalibrate if required 2 13 DC Rear Panel Figure 2 15 illustrates the rear panel of the DC 5 e s HN qu HN MIT QUIL K Int HU a 7i gt Q Tubing Chase 2 e Q Drain Line Connector Switched AC Sockets Fuse Holder Main Power Switch and Power Receptacle External Low Pressure Valve Mounting Slots USB Receptacle B Connector USB Ports 2 A Connectors External Low Pressure Valve Connectors Analog Output and TTL Relay Connectors optional Figure 2 15 DC Rear Panel Tubing Chases The tubing chases route tubing from the front compartment through the DC interior and to the rear panel Foam inserts insulate the chases
221. n are designed for quantitative analysis of specific compounds alcohols amino acids carbohydrates etc With analytical waveforms integration occurs either while a single constant potential is being applied over time see the example waveform in Figure 2 24 or while a series of stepped potentials are being applied see the example waveform in Figure 2 25 With scanning waveforms integration occurs while the potential is being increased linearly over time see the example scanning waveform in Figure 2 30 Although scanning waveforms are typically not as useful for quantitative analysis as analytical waveforms when used to collect 3D amperometric data scanning waveforms can be optimized to provide characteristic I t plots see Section 2 16 7 Comparison of I t plots of a known substance with an unknown can help to identify unknown peaks or to determine whether a substance is coeluting with another 1 0 4 0 0 j i Potential Volts a 1 0 Integration 2 5 0 0 0 5 1 0 15 2 0 Time Seconds E1 E2 mac E1 Pre adsorption potential E2 Scanning potentials E3 Reductive cleaning potential E4 Oxidative cleaning potential Figure 2 30 Example Scanning Waveform Doc 065031 04 1 08 67 ICS 3000 lon Chromatography System 2 16 7 Storing and Reprocessing Amperometry Data NOTE Chromeleon Xpress cannot store or reprocess amperometry data Chromeleon
222. n abnormal pressure increase and hence the restriction is found e TC temperature stabilizer is blocked Rinse the temperature stabilizer and the temperature stabilizer inlet line using an appropriate solvent If necessary replace the temperature stabilizer standard bore P N 064548 microbore P N 064650 8 10 Low Detector Output e Insufficient sample injected Increase the injection size or concentration ED Only e Working electrode fouled 1 Ifa disposable working electrode is being used replace the electrode 2 For conventional nondisposable electrodes clean the working electrode with ASTM Type I 18 megohm cm filtered and deionized water Dry 186 Doc 065031 04 1 08 8 Troubleshooting with pressurized air or nitrogen If the electrode is pitted polish the electrode see Section 9 24 3 3 Check the value of the reference potential shift See Using a Digital Voltmeter to Determine Reference Potential Shift on page 226 If the value fluctuates by more than 30 mV electrode passivation may occur because potentials that are too high are being applied Recalibrate the reference electrode see Section 9 24 5 If the problem persists replace the reference electrode see Section 9 24 4 Analog Output Option e Analog output range set too high Select a more sensitive analog output range 8 11 High Background e CR TC is contaminated Clean the trap column as instructed in the CR TC manual T
223. n in Recycle Mode Eluent from the pump or EG flows into the injection valve e After sample is loaded into the sample loop and the injection valve is toggled to the Inject position eluent passes through the loop e The eluent sample mixture is pumped first through a temperature stabilizer then on to the guard and separator columns and then through the suppressor e From the suppressor the mixture flows through the cell where the analytes are detected A digital signal is sent to Chromeleon or Chromeleon Xpress software e 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 If an EG is installed flow is routed to the CR TC see Section 2 10 for details 56 Doc 065031 04 1 08 2 DC Description 2 16 ED Electrochemical Detector One or two ICS 3000 Electrochemical Detectors EDs can be installed in the DC Each complete ED assembly consists of an amperometry cell and the detector electronics required to collect data and send it to the computer and the analog output if installed The detector is installed in the upper compartment of the DC see Figure 2 13 The cell mounts on the front of the detector The detector electronics are not accessible to the user The ED can perform the following electrochemical detection modes e DC amperometry see Section 2 16 3 e Integrated a
224. nHP valve 2 position 6 port or 2 position 10 port up to two valves can be installed Humidity sensor and gas sensor Temperature control and temperature sensors 348 Doc 065031 04 1 08 B Reordering Information DP SP Reordering Information Part Number 062083 045722 045721 062062 062063 062648 064946 040695 062064 063382 062092 062082 062079 062087 063382 064946 040695 062064 062092 062082 063382 Item Primary Pump Head Components Primary pump head Inlet check valve assembly includes inlet nut and 1 8 in cartridge Outlet check valve assembly includes outlet nut and 1 8 in cartridge Inlet check valve nut use only to replace an existing nut of the same type Outlet check valve nut use only to replace an existing nut of the same type 1 16 in cartridge use only if the following check valve nuts are currently installed inlet nut P N 062062 outlet nut P N 062063 Main piston seal O ring Seal wash body Piston seal wash seal Retainer for piston seal wash seal Piston Secondary Pump Head Components Secondary pump head Priming valve Piston seal wash seal Main piston seal O ring Seal wash body Retainer for piston seal wash seal Piston Priming valve knob seal Doc 065031 04 1 08 349 ICS 3000 lon Chromatography System Part Number 064155 063268 064079 063518 062628 062629 063291 062510 063292 063493 064792 062345 045987 044105
225. nates the need to perform extractions for analyses that do not require spectral data and it conserves disk space ICS Series Variable Wavelength Detector VWD The VWD is a dual beam variable wavelength photometer with one measurement and one internal reference beam Spectral capability from 190 to 900 nm is provided by two light sources a deuterium lamp for ultraviolet detection and a tungsten lamp for visible wavelength operation The four channel detector measures at up to four wavelengths simultaneously The VWD contains a built in holmium oxide filter for wavelength verification To suppress higher order radiation two optical filters can be inserted automatically into the light path Doc 065031 04 1 08 ICS 3000 lon Chromatography System MSQ Plus Mass Spectrometer The MSQ Plus is an advanced analytical instrument that includes an MS detector vacuum pumps and data system When integrated with an IC system the MSQ Plus provides the separation capability of an IC and the detection capability of a single quadrupole MS detector This provides a strong starting point for sample analysis by offering a quick and clear mass identification for chromatographic peaks The MS detector contains an atmospheric pressure ionization API source advanced high efficiency transmission ion optics of a square quadrupole RF lens and dual RF generators a mass analyzer and an ion detection system An optional cone wash pump is available for i
226. nce or service procedures CAUTION Afin d viter toute br lure laisser refroidir le compartiment thermique avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der TC abgekuhlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the TC door 4 Disconnect each liquid line connected to the injection valve 5 Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 330 Doc 065031 04 1 08 TC Service 6 Reconnect all liquid lines to the injection valve see Figure 9 45 SAMPLE IN from door inject port or autosampler 25 pL SAMPLE LOOP Orange TO INJECT VALVE P Figure 9 45 Injection Valve Plumbing 6 Port Valve TOINJ _ Red microbore VALVE C Black standard bore 7 Turn on the power to the TC 8 Turn on the pump flow Check for leaks from the valve Tighten fittings as required see Section 9 25 9 Close the TC door 9 28 Replacing an Injection Valve Pod This procedure describes how to replace the mechanical part the pod of the TC injection valve NOTE If the valve electronics require service contact Dionex Electronics related repair procedures must be performed by Dionex personnel NOTE Substitution of non Dionex parts may impair valve performance and void the
227. nd LEDs 31 System configuration 105 USB connections 37 Waste lines 36 38 Weight 339 Eluent Organizer EO 2 5 30 Eluent proportioning valves 20 Eluent reservoirs See Reservoirs eluent Eluents Aqueous 161 Degassing 21 Filtering 123 Flushing lines after eluent change 181 Monitoring pH 58 Outgassing 312 EluGen cartridges 5 34 Backpressure requirement 34 113 114 209 210 Conditioning procedure 154 Electrical connections 36 Eluent generation 39 Frit outlet 186 282 Leaks 185 207 209 Replacement procedure 282 Selecting the eluent concentration 131 Start up procedures 154 Storage long term 154 Storage short term 153 End line filter See Filter end line 123 EO Regulator Kit 30 EPM Electrolytic pH Modifier 34 36 Electrical connections 36 Equilibration 136 138 Error messages Audit Trail description 169 DC summary 172 DP SP summary 170 EG summary 171 TC summary 173 Error messages DC 213 216 218 221 227 CD cell disconnected 213 CD cell over safe temperature 214 Column open circuit 214 Column over safe temperature 214 Compartment open circuit 214 Compartment over safe temperature 215 ED cell disconnected 215 216 High pressure valve error 216 Lower leak sensor wet 218 Reaction coil open circuit 219 Reaction coil over safe temperature 219 Suppressor open circuit 220 Suppressor over current 219 Suppress
228. ndex too late This error is caused by an internal error in the pump drive mechanism To troubleshoot Turn off the DP SP power for 30 seconds and then turn it on again If the error message appears again contact Dionex for assistance Doc 065031 04 1 08 189 ICS 3000 lon Chromatography System Camshaft sensor always alight Of Camshaft sensor missing or dark This error is caused by an internal error in the pump drive mechanism To troubleshoot Turn off the DP SP power for 30 seconds and then turn it on again If the error message appears again contact Dionex for assistance Degasser malfunction The vacuum degassing module monitors the vacuum system continuously Ifa a problem is detected this error occurs To troubleshoot 1 Check all tubing connections to the vacuum degassing module for leakage tighten loose fitting connections 2 Turn off the DP SP power for 30 seconds and then restart the pump 3 Ifthe message appears again the vacuum degassing module should be replaced Contact Dionex for assistance Excessive drive current Camshaft x x This error occurs if the drive current is above the allowed value When this message appears the DP SP stops running To troubleshoot One or more tubing connections may be plugged blocked or crimped Check all tubing connections and replace as needed see Section 9 1 Be careful not to overtighten fittings 190 Doc 065031 04 1 08 8 DP SP Tro
229. ne Disconnect outlet line Figure 9 32 Disconnecting the Amperometry Cell Titanium Cell Shown Doc 065031 04 1 08 313 ICS 3000 lon Chromatography System 9 24 2 Replacing an Amperometry Cell Gasket These instructions are for conventional nondisposable working electrodes only To install a disposable working electrode refer to the manual which is shipped with the electrode When to Replace the Gasket Replace the gasket if there is a leak between the gasket and electrode or between the gasket and cell body Items Needed e Amperometry cell gasket for nondisposable working electrodes P N 045972 e Gloves e Blunt end tweezers Amperometry Cell Gasket Replacement Procedure NOTE To avoid electrode fouling always wear gloves when handling electrodes 1 Turn off the cell voltage from the Control panel in Chromeleon or Chromeleon Xpress 2 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump 3 Disconnect the cell see Section 9 24 1 4 Loosen the PEEK yoke knob holding the working electrode to the cell body by unscrewing it two to three turns 5 Squeeze the tabs on the sides of the yoke block and pull the block and knob off the working electrode see Figure 9 33 314 Doc 065031 04 1 08 9 e DC Service First loosen the PEEK yoke knob Then squeeze the tabs on the yoke block and pull to remo
230. nline Maintenance Kit DC TC Annual Preventive Maintenance Kit Doc 065031 04 1 08 355 ICS 3000 lon Chromatography System 356 Doc 065031 04 1 08 or Part Number 057896 061759 061961 061962 042857 6710 1505 064786 064548 064650 954776 063246 6000 1004 064792 061796 H i TC Reordering Information Item Valves and Accessories Injection Valve Rebuild Kit for 6 port valve includes valve seal hexagon wrench and instructions Injection Valve Rebuild Kit for 10 port valve includes valve seal hexagon wrench and instructions Injection valve head including seal for 2 position 6 port valve Injection valve head including seal for 2 position 10 port valve Sample loop 25 uL Consumables Column ID Kit includes five column ID chip cards Column Clips Kit includes six column clips Temperature stabilizer standard bore 0 25 mm 0 010 in ID Temperature stabilizer microbore 0 125 mm 0 005 in ID Miscellaneous Fuse IEC 60127 2 time lag rated at 2 A two fuses required USB cable 1 m 3 ft 6 pin mini DIN signal cable 5 m 16 4 ft TC VWD PDA Regulator Bracket Kit Maintenance Kit DC TC Annual Preventive Maintenance Kit Doc 065031 04 1 08 357 ICS 3000 lon Chromatography System 358 Doc 065031 04 1 08 Symbols Offset analog out 82 5V output DC 79 84 Numerics 10 port valve DC 50 74 See also High pressure valves
231. nnel Audit Trail Error Messages The Moduleware the instrument control firmware installed in each ICS 3000 module periodically checks the status of certain parameters If a problem is detected it is reported to Chromeleon or Chromeleon Xpress and logged in the Audit Trail Each error message is preceded by an icon that identifies the seriousness of the underlying problem see the table below For most modules except for the TC you can change the severity level assigned to a problem whenever appropriate Icon Default Description Severity Level 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 065031 04 1 08 169 ICS 3000 lon Chromatography System 8 1 1 DP SP Error Messages The table below lists the most frequently observed DP SP related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table DP SP Related Audit Trail Error Message Default Severity See
232. not light 208 Troubleshooting system wide 169 High background 187 Low detector output 186 Noisy baseline 178 Retention times too early 183 Retention times too late 183 Tailing peaks 185 Troubleshooting TC Alarm conditions TC 227 Alarm LED is lighted 253 Liquid leaks 253 Temperature does not increase 254 Temperature stabilizer not operating 255 TTL and relay connectors DC 49 79 Installation instructions 80 TTL inputs DC 49 Control types 88 Functions available 86 TTL outputs DC 49 Controlling 84 TTL Relay control DC Control panel 84 DC relay output configuration 84 Operating failure 201 Tubing Replacing DC 297 Replacing DP SP 257 Replacing EG 281 Replacing TC 327 U Upper compartment DC Description 44 Temperature control 46 Temperature specifications 342 Upper oven LED 41 USB cables DC 48 DP SP 28 EG 37 Reordering DC 355 Reordering DP SP 350 Reordering EG 351 Reordering TC 357 TC 97 USB connections DC 48 Doc 065031 04 1 08 Index 17 ICS 3000 lon Chromatography System DP SP 28 EG 211 TC 97 V Vacuum degassing module 21 336 Daily maintenance 161 On off control 21 Specifications 336 Vacuum is low 201 VALVE buttons DC 42 Enabling disabling 42 145 Troubleshooting 222 Valve LEDs DC LED is flashing 42 LED is lighted 42 Valve LEDs TC LED is flashing 91 253 LED is lighted 91 Valves See Type o
233. ns DC 48 USB connections DP SP 28 USB connections EG 37 USB connections TC 97 User s guide 10 Virtual Column Separation Simulator 149 Cinch connector Pin assignments 27 Column clips Reordering 357 Column ID chip card 94 101 Reordering 357 Slots for installation 94 Column ID system 101 Chip card readers 94 Installing a chip card 329 Selecting a column 328 Selecting column properties 329 Column open circuit 214 Column oven 46 Column over safe temperature 214 Column properties Primary 101 243 248 Secondary 101 Selecting for column ID system 329 Columns Sizes available 45 Specifications 342 Commands AS Autosampler control 144 AS40 Automated Sampler control 144 Creating a program 147 Remote inject device control 145 Commands dialog box 54 127 Compartment open circuit 214 Compartment over safe temperature 215 Concentrator column 51 99 Condensation 165 Conductivity Detector CD 2 4 Air bubble removal 312 Cell calibration 308 Cell description 53 Doc 065031 04 1 08 Index 3 ICS 3000 lon Chromatography System Cell temperature control 54 Description 53 Effect of temperature on conductivity 54 Leaking 222 Replacement procedure 311 Specifications 344 Configuration drawings 105 112 Connected LED DC LED is lighted 41 Connected LED DP SP LED is lighted 18 Connected LED EG LED is lighted 31 Connected LED TC LED is lighted 91 Control panel 146
234. ns are so low that dilution is not necessary Use eluent or ASTM Type I 18 megohm cm filtered and deionized water to dilute the sample When using carbonate eluents diluting with eluent minimizes the effect of the water dip at the beginning of the chromatogram If you dilute the sample with eluent also use eluent from the same lot to prepare the calibration standards This is most important for fluoride and chloride which elute near the water dip To improve the accuracy of early eluting peak determinations such as fluoride at concentrations below 50 ppb dilute samples in eluent or spike the samples with concentrated eluent to minimize the water dip For example spike a 100 mL sample with 1 0 mL of a 100 X eluent concentrate Fill the Autosampler Vials and Load the Sample Tray 1 Follow the instructions in the autosampler manual to fill the vials and load them into the sample tray or cassette The autosampler manuals are included on the Dionex Reference Library CD ROM P N 053891 2 Load the tray or cassette into the autosampler and close the autosampler door Tips for Filling and Loading Vials e Foran AS fill the vials no higher than the vial shoulder Make sure the needle vent is not immersed in liquid during sampling e For an AS40 fill the vials to the level marked on the vials 120 Doc 065031 04 1 08 4 Startup Install a cap on each vial For an AS make sure the septum is pushed fully into the cap
235. nsumables Storage The columns and other consumable items used with an ICS 3000 system have various short and long term storage requirements Refer to the manuals for the individual products for instructions These manuals are provided on the Dionex Reference Library CD ROM P N 053891 Short term Shutdown Before a TC shutdown of less than one week no special procedure is required Long term Shutdown Before interrupting TC operation for more than one week or before shipping the TC rinse the fluid connections with deionized water Doc 065031 04 1 08 157 ICS 3000 lon Chromatography System 158 Doc 065031 04 1 08 7 Maintenance This section describes routine maintenance procedures for the ICS 3000 system that users may perform All other maintenance procedures must be performed by Dionex personnel For information about maintenance procedures for the EluGen cartridge CR TC trap column or suppressor refer to the appropriate product manual These manuals are included on the Dionex Reference Library CD ROM P N 053891 7 1 System Maintenance Checklists 7 1 1 Daily Maintenance O Check for leaks O Wipe up liquid spills O Check eluent reservoir levels and refill as needed O Check eluent reservoirs for microbial growth clean reservoirs and replace eluent as needed O Check waste containers and empty as needed For detailed daily maintenance instructions for each module see DP SP page 161 EG page
236. nt open circuit This error may indicate a problem in the detector electronics Contact Dionex for assistance Compartment over safe temperature This error occurs when the temperature of the DC lower compartment is higher than the maximum allowed This error may occur if the ICS 3000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Section A 12 for environmental specifications ED cell 1 option disconnected Or ED cell 2 option disconnected This error indicates that the electrochemical detector is unplugged To troubleshoot 1 Check the detector connections Verify that the signal cable from the cell is connected to the appropriate connector on the detector block see Figure 8 4 Also push firmly on the detector to ensure the electronics connector on the back of the detector is securely connected to the receptacle on the detector compartment Doc 065031 04 1 08 215 ICS 3000 lon Chromatography System Push here to ensure the detector s electrical connection is secure Figure 8 4 Electrochemical Detector Connection 2 Ifthe error appears again contact Dionex for assistance The detector electronics may have malfunctioned NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user ED cell 1 working electrode disconnected Or ED cell 2 working el
237. ntial changes is repeated over time By repeatedly pulsing between high positive and negative potentials the electrode surface is continually regenerated Current is measured by integration during a portion of the repeating potential vs time waveform See Section 2 16 6 for more information about waveforms Pulsed Amperometric Detection In pulsed amperometric detection also known as PAD current is integrated at a single constant potential see Figure 2 24 0 7 Integration Potential Volts 0 1 0 1 0 0 0 2 0 4 0 6 E1 Analytical Potential Time Seconds E2 Cleaning Potential Ei E2 ES E3 Reconditioning Potential Figure 2 24 Example Pulsed Amperometry Waveform The potentials labeled E1 E2 and E3 are applied for durations t1 t2 and t3 respectively At tl the E1 potential is applied After a delay the signal is measured by integrating the current for a fixed time Current integrated for a fixed time is charge and the units are coulombs At t2 and t3 positive and negative cleaning pulses are added to the waveform This waveform period repeats until the end of data acquisition or until another waveform is specified Doc 065031 04 1 08 61 ICS 3000 lon Chromatography System Integrated Amperometric Detection With integrated amperometric detection also known as IA or IPAD current is integrated at two or more potentials see Figure 2 25 0 60 0 35 Pot
238. nuals provided on the Dionex Reference Library CD ROM P N 053891 4 1 Operating Precautions 4 1 1 EG Operating Precautions e The EluGen cartridge requires at least 14 MPa 2000 psi of system backpressure This ensures optimal removal of electrolysis gas from the eluent produced by the cartridge During system equilibration monitor the Current Pressure reading on the pump Control panel in Chromeleon or Chromeleon Xpress the pressure should remain between 14 and 21 MPa 2000 and 3000 psi If necessary increase the system backpressure by installing a backpressure coil between the injection valve and the ELUENT OUT port on the EluGen cartridge For instructions refer to Section 9 15 IMPORTANT The recommended maximum operating pressure for the EG is 21 MPa 3000 psi Excessive backpressure may rupture the tubing inside the RFIC Eluent Degasser Doc 065031 04 1 08 113 ICS 3000 lon Chromatography System CAUTION MISE EN GARDE VORSICHT DO NOT CAP THE WASTE CONTAINER The ICS 3000 Eluent Generator EG Atlas Electrolytic Suppressor and Self Regenerating Suppressor SRS use an electrolytic process that results in the production of small amounts of oxygen or hydrogen gas To ensure that the gas is not trapped in a closed container and allowed to concentrate install a 1 3 cm 0 52 in ID black gas separator waste tube P N 045460 in an uncapped waste container Connect the Waste Gas Separator line to the waste tube
239. nvironmental Operating Temperature Ambient Humidity Ambient A 13 Physical Dimensions Weight 4 to 40 C 40 to 104 F 5 to 95 relative humidity noncondensing Height 40 8 cm 16 in Width 44 cm 17 5 in Depth 54 9 cm 21 6 in 38 kg 84 Ib Doc 065031 04 1 08 341 ICS 3000 lon Chromatography System A 14 Lower Compartment Components Column Capacity 2 sets Column IDs 1 to 9 mm Column Lengths Up to 250 mm Injection Valves One or two 2 position electrically activated Rheodyne PEEK valves 6 port or 10 port A 15 Temperature Control A 15 1 Upper Compartment Temperature 15 to 40 C in 1 C increments thermo electric control Control Range Ifthe RCH 1 is off Minimum temperature 10 C below ambient If the RCH 1 is at 80 C or the CD cell is at 60 C Minimum temperature 5 C below ambient Temperature 0 5 C Accuracy Temperature 0 2 C Stability Temperature 0 2 C Precision Heat up lt 30 min from 20 to 40 C Cooldown Time lt 40 min from 40 to 20 C 342 Doc 065031 04 1 08 A DC Specifications A 15 2 Lower Compartment Optional Temperature Control Range Temperature Accuracy Temperature Stability Temperature Precision Heat up Cooldown Time 10 to 70 C in 1 C increments Minimum temperature gt ambient 15 C Maximum temperature gt ambient 50 C 0 5 C 0 2 C 0 2 C lt 30 min from 20 t
240. o 50 C lt 30 min from 50 to 20 C A 16 ICS 3000 Automation Manager A 16 1 RCH 1 Reaction Coil Heater Temperature Control Range Temperature Accuracy Temperature Stability Temperature Precision A 16 2 Valves High Pressure Low Pressure 5 C above the compartment temperature in 1 C increments maximum of 80 C 1 C 0 2 C 0 2 C Electrically activated Rheodyne PEEK valve 2 position 6 port or 2 position 10 port up to two valves can be installed 2 way or 3 way PEEK valve up to two valves can be installed Doc 065031 04 1 08 343 ICS 3000 lon Chromatography System A 17 ICS 3000 Conductivity Detector Electronics Detection Types Cell Drive Linearity Resolution Signal Sampling Rate Electronic Noise Dry Electronic Noise Wet Filter Temperature Compensation Cell Body Cell Electrodes Active Volume of Cell Cell Operating Temperature Cell Maximum Operating Pressure Signal Gain Ranges Optional Analog Output Full Scale Ranges Microprocessor controlled digital signal processing Single or dual conductivity detection Dual detection can be controlled either simultaneously or independently 8 kHz square wave 1 at 1000 uS 0 10 nS Maximum of 100 Hz S N ratio 200 000 1 Example 1000 uS 5 nS At 23 LS noise lt 0 2 nS At 1 uS noise lt 0 1 nS Rise times from 0 to 10 s Factory set at 1 7 per C programmable from 0
241. o more than fingertight Do not use any tools to tighten the priming valve Overtightening may destroy the cap seal Open or close the priming valve only when the system pressure is down e High pressure limit was tripped 1 Make sure that no tubing is plugged or overtightened To determine the source of the high backpressure isolate segments of the flow path a Remove the pump outlet tubing at the injection valve b Press the POWER button on the front of the DP SP to turn on the pump c Set the Flow rate to 1 0 mL min on the Chromeleon or Chromeleon Xpress Control panel and record the backpressure d One at a time reconnect each component of the flow path If reconnecting a component causes an abnormal increase in 198 Doc 065031 04 1 08 8 DP SP Troubleshooting backpressure replace the component Replace as many components as necessary to resume operation at the standard operating backpressure 2 As columns age their backpressure increases It may be necessary to compensate for this by increasing the high pressure limit If the column is the source of the high backpressure clean the column Refer to the column manual provided on the Dionex Reference Library CD ROM P N 053891 for instructions If this does not eliminate the problem replace the column 3 Observe a run to see whether the high pressure limit is triggered when sample is injected if it is the injection valve may be causing a blockage
242. ode DCAmp a CV Mode 050s Rise Time 0 50s Data Collection Rate 1 0Hz Step Auto DC Voltage 9 000V Working Cell On 2 Reference Electrode AgCI z Ref Electrode pH 10 0 116 Doc 065031 04 1 08 4 Startup To set amperometry cell pH limits You can set upper and lower pH limits in the Chromeleon or Chromeleon Xpress Program Wizard The Audit Trail displays an alarm if the limits are exceeded Program Wizard EDet1 Options RE e Tessin Tt lt New Waveform gt Description goes here NOTE To disable the alarm set the upper limit to 14 and the lower limit to 0 Doc 065031 04 1 08 117 ICS 3000 lon Chromatography System 4 2 System Startup Checklist O 0 O0 O0 g0 O oO O O Set up the eluent reservoirs see page 123 Set up the piston seal wash system see page 124 Start the pump see page 127 Set the pressure limits see page 130 If an EG is installed start the EG and set the eluent concentration see page 131 Start the DC see page 135 or TC see page 137 Equilibrate the system and verify operational readiness DC see page 136 TC see page 138 Prepare the samples see page 119 Fill the autosampler vials and load the sample tray see page 120 Notes If the system is controlled by Chromeleon you can use the SmartStartup Wizard to create a startup program and sequence SmartStart
243. og output when it is plotted 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 level does not affect the magnitude of the output signal Polarity Positive Negative Use this setting to set the polarity of the analog output signal to either positive the default or negative In applications in which the analyte output is lower than the background signal the polarity must be negative to display peaks instead of dips on the chromatogram Mark 10 of the full scale analog output Use this setting to send a positive pulse to the analog output as an event marker A mark is typically used to indicate a sample injection Table 2 2 Analog Output Configuration Settings Continued 82 Doc 065031 04 1 08 2 DC Description IcS 3000 Home Sequence Control Status Gradient Pumps Eluent Generator Detector Compartment Cond Detector System Log Audit Trail ICS 3000 server ei 0 43 46 AM User AMar from AMAR2 has acquired control over timebase 10 44 58 AM User AMar from AMAR has connected Server Configuration to this Conductivity Detector Settings _ CDet1 Autozero Signal Total Signal Calibration Rise Time 0 50s Data Collection Rate 5 0Hz Cell Heater Cell Heater Mode On x Cell Heater Set Point 35 00 C
244. ogramming flash memory Abort page 237 Executing this command will reset associated counter Warning page 237 values stored in the module Firmware download failed Abort page 237 Firmware download in progress Please wait Error page 237 174 Doc 065031 04 1 08 8 Troubleshooting TC Related Audit Trail Error Message Default Severity See Level Gas leak detected Error page 238 Humidity leak detected Error page 238 Illegal parameter Abort page 238 Invalid date time format Either use DD MMM YYYY or Error page 239 current Nyear s Nmonth s Nday s Examples 31 Dec 1999 current 1year 6months Invalid enumerated value Warning page 239 Next qualification of this module is due in x day s due Warning page 239 date is date Next qualification of this module is overdue due date Warning page 239 was date Next qualification of this module is overdue due date Error page 239 was date Module may no longer be used Next qualification of this module was due on date Warning page 239 Allowing x more grace day s Next service of this module is due in x day s due date is Warning page 240 date Next service of this module is overdue due date was Warning page 240 date No chip card in the reader for the column x Error page 241 No response from x for x seconds Warning page 241 No response from x for x secon
245. ohm cm filtered and deionized water and dry it with a lint free paper towel Inspect the piston for signs of damage If the piston is scratched or scored replace it see Section 9 6 Even minute scratches or particles of dust dirt etc on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance Removing the Main Piston Seal 1 If this is the primary pump head insert a 10 32 fitting plug P N 042772 into the 10 32 outlet hole of the check valve nut If this is the secondary pump head insert a 10 32 fitting plug P N 042772 into both the 10 32 inlet and outlet holes Using a 10 cc syringe P N 054578 inject a few drops of ASTM Type I 18 megohm cm filtered and deionized water through the main piston seal P N 064946 and into the piston cavity Reinsert the piston P N 062082 approximately 3 mm 0 125 in into the piston seal and press gently The seal should pop out of the head and onto the piston Do not use a sharp tool such as tweezers to remove the piston seal This will scratch the inside of the pump housing these scratches will prevent a proper seal and cause leakage 5 If the piston seal was not removed in Step 4 follow these steps a Verify that the 10 32 fitting plugs in the inlet and outlet holes are tightened enough to prevent any leaks from the pump head b Fill the piston cavity with water and check for bubbles c If there are no bubbles
246. ollow the instructions in Section 9 12 Step 4 through Step 9 to disconnect the EluGen cartridge electrical cable from the bulkhead connector cap the EluGen cartridge vent opening remove the EluGen cartridge and disconnect the inlet and outlet tubing Pull the CR TC off the ball studs on the component mounting panel Disconnect the liquid lines from the four ports on the CR TC 290 Doc 065031 04 1 08 9 EG Service 7 Twist the ring on the CR TC electrical cable counterclockwise to loosen it and then pull the cable straight out of the CR TC 1 or CR TC 2 bulkhead connector Remove the CR TC from the EG 9 13 2 Installing and Hydrating the New CR TC Always hydrate a new CR TC before initial operation This requires pumping ASTM Type I 18 megohm cm filtered and deionized water through the CR TC for 10 minutes while bypassing the analytical columns and the suppressor 1 Remove the plugs from the ports on the new CR TC CR ATC P N 060477 CR CTC P N 060478 2 Locate the CR TC Hydration Tubing Kit P N 063487 provided in the EG Ship Kit 3 Refer to Figure 9 18 to plumb the four ports on the CR TC for the hydration procedure Preplumbed to RFIC Eluent Degasser REGEN IN Port j Regen Out Port blue label CR TC From Pump Outlet gt a 1 4 in Fitting 10 32 Fitting CR TC Hydration Kit Tubing Assembly PIN 063487 Figure 9 18 CR TC Plumbing for Hydration 4 On the
247. omatography System A Gas leak detected This error occurs if the gas sensor detects an increased concentration of gas inside the TC To troubleshoot 1 Find and eliminate the leak 2 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation A Humidity leak detected This error occurs if the humidity sensor detects an increased concentration of humidity inside the TC To troubleshoot 1 Find and eliminate the leak 2 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation Illegal parameter This error occurs if you enter a parameter that is not valid for the TC To troubleshoot Select a valid parameter 238 Doc 065031 04 1 08 TC Troubleshooting Invalid date time format Either use DD MMM YYYY or A current Nyear s Nmonth s Nday s Examples 31 Dec 1999 current 1 year 6 months This error occurs if you enter the date associated with an event in an invalid format To troubleshoot Enter the date in the format specified in the message Invalid enumerated value This error occurs if you attempt to enter an invalid value for a property rather than selecting a value from the drop down list box in the Commands dialog box To troubleshoot Select a valid option from the dr
248. omatography System AS Autosampler AS The AS is a powerful full featured autosampler that precisely delivers from 1 0 to 99 9 uL in 0 1 uL increments or 100 to 1000 uL in 1 uL increments of sample to an injection valve The autosampler can operate in several modes Concentrate Sample is delivered to a single analytical system for trace analysis and matrix elimination a concentrator column is installed on the injection valve in place of a loop Simultaneous Sample is delivered to two analytical systems simultaneously a sample loop is installed on each injection valve Sample is delivered equally to the two systems 50 of the volume to each allowing two complete separate analyses to be performed with just one sample Sequential Sample is delivered to two analytical systems in sequence This allows on demand injection of two independent samples to two applications using one autosampler While the first system is being analyzed the second system is being prepped and loaded for sample analysis Sequential Concentrate Sample is delivered to two analytical systems in sequence a concentrator column is installed on the injection valve in place of a loop Reagent Prime available in Concentrate mode only Primes the lines with reagent For example implementing the Reagent Prime mode during the matrix elimination step ensures that the appropriate reagent is in line for matrix elimination and prevents cross contaminati
249. ompartiment thermique avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der TC abgek hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 9 25 Replacing Tubing and Fittings The TC is plumbed with the tubing and fittings listed below Tubing Size and Type Color P N Used For 0 125 mm 0 005 in ID PEEK Black 052310 Standard bore system connections 0 25 mm 0 010 in ID PEEK Red 052306 Microbore system connections 10 mm 0 39 in ID polyethylene Colorless 055075 Waste line Use double cone 10 32 ferrule fittings P N 043276 and 10 32 bolts P N 043275 for all tubing connections For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Dionex Reference Library CD ROM P N 053891 Use a tubing cutter to cut tubing to the required length Make sure the cut is at a right angle to the length of the tubing and there are no nicks or burrs on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 062614 dual P N 063408 single Refer to the instructions provided with the cutter Doc 065031 04 1 08 327 ICS 3000 lon Chromatography System 9 26 Setting Up the Column ID System The TC Ship Kit P N 064789 includes two column ID chip cards P N 5710 1500 The optional Column ID Kit P N 066353 in
250. ompensation Built in temperature compensation helps minimize changes in the baseline or in peak heights if the operating temperature is different from the temperature at which the cell was calibrated The default temperature compensation is 1 7 per C This can be reset to between 0 and 3 0 per C depending on the eluent If you notice that the baseline shifts up when the temperature increases the compensation factor is too low and should be reset to a higher value Follow these steps to change the temperature compensation factor 1 In Chromeleon or Chromeleon Xpress select Command on the Control menu or press the F8 key 2 Inthe Commands dialog box select the conductivity detector 3 Select the Temperature Compensation command and enter the desired value 4 Click Execute 54 Doc 065031 04 1 08 2 DC Description 2 15 2 Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions thereby increasing detection sensitivity The CD can operate with an AES SRS 300 SRS ULTRA II MMS 300 or MMS III suppressor The suppressor is installed below the cell on the CD see Figure 2 19 The suppressor cable plugs into the connector next to the detector on either the left or the right side depending on which side the CD is installed see Figure 2 20 Plug in the suppressor cable here Figure 2 20 Suppressor Connection Right Side Installation NOTE
251. on Valve Plumbing 6 Port Valve 7 Turn on the power to the DC 8 Turn on the pump flow Check for leaks from the valve Tighten fittings as required see Section 9 17 9 Close the door Doc 065031 04 1 08 301 ICS 3000 lon Chromatography System 9 20 Replacing a High Pressure Injection Valve Pod This procedure describes how to replace the mechanical parts the pod of a high pressure valve P N 061947 6 port P N 061948 10 port NOTE If the valve electronics require service contact Dionex Electronics related repair procedures must be performed by Dionex personnel NOTE Substitution of non Dionex parts may impair valve performance and void the product warranty 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump To avoid injury wait for the DC to cool down before opening the door or performing any maintenance or service procedures CAUTION Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 2 Open the DC door 3 Disconnect each liquid line connected to the valve 302 Doc 065031 04 1 08 9 e DC Service 4 Unscrew the black locking ring on the front of the valve se
252. on any head with a leak see Section 9 5 2 Check for leaks throughout the remainder of the system including the check valves injection valve and columns Tighten or replace fittings as needed e DP SP not primed Prime the pump see Section 9 3 e Liquid lines incompletely flushed after an eluent change Attach a 10 cc syringe P N 054578 to the waste port on the priming valve Open the priming valve turn the knob one half turn counterclockwise Draw at least 20 mL of the new eluent through the liquid lines before operation Doc 065031 04 1 08 181 ICS 3000 lon Chromatography System Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Dionex for assistance Inoperative check valves Replace the check valve cartridges see Section 9 4 Insufficient mixing gradient pump only The static mixer may be dirty or contaminated Flush with IPA isopropyl alcohol If this does not eliminate the problem install a new mixer GM 3 P N 042126 GM 4 P N 049135 Eluent is contaminated 1 Clean all eluent reservoirs thoroughly inside and out with ASTM Type I 18 megohm cm filtered and deionized water and dry with clean particulate free air If a reservoir still appears dirty or if there is a slimy film on the interior follow the cleaning instructions in Section 9 2 2 Flush the system with ASTM Type I 18 megohm cm filtered and deionized water
253. on between reagents Reagent Flush available in Concentrate mode only Flushes the concentrator column with reagent for example a known source of clean deionized water to remove unwanted sample matrix Doc 065031 04 1 08 1 Introduction AS40 Automated Sampler AS40 The AS40 is a low cost metal free sample loading device designed for ion chromatography applications The AS40 is capable of delivering between 0 2 and 5 0 mL of sample in set increments The AS40 holds between 66 and 88 vials depending upon the vial size in use 0 5 mL 5 0 mL or a combination of both sizes Up to three injections can be taken from each vial The AS40 holds up to 11 cassettes of six 5 mL vials or eight 0 5 mL vials Each sample is filtered during loading through a 20 um filter in the vial cap so there is no need to prefilter samples Samples can be loaded against backpressures up to 690 kPa 100 psi without an external sampling pump thus facilitating preconcentration work ICS Series Photodiode Array Detector PDA The PDA optical detector is capable of measuring the absorbance spectrum from 190 to 800 nm A deuterium lamp optimizes the UV range 190 to 380 nm and a tungsten lamp optimizes the visible range 380 to 800 nm The PDA enables you to collect up to five single wavelengths 2D chromatograms without being required to collect 3D data Collecting individual wavelengths instead of the spectra offers two advantages it elimi
254. on valve usage Reminders for service and qualification periods including display of warning messages when limits are approaching or overdue Predictive Performance commands and parameters are available in the Commands dialog box 104 Doc 065031 04 1 08 3 Configurations 3 1 Overview This chapter provides some example component and plumbing drawings for the following ICS 3000 system configurations ICS 3000 Configuration See IC System CD page 106 Reagent Free IC RFIC single system page 107 RFIC Dual System with two CDs page 108 RFIC Dual System with CD and ED page 109 RFIC with Matrix Elimination Using a DP and a 6 Port Valve page 110 RFIC with Matrix Elimination Using an SP and a 10 Port Valve page 111 RFIC with Post Column Reagent Addition Bromate page 112 Doc 065031 04 1 08 105 ICS 3000 lon Chromatography System To the pump inlet via the pump rear chase n Eluent DC front view Pump front view Seal pE E Piston Seal Wash To AS Waste l jejui dwing ae aa E ARE To waste Figure 3 1 IC System with CD 106 Doc 065031 04 1 08 3 Configurations Pump front view To the pump inlet via the pump rear chase SP A Wash Pump I E pump not to scale i P S f Piston E
255. ondensation inside the TC Condensation may build up when the TC is operated in a highly humid environment and the majority of applications are run at cold temperatures To remove condensation run the TC at its maximum temperature for at least 72 hours Some IC columns should not be operated at temperatures above 70 C 158 F Remove all columns from the TC before beginning the maintenance procedure above e Inspect the door seal for signs of damage A defective seal impairs the performance of the instrument If the seal is defective contact Dionex Technical Support 7 16 TC Annual Maintenance e Dionex recommends performing preventive maintenance annually A DC TC Preventive Maintenance Kit P N 061796 is available 168 Doc 065031 04 1 08 8 1 8 Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the ICS 3000 system 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 Dionex Technical Support In the U S call 1 800 346 6390 Outside the U S call the nearest Dionex office Please have this chapter at hand when talking with Technical Support perso
256. ons 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 change in anion concentration Pretreating Samples Analyze rainwater drinking water and air particulate leach solutions directly with no sample preparation other than filtering and if required diluting Filter groundwater and wastewater samples through 0 45 micron filters before injection unless samples were filtered after collection A Dionex High Pressure Inline Filter P N 044105 is available for removing particulates down to 0 45 micron from samples Connect the inline filter between the autosampler outlet and the sample inlet port on the injection valve For details see the instructions provided with the inline filter Doc 065031 04 1 08 119 ICS 3000 lon Chromatography System 4 3 3 4 3 4 Before injection pretreat samples that may contain high concentrations of interfering substances by putting them through Dionex OnGuard cartridges Refer to the installation and troubleshooting guide for the OnGuard cartridge for instructions The guide is located on the Dionex Reference Library CD ROM P N 053891 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 concentratio
257. op down list box available for this property Next qualification of this module is due in x day s due date is date or Next qualification of this module is overdue due date was date or Next qualification of this module was due on date Allowing x more grace day s or Next qualification of this module is overdue due date was date Module may no longer be used gt Chromeleon and Chromeleon Xpress monitor the date on which qualification was last performed and display an appropriate message shown above at the following times when the due date for the next qualification is approaching when the due date is overdue but the TC can still be used and when the due date is overdue and the TC can no longer be used Doc 065031 04 1 08 239 ICS 3000 lon Chromatography System The Qualification WarningPeriod property determines the number of days before the due date that the warning is first displayed The Qualification GracePeriod property determines for how many days after the due date you can continue using the TC without performing the qualification To troubleshoot Contact Dionex to schedule an Operational Qualification and Performance Qualification Next service of this module is due in x day s due date is date Or Next service of this module is overdue due date was date Chromeleon and Chromeleon Xpress monitor the date on which service was last performed and
258. or over power 220 Suppressor over voltage 220 Index 6 Doc 065031 04 1 08 Index Upper leak sensor wet 221 Error messages DP SP 189 196 Abnormal drive current 189 Camshaft index too early 189 Camshaft index too late 189 Camshaft sensor always alight 190 Camshaft sensor missing or dark 190 Degasser malfunction 190 Excessive drive current 190 Function cannot be adjusted by user 196 Invalid flow value 191 Leak detected 191 Maximum purge pressure exceeded 194 Motor malfunction 192 Motor position error 192 Pressure fallen below lower limit 193 Pressure in working cylinder exceeded safety limit 194 Program with this name already exists 189 Pump block carryover pressure too high 192 Rear seal leak count exceeded limit 195 Rear seal leak sensor malfunctioning 196 Rear seal wash system out of wash solution 193 Relay 4 configured for inject synchronization 194 System pressure exceeded safety limit 194 Upper pressure limit exceeded 196 Error messages EG 203 207 CR TC over current 203 CR TC stopped due to zero flow 203 EG cartridge disconnected 204 EG invalid concentration 204 EG invalid flow 205 EG invalid flow rate concentration 205 EG over current 205 EG over power 206 EG over voltage 206 Leak sensor wet 207 Error messages TC AcqOff with previous AcqOn 227 Acquisition still on at program end 227 All samples must specify same value
259. ost cases Reference Electrode Calibration Procedure 1 Complete the following if you are calibrating an existing electrode a Turn off the cell voltage from the Control panel in Chromeleon or Chromeleon Xpress b Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump Disconnect the cell see Section 9 24 1 d Unscrew the reference electrode and remove it from the cell body e Rinse the reference electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water to remove any precipitated salt 2 With the reference electrode removed from the cell connect the electrical cables to the cell and electrode 3 Click the EC Detector tab in Chromeleon Xpress or on the panel tabset in Chromeleon 322 Doc 065031 04 1 08 9 e DC Service 4 Click the Calibration button under Electrochemical Detector Settings The Wellness panel opens see Figure 9 38 Z Electrochemical Detector Wellness By xi PH Electrode Calibration Current and Previous Values Press for instructions Instructions Current pH Electrode Offset 0 00 10 00 Current pH Electrode Slope 59 17 Current pH Reading pH 7 Offset Calibration Offset Cal Current Calibration Date 411912006 pH Slope Buffer Value 10 00 z Previous pH Electrode Offset 0 00 pH Slope Calibration Slope Cal Previous pH Electrode Slope 59 17 Previous Calibration Date 41191200
260. ower door opened This message occurs when the door to the lower compartment is opened during a run To troubleshoot 1 2 3 Verify that the door is fully closed Check for and remove any obstruction If the door is fully closed and the error persists contact Dionex for assistance Lower leak sensor wet The leak sensor is installed in the drip tray at the bottom of the column compartment see Figure 9 21 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 Tighten fittings or replace tubing and fittings as required Refer to Section 8 26 for detailed troubleshooting of various types of leaks After fixing the leak dry the drip tray thoroughly to prevent the leak sensor from triggering additional error messages 218 Doc 065031 04 1 08 8 DC Troubleshooting Reaction coil open circuit This error occurs when the reaction coil heater is unplugged from the DC To troubleshoot 1 Check that the reaction coil heater is correctly plugged into the component panel 2 If the error persists the heater may be faulty Replace the heater P N 061746 Reaction coil over safe temperature This error occurs when the temperature of the DC upper compartment is higher than the maximum allowed This error may occur if the ICS 3000 Ion Ch
261. panel Status Bar Secondary Pump Head Priming Valve Pressure Transducer Primary Pump Head Peristaltic Pump for seal wash system Vacuum Degas Chamber one channel Eluent Supply On Off Valve Tubing Chase Pump 2 Handle Piston Seal Wash Reservoir Vacuum Degas Chambers four channels Static Mixer Proportioning Valve Fittings Tubing Chase Pump 1 69666 86606009 O0O6006 Leak Sensor Figure 2 3 DP SP Interior Components DP Shown Doc 065031 04 1 08 19 ICS 3000 lon Chromatography System 2 2 1 2 2 2 2 2 3 Pump Heads The DP SP is a zero pulsation serial dual piston pump with electronic compressibility compensation Two pump heads a primary head and a secondary head are connected in series Eluent passes through both pump heads in succession The primary pump head delivers eluent at the selected flow rate while simultaneously filling the secondary pump head The latter serves as a reservoir and delivers eluent while the primary head carries out the refill stroke The characteristic feature of the patented isokinetic pre compression phase is the programmed overlapping of the delivery strokes of the two pump heads When delivering compressible liquids without controlled pre compression the pulsation increases as the operating pressure increases since part of the delivery stroke is required to compress eluent in the pump head During the pre compression phase pulsation
262. perature specifications 343 Lower oven LED 41 Low pressure valves 49 Controlling 76 External valve outputs DC 49 Flow schematic 75 Installed in AM 73 Reordering 353 Luer adapter fitting Reordering 353 M Main power receptacle DC 48 DP SP 25 EG 38 TC 95 Main power switch DC 48 DP SP 25 EG 38 TC 95 Index 10 Doc 065031 04 1 08 Index Maintenance annual DC 166 168 DP 162 EG 163 SP 162 TC 168 357 Maintenance daily DC 165 167 DP SP 161 EG 163 TC 167 Maintenance periodic DP SP 162 TC 168 Maintenance weekly DC 165 DP SP 161 EG 163 TC 167 Manual sample processing 139 Manuals for ICS 3000 system 10 11 Mark analog output 82 Matrix elimination 44 73 System configuration 110 111 Methanesulfonic acid eluent 34 Methanol 58 MicroMembrane Suppressor MMS 45 55 See also Suppressor Mixer static 22 Mobile phases See Eluents Moduleware 169 MSQ Plus Mass Spectrometer 3 8 N Needle seal assembly AS 297 Nitrite in samples 119 Noisy baseline 178 Normal edge TTL input control DC 89 Normal pulse TTL input control DC 89 O Offset percentage analog out 82 Offsetting background conductivity 136 Open circuit 219 Operating temperature DC 341 DP SP 335 EG 339 TC 347 Operation Automatic sample processing 147 Creating a sequence 148 Example program 144 Filling vials 118 120 Loading samples 140 Manual sample pro
263. plugs into the IEC 320 three prong receptacle Doc 065031 04 1 08 95 ICS 3000 lon Chromatography System The power supply cord is used as the main disconnect device Make sure the socket outlet is located near the TC and is easily accessible CAUTION 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 Digital I O Connectors The two 6 pin mini DIN connectors can be used to exchange digital signals with any external device capable of being controlled through a relay or TTL input The two connectors are identical in function Relay_Com Relay_N O Digital Input Digital_GND Not Used Not Used N O Normally open contact Figure 2 54 Digital I O Connector When the relay is activated the connection is between Com and N O Digital Input lt gt Digital GND 0to 5 V Relay_Com lt gt Relay_N O Switching voltage 100 VDC Switching current 0 25 A Carry current 1 0 A Switching capacity 3 W Contact resistance Max 150 megohms 96 Doc 065031 04 1 08 TC Description Use the 6 pin mini DIN signal cable P N 6000 1004 provided in the TC Ship Kit P N 064789 to
264. pplication that uses a concentrator column NOTE Other plumbing configurations for the 10 port valve are possible depending on the components to be connected to the valve and the application to be run Refer to the appropriate Dionex Application Note for more information Sample In LOAD POSITION INJECT POSITION Loop Loading Concentrator Loading Concentrator Concentrator To Column Eluent Pump In Se wae To Waste lt v c 3 T 5 RS OUT Loop 7 te To Waste an 7 L4 10 Carrier Pump In Sample In Carrier Pump In To Waste To Waste Sample sussses Carrier Eluent Figure 2 17 Injection Valve Flow Schematics 10 Port Valve Example Connections Large Loop to Concentrator Liquid flows through either the Load or Inject path depending on the valve position For the example shown in Figure 2 17 the flow occurs as follows e In the Load position sample flows from the syringe or autosampler line through the valve and into the sample loop Excess sample flows out to waste Eluent flows from the eluent pump through the valve through the concentrator column and to the separator column If sample was previously loaded onto the concentrator column it is swept to the separator column for analysis Doc 065031 04 1 08 51 ICS 3000 lon Chromatography System e In the Inject position carrier liquid flows through the sample loop and on
265. problem 255 Thermal Compartment TC 2 4 Alarm LED is lighted 91 Digital I O connectors 96 Dimensions 347 Electrical specifications 347 Front description 91 Fuse requirements 347 Injection valve specifications 348 Maintenance 167 168 Moduleware update 230 Operating humidity 347 Operating temperature 347 Oven LED is flashing 92 Oven LED is lighted 92 Power requirements 347 Rebuilding the injection valve 330 Regulator Bracket Kit 30 Index 16 Doc 065031 04 1 08 Index Replacing the injection valve Pod 331 Service procedures 327 Shutdown procedure 157 Signal cable 97 357 Specifications 347 Theory of operation 103 Weight 347 Trap column 5 Tray autosampler Loading 118 120 Triangle waveform 63 Troubleshooting DC Alarm conditions DC 213 Amperometry cell 223 Error messages DC 213 227 Liquid leaks DC 221 pH readout always at 7 0 223 pH readout cannot be set to 7 0 224 pH readout nonexistent 225 Reference electrode leaks 225 Reference potential shifts 226 VALVE button not working 222 Troubleshooting DP SP Chromatographic reproducibility 181 Digital I O port not operating 201 Leak alarm 199 Liquid leaks 199 Pump does not start 197 Pump stops unexpectedly 198 Vacuum degassing module low vacuum 201 Troubleshooting EG Alarm LED is lighted 207 EG stops operation 210 Error messages 203 Leaking fittings 207 Liquid leaks 208 No flow 209 Power LED does
266. product warranty 1 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump Doc 065031 04 1 08 331 ICS 3000 lon Chromatography System To avoid injury wait for the TC to cool down before opening the door or performing any maintenance or service procedures CAUTION Afin d viter toute br lure laisser refroidir le compartiment thermique avant d ouvrir la porte ou d effectuer des op rations de maintenance MISE EN GARDE Um Verletzungen zu vermeiden warten Sie bitte bis der TC abgek hlt ist ehe Sie die T r ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 2 Open the TC door 3 Disconnect each liquid line connected to the valve 4 Unscrew the black locking ring on the front of the valve see Figure 9 46 and remove the ring 5 Grasp the front of the valve pod and pull out firmly to remove it from the TC Figure 9 46 Unscrewing the Locking Ring Black Locking Ring 6 Check that the new pod P N 061961 6 port P N 061962 10 port has the correct number of ports for the injection valve being serviced 7 Align the slots in the new pod with the runner in the valve holder in the TC see Figure 9 47 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 332 Doc 065031 04 1 08 TC Service
267. pump head NOTE The inlet check valve assembly housing has a 1 4 28 port the outlet check valve assembly housing has a smaller 10 32 port see Figure 9 3 Doc 065031 04 1 08 263 ICS 3000 lon Chromatography System 10 Inspect the new inlet check valve assembly P N 045722 to verify that Inlet Check Valve Outlet Check Valve the double hole end of the cartridge MA ee Ron Wes see Figure 9 3 is visible If the double hole end is not visible remove the cartridge from the housing and install it correctly ne Se 11 Inspect the new outlet check valve assembly P N 045721 to verify that the single hole end of the cartridge is visible see Figure 9 3 If the single hole end is not visible Check remove the cartridge from the housing and install it correctly Outlet Figure 9 3 Check Valve Assemblies NOTE The pump cannot operate properly unless the cartridges are installed in their respective housings in the correct orientation Liquid enters through the check valve in the large single hole and exits through the small double holes 12 Install the inlet check valve assembly on the bottom of the primary pump head Install the outlet check valve assembly on the top of the pump head NOTE The opening for the outlet check valve assembly is slightly closer to the back of the pump head than the opening for the inlet check valve assembly 13 Tighten the check valves fingertight and then use the 1 2 in
268. r s electrical connection is secure Figure 8 1 Conductivity Detector Connection ED Verify that the signal cables from the cell are connected to the detector block see Figure 8 2 In addition an electronics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the detector to make certain the connector is securely connected Push here to ensure that the detector s electrical connection is secure Figure 8 2 Electrochemical Detector Connection 184 Doc 065031 04 1 08 8 Troubleshooting ED Only e Cellis off Turn on the cell from the Control panel in Chromeleon or Chromeleon Xpress 8 7 Tailing Peaks e Excess tubing void volumes Check tubing connections for void volumes e CD Long tubing lengths connecting Minimize all tubing lengths between the injection valve and the detector e DC Amperometry and Integrated Amperometry modes Dirty or pitted conventional nondisposable working electrode Clean the working electrode with water and dry with pressurized air or nitrogen Polish the working electrode see Section 9 24 3 If you are using a disposable electrode replace it 8 8 Low System Backpressure e Loose fitting Make sure there are no liquid leaks in the flow system Check tubing connections throughout the system including the check valves injection valves and columns and tighten or replace fittings as needed e RF
269. r The PEEK yoke knob ensures constant pressure is applied to the cell Orient the cell assembly with the PEEK yoke knob on the left and push the cell onto its mounting location in the DC compartment Reconnect the cell s inlet and outlet lines Reconnect the electrical cables Start the pump flow Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 316 Doc 065031 04 1 08 9 e DC Service 9 24 3 Polishing an Amperometry Cell Working Electrode These instructions are for conventional nondisposable working electrodes only Do not polish disposable electrodes When to Polish the Working Electrode Polish carbohydrate gold platinum silver and glassy carbon working electrodes before initial installation in the amperometry cell Do not polish new AAA gold electrodes before installation After the working electrode is polished and installed background signal and analyte sensitivity require several hours to stabilize Once stabilized do not polish the electrode unless you observe a loss of signal or severe electrode recession Items Needed Polishing kit P N 036313 shipped with the electrode The kit contains polishing pads P N 036321 a bottle of fine polishing compound P N 036318 and a bottle of coarse polishing compound P N 036319 Pen that writes with indelible ink Gloves Tweezers Working Electrode Polishing Procedure NOTE To avoid electrode fouling
270. r occurs if there is a communication failure between the TC and the PC on which Chromeleon or Chromeleon Xpress is installed To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 Ifyou cannot identify the cause of the error contact Dionex for assistance Doc 065031 04 1 08 245 ICS 3000 lon Chromatography System The compartment door is open a batch or a program may need to wait until the door has been closed Please close the door This error occurs if you attempt to operate the TC when the door is open or not fully closed To troubleshoot 1 Verify that the door is fully closed 2 Ifthe door is not fully closed check for and remove any obstruction 3 Ifthe door is fully closed but the error persists contact Dionex for assistance The counter name value x has exceeded its limit y Module should no longer be used Replace the name This error occurs if the number of hours a TC part has been in use exceeds the lifetime set by the OperationTime Limit property To troubleshoot Replace the part identified in the message before resuming operation The data format stored on the chip card is unsupported format version x This error occurs if the column ID chip card data is inadvertently saved in an invalid format To troubleshoot 1 Inthe Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to displ
271. raphy System Specifications AM 343 CD 344 DC 341 ED 345 Lower compartment DC 343 RCH 1 343 TC 347 Upper compartment DC 342 Start up procedures DC 135 DP SP 123 EG 131 Equilibrate the system 136 138 Offsetting the background 136 TC 137 Static mixer 182 See also GM 3 Gradient Mixer Status bar DC 41 LEDs described 41 91 Status bar DP SP LEDs described 18 Status bar EG LEDs described 32 Status bar TC LEDs described 91 Sulfite in samples 119 Suppressor Description 55 Leaking 222 Reordering 354 Replacement procedure 309 Types supported 45 Suppressor alarms Suppressor open circuit 220 Suppressor over current 219 Suppressor over power 220 Suppressor over voltage 220 Suppressor LEDs DC LED is lighted 41 Switched AC sockets DC 48 Syringe Reordering 353 Syringe injection 141 Vacuum 143 System configuration drawings 105 112 IC system 106 Matrix elimination 110 111 RFIC dual CD and ED system 109 RFIC dual CD system 108 RFIC single system 107 RFIC with post column reagent addition 112 System Wellness 104 T TC VWD PDA Regulator Bracket Kit 30 Technical Support 169 257 Temperature control CD 53 Minimizing the effect of variations 54 Temperature compensation 54 Temperature control DC 46 Cell heater 54 Specifications 342 Temperature control TC 94 103 Specifications 348 Temperature stabilizer TC 4 94 Liquid leaks 254 Operating
272. rds with an invalid Error page 245 data structure The communication interface is closed Reconnect the Error page 245 instrument The compartment door is open a batch or a program Warning page 246 may need to wait until the door has been closed Please close the door The counter name value x has exceeded its limit y Warning page 246 Module should no longer be used Replace the name The data format stored on the chip card is unsupported Error page 246 format version x The injections limit for the column has been exceeded Warning page 247 The injections limit will be exceeded for the column x Warning page 247 The nominal temperature must be set within the current Error page 247 limits The nominal temperature value is out of range defined by Error page 247 the active column ID The oven is not fully operable yet Check the values of Error page 248 Standby Ready Door and CardState The primary column ID property x will be changed The Warning page 248 property can t be changed in the future 176 Doc 065031 04 1 08 8 Troubleshooting TC Related Audit Trail Error Message Default Severity See Level The upper limit must be higher than the lower limit Error page 249 The Warning threshold must be higher than the Limit Error page 249 threshold The Warning threshold must
273. rloaded This error occurs if the pump motor is overloaded To troubleshoot 1 One or more tubing connections may be plugged or blocked Check all tubing connections and replace as needed see Section 9 1 2 Ifthe Upper pressure limit exceeded message is also displayed refer to page 196 for additional troubleshooting steps 192 Doc 065031 04 1 08 8 DP SP Troubleshooting Pressure fallen below lower limit This error occurs if the DP SP pressure falls below the low pressure limit specified in Chromeleon or Chromeleon Xpress To troubleshoot 1 2 The eluent supply may be depleted Refill any empty eluent reservoirs Check all eluent lines for air bubbles If air is trapped in a line replace the end line filter P N 045987 See Section 4 4 for instructions Verify that the end of each filter extends to the bottom of the reservoir and is submerged in eluent Prime the pump see Section 9 3 Eluents may be insufficiently degassed Check the vacuum degassing module Check all tubing connections for leaks tighten loose fitting connections A check valve may be defective Replace the check valve cartridges see Section 9 4 and then prime the pump see Section 9 3 Rear seal wash system has run out of wash solution This error occurs only when the cap on the seal wash reservoir is equipped with a drop sensor and the sensor does not detect any wash solution when piston seal washing is activat
274. rmal element For detailed instructions refer to the JCS 3000 Ion Chromatography System Installation Instructions Document No 065032 e TC calibration is incorrect The TC cannot be calibrated by the user Contact Dionex for assistance e Defective temperature stabilizer Replace the temperature stabilizer standard bore P N 064548 microbore P N 064650 Doc 065031 04 1 08 255 ICS 3000 lon Chromatography System 256 Doc 065031 04 1 08 9 Service This chapter describes ICS 3000 Ion Chromatography System service and repair procedures that users may perform All procedures not included here including electronics related repair procedures must be performed by Dionex personnel For assistance contact Dionex Technical Support In the U S call 1 800 346 6390 Outside the U S call the nearest Dionex office Before replacing any part refer to the troubleshooting information in Chapter 8 to correctly identify the cause of the problem Substituting non Dionex parts may impair a module s performance IMPORTANT thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information DP SP Service 9 1 Replacing Tubing and Fittings The DP SP is plumbed with the tubing and fittings listed below Tubing Size and Type 0 25 mm 0 010 in ID PEEK 0 51 mm 0 020 in ID PEEK 13 cm 5 in 1 02 mm 0 040 in ID PEEK 13 cm 5 in 0 159 cm 0 0625
275. rning value selected for a Predictive Performance command for example LeftRotorSealSwitches is lower than the Limit value Chromeleon or Chromeleon Xpress issues a warning message in the Audit Trail when the Warning value is reached and an error message when the Limit value is reached To troubleshoot Select a Warning value that is higher than the Limit value A The Warning threshold must be lower than the Limit threshold This error occurs if the Warning value selected for a parameter is higher than the Limit value Chromeleon or Chromeleon Xpress issues a warning message in the Audit Trail when the Warning value is reached and an error message when the Limit value is reached To troubleshoot Select a Warning value that is lower than the Limit value Doc 065031 04 1 08 249 ICS 3000 lon Chromatography System There was already an AcqOff command for this channel before Or There was already an AcqOn command for this channel before Or Two AcqOn commands for the same channel The second chromatogram will overwrite the first A Chromeleon or Chromeleon Xpress program can include no more than one command to start or terminate data acquisition for a channel if multiple commands are present the appropriate message shown above appears To troubleshoot Remove the duplicate commands from the program This function cannot be adjusted by the user This error occurs if you attempt to change the setting for
276. romatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Section A 12 for environmental specifications Suppressor 1 over current Or Suppressor 2 over current This error may be caused by a depleted or dirty suppressor or by a malfunction in the suppressor controller electronics To troubleshoot 1 Follow the instructions in the suppressor manual to regenerate the suppressor Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 2 Follow the instructions in the suppressor manual to clean the suppressor Doc 065031 04 1 08 219 ICS 3000 lon Chromatography System 3 If you suspect a malfunction in the suppressor controller contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user Suppressor 1 over power Or Suppressor 2 over power This error appears when in order to maintain the selected current the ICS 3000 Ion Chromatography System is required to apply a higher voltage than the suppressor can support To troubleshoot 1 Reduce the flow rate 2 Rehydrate the suppressor Refer to the suppressor manual for instructions Suppressor manuals are included on the Dionex Reference Library CD ROM P N 053891 3 Ifthe error persists replace the suppressor see Section 9 23 2 Suppressor 1 over voltage Or Suppres
277. ror contact Dionex for assistance 232 Doc 065031 04 1 08 TC Troubleshooting A Configuration doesn t match X not installed Or Configuration mismatch x CM uses y Column Compartment uses z Please use the Server Configuration program to check the installation This error occurs if there is a discrepancy between the TC properties and the actual configuration To troubleshoot 1 Start the Server Configuration program 2 Inthe timebase right click the TC and select Properties on the context menu 3 Correct any discrepancies in the Properties dialog box Current flow is out of limits defined for the column This error occurs if the current flow rate exceeds the value specified by the Column_x FlowRate_UpperLimit command To troubleshoot Select a valid flow rate Current pressure is out of limits defined for the column This error occurs if the current pressure reading is outside the range specified by the Column_x Pressure_UpperLimit and Column_x Pressure_ LowerLimit commands To troubleshoot Find and eliminate any liquid leaks or blockages in tubing connections see Section 8 31 Adjust the flow rate accordingly Doc 065031 04 1 08 233 ICS 3000 lon Chromatography System Current temperature is out of limits defined for the column This error occurs if the current temperature reading is outside the range specified by the Column_x Temp_UpperLimit and Column _x Temp_
278. rs if the column ID chip card is installed incorrectly or is defective To troubleshoot When the chip card is properly installed the Dionex logo on the card faces up and the LED on the memory slot is green If this error occurs when the chip card is properly installed it indicates that the card is defective and should be replaced for instructions refer to Section 9 26 236 Doc 065031 04 1 08 TC Troubleshooting Error programming flash memory This error occurs if during a firmware Moduleware download the new firmware cannot be programmed into memory To troubleshoot Flash memory cannot be serviced by the user Contact Dionex for assistance Executing this command will reset associated counter values stored in the module This error occurs when you select a command RotorSealChanged for example that updates information stored in the TC To prevent information from being inadvertently changed Chromeleon or Chromeleon Xpress requests confirmation before executing the command To troubleshoot If you want to execute this command click Execute otherwise click Cancel A Firmware download in progress Please wait This error occurs if you attempt to issue a command while firmware Moduleware is being downloaded to the TC To troubleshoot Wait until the firmware download is complete Audit Trail messages will inform you of the status of the download Doc 065031 04 1 08 237 ICS 3000 lon Chr
279. rtment Doc 065031 04 1 08 31 ICS 3000 lon Chromatography System Button LED Label If the LED Is On Comment POWER Use this POWER button for routine on off control of the EG When the power is on this LED is lighted To turn off the EG press and hold this POWER button for 2 seconds The main power switch is on the EG rear panel NOTE The EG status bar LEDs do not flash 32 Doc 065031 04 1 08 2 EG Description 2 8 EG Interior Components Figure 2 8 shows the EG component compartment which is located directly behind the front door The component mounting panel divides the compartment into two sections In a single channel EG components are installed in the left section only To access components for maintenance or service procedures push down on the slide release latch and pull the tray forward until it reaches the stop EluGen Cartridge RFIC Eluent Degasser Electrical Connectors CR TC Waste Line SYSTEM i Drip Tray 0000000 Slide Release Latch d Mi Ye a uf i c gt NT o Figure 2 8 EG Interior Components Second Right Side Channel of a Dual System EG Shown Doc 065031 04 1 08 33 ICS 3000 lon Chromatography System EluGen Cartridge Several types of EluGen cartridges are available for use with the EG see the table below Each cartridge contains 900 mL of the appropriate ele
280. ry and secondary pump heads on pump see Figure 4 1 Connect this tubing to the pump heads on pump 2 When you finish these connections go to the next section to continue setting up the seal wash system 124 Doc 065031 04 1 08 4 DP SP Startup Seal Wash Reservoir Outlet Line Connection between pump heads Connection from peristaltic pump to secondary pump head Seal Wash Reservoir Inlet Line Figure 4 1 Piston Seal Wash Connections to Pump 1 Setting Up the Seal Wash System All pumps 1 Add ASTM Type I 18 megohm cm filtered and deionized water to the seal wash reservoir P N 064155 The liquid level should be between the Min and Max markers on the reservoir label Do not overfill the reservoir 2 Place the cap on the reservoir and tighten fingertight 3 Insert the reservoir into the holder on the component panel 4 Check that the tubing is engaged in the peristaltic pump see Figure 4 2 If it is not lift the lever on the peristaltic pump up and to the right insert the tubing neatly between the lever and the rotor and release the lever to secure the tubing Doc 065031 04 1 08 125 ICS 3000 lon Chromatography System Tubing to Secondary Pump Head Outlet Tubing from Seal Wash Reservoir Figure 4 2 Peristaltic Pump 5 Ifa seal wash reservoir with a drop sensor cap is installed connect the outlet line from the reservoir cap to the secondary pump he
281. s can be either two ICS 3000 Conductivity Detectors CDs two ICS 3000 Electrochemical Detectors EDs or one detector of each type See Section 2 15 for details about the CD and Section 2 16 for details about the ED 44 Doc 065031 04 1 08 2 DC Description Suppressors for conductivity detection are installed in this compartment also The following types of suppressors can be used e SRS Self Regenerating Suppressor SRS 300 or ULTRA II 2 and 4 mm e AES Atlas Electrolytic Suppressor e MMS MicroMembrane Suppressor MMS 300 or MMS II Lower Compartment The lower compartment can hold up to two column sets four columns with IDs of 1 mm to 9 mm and lengths of 100 mm to 250 mm The lower compartment also holds one or two injection valves Two valve versions 6 port and 10 port are available Both versions are electrically activated two position valves See Section 2 14 for details about the injection valves The compartment tray slides forward about 10 cm 4 in for easy access to columns and valves To pull the tray forward use the handle installed in the center of the compartment see Figure 2 14 Handle for pulling tray forward Figure 2 14 DC Side View with Lower Compartment Tray Pulled Out Doc 065031 04 1 08 45 ICS 3000 lon Chromatography System Temperature Control The following temperature control zones are possible with the DC depending on the options installed
282. s needed see Section 9 1 2 As columns age their backpressure increases It may be necessary to compensate for this by increasing the high pressure limit If the column is the source of the high backpressure clean the column Refer to the column manual provided on the Dionex Reference Library CD ROM P N 053891 for instructions If this does not eliminate the problem replace the column 3 Observe a run to see whether the high pressure limit is triggered when injection occurs if it is the injection valve may be the source of the 196 Doc 065031 04 1 08 8 DP SP Troubleshooting blockage 1 e the rotor seal or stator may need to be replaced Contact Dionex for assistance 8 13 DP SP Does Not Start e Power is off Check that the main power switch on the DP SP rear panel is turned on Press the POWER button on the front of the DP SP to turn on the pump e Flow rate is set to zero Select a Flow rate on the Chromeleon or Chromeleon Xpress Control panel e While being primed pump starts briefly and an alarm sounds If the high pressure limit was tripped check that the priming valve on the secondary pump head is opened see Figure 2 3 To open the valve turn the knob one half turn counterclockwise If the low pressure limit was tripped 1 Verify that the Minimum Pressure setting is several hundred psi below the Current Pressure reading on the Chromeleon or Chromeleon Xpress Control panel 2 Make sure there
283. s not allow data to be saved If you are using Chromeleon data from manual processing is saved in the manual sequence folder in the timebase folder of the local datasource This data is overwritten each time a new manual sample is processed To save the data from a manual run 1 Select the manual folder and select Save As from the File menu 2 Enter a new name for the sequence and select the Save raw data check box 3 Click Save 5 6 Automatic Batch Sample Processing You can use Chromeleon or Chromeleon Xpress to create a list of samples a sequence to be processed automatically e For each sample the sequence includes a program with commands and parameters for controlling ICS 3000 modules and acquiring sample data To create a program click Create Program on the Sequence Control panel e Ifyou are using Chromeleon the sequence also includes a quantification method for peak identification and area determination To create a quantification method select New on the File menu and select Method File from the list e You can also enter additional sample processing parameters in the sequence for example the sample name sample type injection volume etc After creating the sequence you can start batch processing Doc 065031 04 1 08 147 ICS 3000 lon Chromatography System 5 6 1 Creating a New Sequence Two wizards are available to help you create a new sequence Sequence Wizard and Application Wizard e I
284. s the tab in and then up to Tab release the fuse drawer Pull the fuse drawer out of the rear panel and remove the old fuses Replace the two fuses with new 2A IEC 60127 2 slow blow fuses P N 954773 Dionex recommends always replacing both fuses Figure 9 20 EG Fuse Drawer Insert the fuse drawer into the rear panel and press until the drawer snaps into place Reconnect the main power cord and turn on the power 296 Doc 065031 04 1 08 DC Service 9 17 Replacing Tubing and Fittings The DC is plumbed with the tubing and fittings listed below PEEK Tubing Size and Type Color P N Used For 0 75 mm 0 030 in ID Green 044777 Connection from injection PEEK valve to waste AS needle seal assembly Pink 057301 AS normal and concentrate 46 cm 18 in with 10 32 modes only Connection from ferrule fitting the injection valve to the AS inject port 0 33 mm 0 013 in ID Light 049714 AS sequential modes only PEEK Blue Connection from injection valves to AS diverter valve 0 51 mm 0 020 in ID Orange 042855 AS simultaneous mode only PEEK Connection from each injection valve to the AS simultaneous injection tee 1 58 mm 0 062 in ID Colorless 014157 Connection from REGEN OUT Teflon port on the suppressor 0 125 mm 0 005 in ID Red 044221 Microbore systems PEEK Connections between other system components 0 25 mm 0 010 in ID Black 042690 St
285. sample loop Loading sample with a syringe through the sample loading port on the front of the DC push method Loading sample with a vacuum syringe through the sample loading port on the front of the DC pull method NOTE For instructions on how to load and inject samples with an autosampler see Section 5 2 140 Doc 065031 04 1 08 5 Operation 5 3 1 Loading Samples with a Syringe Push Method Connecting a Sample Loading Port to the Injection Valve 1 For each sample loading port to be connected locate the following items in the DC Ship Kit P N 062614 dual P N 063408 single One 1 4 28 fitting P N 052230 and ferrule P N 052231 One 10 32 fitting P N 062980 and ferrule P N 062978 0 75 mm 0 030 in ID green PEEK tubing P N 052304 One luer adapter fitting P N 024305 2 Press the metal release tab under the sample loading port on the front of the DC see Figure 5 3 and pull the port out the front of the DC Figure 5 3 Sample Loading Ports and Release Tabs Doc 065031 04 1 08 141 ICS 3000 lon Chromatography System 3 Remove the fitting plug from the rear of the port 4 Cuta length of green 0 75 mm 0 030 in ID PEEK tubing The tubing will be used to connect the sample loading port and the sample port on the valve 5 Attach a 1 4 28 fitting and ferrule to one end of this tubing and connect it to the rear of the sample loading port see Figure 5 4 1 4 28 Fi
286. se of the error contact Dionex for assistance Doc 065031 04 1 08 241 ICS 3000 lon Chromatography System Operating columns above 70 C could affect column performance Verify recommended column operating conditions before setting temperature above 70 C This error occurs if you select a TC temperature setting above 70 C 158 F To troubleshoot Refer to the column manual for the recommended operating conditions Column manuals are provided on the Dionex Reference Library CD ROM P N 053891 Parameter x value exceeded its allowed range Set to closest valid value x or Value for name parameter is not within valid range Value passed x will be substituted by y or Value x replaced by valid table entry y If you select a value outside the allowable range for certain parameters Chromeleon ignores the setting replaces it with the closest valid setting and this error occurs To troubleshoot No immediate action is required In future specify a valid setting for the parameter 242 Doc 065031 04 1 08 TC Troubleshooting Primary property x is already assigned and cannot be changed This error occurs if you attempt to change one of the primary column properties batch or lot number date of manufacture etc used for column identification To troubleshoot Once a primary column property has been assigned it cannot be changed As an alternative consider ch
287. see Section 5 3 2 or autosampler see Section 5 2 2 On the Sequence Control panel click Acq On 3 On the Detector Control panel click Autozero 4 The signal plot is displayed on the Detector Control panel see Figure 5 6 Monitor the chromatogram and when sample data has been collected click Acq Off ICS 3000_2 gt k Home Sequence Control Status Gradient Pump Detector Compart Cond Detector 1 System Log Audit Trai I 12 55 41 PM 0 500 Pump_1 60 2 55 41 PM 0 500 CDet1 Log Background 0 0 uS 22 55 11 PM 0 000 CDet1 Autozero 2 55 11 PM 0 000 CD_1 AcqOn 92 55 11 PM 0 000 CD_1_TotalAcqOn Log Pressure 0 0 psi Serial Rise Tim Total Signal 0 0174S Data Collection Rate 5 0 Hz Conductivity Detector Settings Sup Calibration pressor Settings Analog Out Type None bd Range A Mode Off M Full Scale 1 2 Signal P OmA 2 Current Offset Level Calculate Current Polarity Negative e 0 505 z 69 7 Cell Heater Cell Heater Mode Cell Heater Set Point Cell Heater Temp Cell Heater Status 40 0 00 C 2 Ea 35 00 C Moo At_setpoint Figure manual 5 Manual Acquisition from Pos CD_1_Total 0 017 CD 1 2 00 3 00 4 00 5 6 Manual Data Acquisition 146 Doc 065031 04 1 08 5 Operation 5 5 1 Saving Manual Data NOTE Chromeleon Xpress doe
288. sired settings on the detector Control panel see Figure 2 46 Analog Output Setting Values Description Full scale voltage 0 01 0 10 or 1 00 V Sets the voltage output of a full scale detector response The voltage to use depends on the recording device to which the analog output is connected For example if the analog output is connected to a device that accepts input voltages up to V select a full scale voltage output of 1 V Range Conductivity Sets the full scale detector response 0 01 to 15 000 uS value The range to use depends on DC Amperometry the detector readings expected for the 50 pA to 300 uA application For example selecting a range of 20 microSiemens uS will limit you to viewing conductivity readings of 20 uS or less Integrated Amperometry 50 pC to 200 uC Table 2 2 Analog Output Configuration Settings Doc 065031 04 1 08 81 ICS 3000 lon Chromatography System Analog Output Setting Values Description Recorder calibration Zero Full Scale Normal Use this setting to calibrate a recording device Select Zero to set the output signal to zero volts Select Full Scale to set the output signal to the selected full scale voltage 0 01 0 10 or 1 00 V For normal operation select Normal the default to output a signal corresponding to the detector output Offset level 0 to 100 Use this setting to adjust the zero position of the anal
289. sis Eluent flows from the pump through the sample loop and on to the column carrying the contents of the sample loop with it Section 5 2 describes how to inject samples The 10 port injection valve has two operating positions 10 1 and 1 2 Liquid flows through the path between either ports 10 and 1 or ports 1 and 2 depending on the valve position Figure 2 56 shows example flow schematics for the 10 port valve when it is connected for an application that uses a concentrator column 10_1 POSITION 1_2 POSITION Loop Loading Concentrator Loading Concentrator Concentrator To Column Eluent Pump In To Column Eluent Pump In A e ee ss To Waste a a io Sample In Carrier Pump In Sample In Carrier Pump In To Waste To Waste Sample sssssss Carrier Eluent Figure 2 56 TC Injection Valve Flow Schematics 10 Port Valve Example Connections Large Loop to Concentrator e Inthe 10 1 position sample flows from the syringe or autosampler line through the valve and into the sample loop Excess sample flows out to waste Eluent flows from the eluent pump through the valve through the concentrator column and to the separator column If sample was previously loaded onto the concentrator column it is swept to the separator column for analysis e Inthe 1 2 position carrier liquid flows through the sample loop and on to the concentrator column carrying the contents
290. sor 2 over voltage This error appears if you turn on the suppressor and the system cannot establish a connection with the suppressor To troubleshoot 1 Check the suppressor cable connection 2 Ifthe error persists replace the suppressor see Section 9 23 2 220 Doc 065031 04 1 08 8 DC Troubleshooting Suppressor 1 open circuit Or Suppressor 2 open circuit To troubleshoot 1 Verify that the suppressor cable is connected correctly Upper door opened This message occurs when the door to the upper compartment is opened during a run To troubleshoot 1 Verify that the door is fully closed 2 Check for and remove any obstruction 3 Ifthe door is fully closed and the error persists contact Dionex for assistance 8 26 Liquid Leaks from DC Components Leaking fitting Locate the source of the leak Tighten or if necessary replace the liquid line connection see Section 9 17 Broken liquid line Replace the line and fittings with the same length and internal diameter tubing see Section 9 17 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 DC If a line is blocked replace it see Section 9 17 Doc 065031 04 1 08 221 ICS 3000 lon Chromatography System e Leaking injection valve 1 Make sure the liquid line connections to
291. source and also from the rear panel of the DC DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du DC DANGER HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des DC ACHTUNG 4 Onthe DC rear panel remove the two screws that attach the I O option cover plate or the existing I O option board to the rear panel see Figure 9 26 Save the screws Remove two screws Figure 9 26 DC Rear Panel Removing the I O Option Cover Plate Doc 065031 04 1 08 305 ICS 3000 lon Chromatography System 5 Slide the new I O option board P N 062201 into the rear panel opening and press firmly to connect the board to the DC motherboard 6 Replace the two screws Figure 9 27 shows the I O option installed am ST oe QUE TANNIN ge Bow s I O Option Figure 9 27 DC Rear Panel I O Option Installed 7 Reconnect the main power cord and turn on the power 306 Doc 065031 04 1 08 9 e DC Service 9 22 Changing the DC Main Power Fuses 1 Press the POWER button on the front of the DC for 2 seconds to turn off the power 2 Turn off the main power switch on the DC rear panel see Figure 2 15 3 Disconnect the main power cord from both its source and from the DC rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the DC
292. t gravement endommager l instrument mais qui n entra nera pas de blessures Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr Mi amp achtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gef hrdung MiRachtung kann zum Tod oder schwerwiegenden Verletzungen f hren Bedeutet eine m gliche Gef hrdung MiRachtung kann zu kleineren oder mittelschweren Verletzungen f hren Wird auch verwendet wenn eine Situation zu schweren Sch den am Ger t f hren kann jedoch keine Verletzungsgefahr besteht Doc 065031 04 1 08 13 ICS 3000 lon Chromatography System 1 4 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 Safety and Regulatory Information The ICS 3000 system is designed for IC ion chromatography and HPLC high performance liquid chromatography applications and should not be used for any other purpose Operation of an ICS 3000 module in a manner not specified by Dionex may result in personal injury 1 4 1 Safety Labels The TUV GS C US Mark safety label and the CE Mark label on the ICS 3000 modules indicate that they are in compliance with the following standards EMC Susceptibility and Immunity e DC EG DP SP EN 61326 1997 including A1 1998 and
293. t ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the DC lower door 298 Doc 065031 04 1 08 9 e DC Service 4 Loosen the screw on the front of the leak sensor P N 062437 see Figure 9 21 Note The screw remains attached to the sensor Figure 9 21 Leak Sensor 5 Pull out the leak sensor from the component panel and continue pulling until the attached cable is also out of the opening Disconnect 6 The cable attached to the leak maples sensor connects to a cable inside the DC Continue pulling the cable until the connectors for the two cables are outside the panel see Figure 9 22 7 Disconnect the two cables Figure 9 22 Leak Sensor Cable 8 Connect the cable from the new leak sensor to the DC cable 9 Feed the cables back inside the DC Align the leak sensor with the component panel opening and fingertighten the screw 10 Make sure the leak sensor does not touch the bottom of the drip tray Doc 065031 04 1 08 299 ICS 3000 lon Chromatography System 9 19 Rebuilding a High Pressure Injection Valve Dionex recommends rebuilding the injection valve annually The Injection Valve Rebuild Kit P N 057896 6 port valve P N 061759 10 port valve contains all required replacement parts This procedure also applies to high pressure valves installed in an ICS 3000 Automation Manager NOTE Substitution of non Dionex
294. t select the check box of one or more functions to be controlled by this input When connected to a controlling device the device can send a signal to the input to trigger the selected functions 6 By default several functions are selected Scroll down the list and disable all unwanted functions TTL Input Control Types Normal Edge The DC TTL inputs respond to four types of signals to Normal Pulse accommodate different controlling devices The default Inverted Edge control type Normal Edge is compatible with the output Inverted Pulse signals provided by Dionex modules If the device connected to the DC 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 determine the 88 Doc 065031 04 1 08 2 DC Description correct type Select the input control type in the Device Configuration dialog box for each TTL input see Figure 2 50 e Normal Edge In normal edge Action Off or No Effect operation the negative falling ER edge of a signal turns on the suit function EDGE 9 y The action of the positive Action On rising edge depends on the function For on off or other functions that have two options the rising edge turns off the function However for functions with only one option the rising edge has no effect For example for the injection valve position the falling edge switches
295. t Severity See Level Can t use device x as a source of the column pressure Error page 231 Please check the property y for a valid device name The device must have the Pressure property available Card data checksum error Error page 231 Command is not available in demo mode Abort page 232 Communication error x Abort page 232 Communication time out Abort page 232 Configuration doesn t match X not installed Warning page 233 Configuration mismatch x CM uses y Column Abort page 233 Compartment uses z Please use the Server Configuration program to check the installation Current flow is out of limits defined for the column Warning page 233 Current pressure is out of limits defined for the column Warning page 233 Current temperature is out of limits defined for the Warning page 234 column Data buffer overrun Abort page 234 Device control feature is not available Please check key Abort page 234 code and CM Features see About Chromeleon in the client s Help menu Device is not remote Abort page 235 Device not found on the USB Abort page 235 Either the current date is later than the expiration date for Warning page 236 x or the program or batch will end later than 24 hours before the expiration time for y Error deleting flash memory Abort page 236 Error during storing of the card data to the chip card Error page 236 Error finishing download Abort page 230 Error pr
296. t of the TC 2 To display the TC Control panel select the TC tab see Figure 4 6 System_1 Sequence Control Status Gradient Pump TC M Column Details Figure 4 6 TC Control Panel 3 Click the Oven on button and set the temperature required for the application Doc 065031 04 1 08 137 ICS 3000 lon Chromatography System 4 11 Equilibrate the System and Verify Operational Readiness NOTE Sample preparation can be performed while the system is equilibrating 1 Onthe Chromeleon or Chromeleon Xpress Control panel verify that the TC temperature is at its set point and is stable 2 Monitor the pump pressure make sure it is at the expected reading for the installed column and is stable The system is now ready for operation 138 Doc 065031 04 1 08 5 Operation 5 1 Overview Samples can be run manually one at a time or else grouped in batches and run automatically Figure 5 1 compares the typical steps performed in manual and batch sample processing Manual Sample Batch Sample Processing Processing Load the sample Create a program 4 Start data Create a sequence acquisition J J Jl Load the C Autozero sequence Inject the sample C Start the batch Includes commands Stop data for sample loading acquisition autozero injection and data acquisition Figure 5 1 Samp
297. t view Reagent in A from pump 2 A H To pump 1 inlet A via the pump rear chase To 3 way valve 1 COM Pot via the DC rear chase Pump 2 J pump not to scale gt Deionized To the Pump 1 Water absorbance or PDA detector rear chase EG left side view Separator Backpressure Device To AS Waste To Waste Mixer Pump front view DP pan O wesn Pump lt lt g und amp fonott CE d 4u To waste Mixer Piston Seal Wash Valve a ll El Oc 1 E 10 95 D Ge 1 y ua To waste RFIC Eluent Degasser Regen Regen Out In Figure 3 7 RFIC with Post Column Reagent Addition Bromate 112 Doc 065031 04 1 08 4 Startup This section is an overview of the steps required to start up the ICS 3000 system components and prepare the system to run samples The operating parameters flow rate compartment temperature suppressor current etc depend on the application you plan to run Refer to the column manual as well as the schematics in Chapter 3 of this manual for the required operating parameters NOTE Before beginning operation be sure to perform any special startup procedures required for the columns suppressors etc Startup procedures are described in the quick start guides and ma
298. talled in the DC and set the desired temperatures e Compartment temperature control e Column temperature control e Reaction coil heater e Conductivity detector cell heater select the Cond Detector tab Doc 065031 04 1 08 135 ICS 3000 lon Chromatography System 4 9 Equilibrate the System and Verify Operational Readiness NOTE Sample preparation can be performed while the system is equilibrating 1 On the Chromeleon or Chromeleon Xpress Control panel view the detector signal and monitor the background Refer to the column manual for the appropriate background for your application The column manuals are included on the Dionex Reference Library CD ROM P N 053891 2 Offset the background and zero the reading by clicking the Autozero button 3 Verify that the detector baseline is at the expected reading for your application and is stable See Section 8 11 for troubleshooting information if the reading is too high See Section 8 2 for troubleshooting information if the baseline is drifting or is excessively noisy there are large fluctuations in readings 4 Verify that all installed temperature control devices are at their set points and are stable 5 Monitor the DP SP pressure and make sure it is at the expected reading for the installed column and it is stable The system is now ready for operation 136 Doc 065031 04 1 08 H TC Startup 4 10 Start the TC 1 Press the POWER button on the fron
299. talled in the upper compartment of the DC see Figure 2 13 The detector electronics are not accessible to the user Conductivity Cell a DIONEX CONDUCTIVITY DETECTOR 4 ut Suppressor Optional h Pe rare DION Ex shown ASRS TR Figure 2 19 Conductivity Detector with Suppressor 2 15 1 Heated Conductivity Cell The DC 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 lt 1 pL and low dispersion Temperature control and compensation help ensure good peak reproducibility and baseline stability Doc 065031 04 1 08 53 ICS 3000 lon Chromatography System 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 To reduce the effect of temperature variation the DC provides temperature control of both the DC compartment and the cell A heater inside the cell regulates the cell temperature The cell heater temperature range is from a low of 5 C above the temperature of the middle and upper compartment to a high of 60 C Temperature C
300. tance 8 5 Peak Retention Times Are Too Late e Eluent concentration setting is too low The correct eluent concentration setting depends on several factors the flow rate EluGen cartridge type etc Refer to Section 4 7 for a list of valid concentration ranges for the cartridges and then edit the program as required e DP SP flow rate is too high Decrease the DP SP flow rate e Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Dionex for assistance 8 6 No Peaks e KG power is not turned on 1 Check that the POWER button on the front of the EG is turned on 2 Check that the EG main power switch on the rear panel is turned on 3 Check that the main power cord is plugged into both the EG rear panel connector and the power source Check that the wall outlet has power Doc 065031 04 1 08 183 ICS 3000 lon Chromatography System e Injection valve is not actuating or the sample loop is plugged 1 Test the valve by manually switching the position from the Detector Chromatography tab on the panel tabset 2 Check the sample loop for blockage Clean or replace the loop if needed e Detector not properly installed CD An electronics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the detector to make certain the connector is securely connected see Figure 8 1 Push here to ensure that the detecto
301. tch Sample Processing 147 5 6 1 Creating a New Sequence 148 5 6 2 Starting Batch Sample Processing 149 Doc 065031 04 1 08 Vv ICS 3000 lon Chromatography System 6 Shutdown DP SP Shutdown EG Shutdown 6 1 Short term Shutdown 153 6 2 Long term Shutdown 153 DC Shutdown 6 3 Consumables Storage 155 6 4 Amperometry Cell Storage 155 6 4 1 Short term Storage of the Amperometry Cell 155 6 42 Long term Storage of the Amperometry Cell 155 TC Shutdown 6 5 Consumables Storage 157 6 6 Short term Shutdown 157 6 7 Long term Shutdown 157 7 Maintenance 7 1 System Maintenance Checklists 159 7 1 1 Daily Maintenance 159 7 1 2 Weekly Maintenance 159 7 1 3 Periodic Maintenance 160 7 1 4 Annual Maintenance 160 DP SP Routine Maintenance 7 2 DP SP Daily Maintenance 161 vi Doc 065031 04 1 08 Contents 7 3 DP SP Weekly Maintenance
302. tch on the rear panel is turned on 210 Doc 065031 04 1 08 8 EG Troubleshooting 3 Check that the main power cord is plugged into both the EG rear panel connector and the power source Check that the wall outlet has power Check the USB connections The EG should be connected to the DP SP or other ICS 3000 module via a USB cable P N 960777 In addition one module in the system must be connected to the PC on which Chromeleon or Chromeleon Xpress is installed Check that the EG is configured in Chromeleon or Chromeleon Xpress and is assigned to a timebase Doc 065031 04 1 08 211 ICS 3000 lon Chromatography System 212 Doc 065031 04 1 08 4 DC Troubleshooting 8 25 Troubleshooting DC Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon or Chromeleon Xpress Audit Trail CD cell 1 option disconnected Or CD cell 1 option disconnected This error occurs when the conductivity cell is disconnected To troubleshoot 1 Check the detector connection An electronics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the upper part of the detector see Figure 8 3 to make certain the connector is securely connected 2 Ifthe error persists there may be a problem in the detector electronics Contact Dionex for assistance NOTE The ICS 3000 Ion Chromatography System electronics componen
303. tdown If the ICS 3000 Dual Pump DP or ICS 3000 Single Pump SP will not be operated for a period of one week or more follow the instructions below e Fill the pump with methanol or a similar alcohol such as 2 propanol or ethanol If the eluents in the pump are not miscible with water replace the eluents step by step e Fill the seal wash reservoir with wash solution see Section 2 2 5 e Rinse out buffers This will reduce the time required for column equilibration when you resume operation e Disconnect the tubing from the peristaltic pump on the component panel lift the lever up and to the right remove the tubing and release the lever see Figure 6 1 Figure 6 1 Peristaltic Pump for Seal Wash System Doc 065031 04 1 08 151 ICS 3000 lon Chromatography System Before shipping the pump e Empty the seal wash reservoir e Disconnect the tubing from the peristaltic pump on the component panel press the lever to the right remove the tubing and release the lever see Figure 6 1 152 Doc 065031 04 1 08 EG Shutdown 6 1 Short term Shutdown If the shutdown is for 3 months or less follow the instructions below To prepare the EG for the shutdown 1 Turn off the EG including all consumables installed in the EG the CR TC suppressor etc 2 Verify that the current to the EluGen cartridge and the suppressor is off Supplying power to the EluGen cartridge when there is no eluent f
304. the POWER button on the front of the TC to turn off the power after 30 seconds press the button again to turn on the power 3 Try to toggle the injection valve from Load to Inject by clicking the Load and Inject buttons on the Control panel 4 Ifthe error occurs again contact Dionex for assistance Doc 065031 04 1 08 251 ICS 3000 lon Chromatography System You do not have the privilege to approve the module s qualification You do not have the privilege to change the performance limits You do not have the privilege to change the qualification intervals In controlled environments users are not allowed to perform certain operations unless they have been granted the appropriate privileges If you attempt to do so the appropriate message shown above is displayed To troubleshoot The Chromeleon administrator assigns various privileges to individual users or to user groups Contact the administrator if you need one or more of the above privileges assigned to you 252 Doc 065031 04 1 08 TC Troubleshooting 8 30 TC ALARM LED Is Lighted If the ALARM LED lights red check the Chromeleon or Chromeleon Xpress Audit Trail for the cause e Gas leak inside the TC 1 Find and eliminate the leak 2 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Humidity leak inside the TC 1 Find and eliminate the l
305. the ambient temperature changes during the analysis increased heating or cooling ensures that the column temperature remains constant Operating IC columns at temperatures above 70 C 158 F may affect column performance Before selecting the TC temperature refer to the column manual for the recommended operating conditions Column manuals are provided on the Dionex Reference Library CD ROM P N 053891 The thermo optimized design of the TC reduces the time required to equilibrate the temperature between the column and the eluent Peltier elements in the TC heat up and cool down the columns They also help to bring the air and all of the installed components including the injection valves to the desired temperature If necessary a temperature stabilizer standard bore P N 064548 microbore P N 064650 can be installed in the TC Installation of a temperature stabilizer ensures that e The stationary phase temperature remains constant over the total column length e The column and the eluent have the same temperature during the analysis Under these conditions the separation is performed at the nominal temperature This minimizes fronting and tailing of peaks as well as retention time variations The temperature achieved may vary from the control range depending on the ambient temperature see the table below Control Range Achieved Temperatures Based on Ambient 5 to 85 C Minimum temperature 18 C below ambi
306. ther auxiliary device The connector includes three TTL inputs and four relay outputs Table 2 1 indicates the functions assigned to the connector pins For instructions on connecting the pump to an AS40 refer to the JCS 3000 Ion Chromatography System Installation Instructions Document No 065032 The manual is included on the Dionex Reference Library CD ROM P N 053891 IMPORTANT The maximum switching voltage of the relays is 24 V The switching current must not exceed 100 mA Pin Number Signal Name Signal Level Description Poe Not used 2 en Not used 3 Relay 3 Out Potential free Normally open 4 Relay 1 Out Potential free Normally closed 5 Relay 2 Out Potential free Normally closed 6 Relay 3 Out Potential free Normally closed Table 2 1 25 Pin D Sub I O Port Female 26 Doc 065031 04 1 08 2 DP SP Description Pin Number 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 Signal Name Relay 1 Out Relay 2 Out Gnd Gnd Gnd Gnd Relay 4 Out Relay 4 Out Relay 4 Out Relay 3 Out Relay 1 Out Relay 2 Out Vcc Out TTL Input 1 TTL Input 2 TTL Input 3 Analog Pressure Output Signal Level Potential free Potential free Ground Ground Ground Ground Potential free Potential free Potential free Potential free Potential free Potential free 5V TTL TTL TTL Description Common Common Ground Ground Ground Ground Not used Normally open Common Normally closed Not used
307. tion 353 Replacing 320 Shutdown procedure 155 Reference potential shift 59 226 Regulator Bracket Kit TC VWD PDA 30 Regulator Kit EO 30 Relay connectors DC 49 79 80 Configuring 84 Relay outputs DC 49 Controlling 85 Remote inject device 145 Reordering information DC 353 DP SP 349 EG 351 TC 357 Reprocessing amperometry data 68 Reproducibility Affected by amperometry cell pH 59 Affected by temperature changes 54 Reproducibility is poor 181 Reservoirs eluent 29 Cleaning 178 182 258 Installation in EO 5 30 Retention time Troubleshooting 183 Variations 94 Reversed phase solvents 58 RFIC Eluent Degasser 34 39 Leaks 207 209 Pressure requirements 113 Replacing 294 Tubing rupture 113 185 209 Waste line 36 Running samples 139 See also Sample processing S Safety icons 29 Safety messages 12 29 Salt crystals preventing 163 Sample loading With a syringe 142 143 With an autosampler 140 Sample loading ports 43 Sample loop DC Injecting 50 52 Injection valve connections 52 Loading 50 51 140 143 Reordering 353 Sample loop TC Injecting 99 Injection valve connections 100 Loading 98 99 Reordering 357 Sample processing 139 146 147 Automatically batch 147 Manual 146 With Chromeleon Chromeleon Xpress 146 Sample tray Loading 118 120 See Tray Samples Collecting and storing 119 Diluting 120 Filtering 119 Loading 140 143 14
308. tment of the DC see Figure 2 13 Connections to other components in the system pump injection valve reagent reservoirs etc depend on the application Refer to Chapter 3 for the configuration schematic for your application Low Pressure Low Pressure Temperature Valve 1 Valve 2 Stabilizer RCH 1 Reaction as Coil Heater High Pressure High Pressure lh Valve 1 Valve 2 Figure 2 37 ICS 3000 Automation Manager The AM is available in the following configurations Components Included AM Part Number Two 10 port high pressure valves 061738 Two low pressure 3 way valves One 10 port high pressure valve 061736 One low pressure 3 way valve One 6 port high pressure valve 061740 One low pressure 3 way valve AM tray with no valves 061734 Doc 065031 04 1 08 73 ICS 3000 lon Chromatography System In addition to the configurations described above you can order the following components separately for installation on an AM AM Component Part Number High pressure valve 6 port 061961 High pressure valve 10 port 061962 Low pressure valve 3 way 061971 Low pressure valve 2 way 061745 RCH 1 Reaction Coil Heater 061746 Temperature stabilizer standard bore 0 25 mm 0 010 in ID 062561 Temperature stabilizer microbore 0 125 mm 0 005 in ID 062562 2 17 1 High Pressure Switching Valves Up to two high pressure switching valves can be installe
309. to the concentrator column carrying the contents of the sample loop with it Excess flows out to waste Eluent flows from the pump through the valve and to the separator column bypassing the concentrator column 2 14 2 Injection Valve Plumbing Figure 2 18 shows the injection valve connections for the 6 port valve The injection valve is plumbed at the factory with all tubing and fittings for connection to the pump sample loading port column and waste A 10 uL PEEK sample loop P N 042949 is installed between ports L 1 and L 4 Dionex offers sample loops in various sizes If needed the pre installed 10 uL loop can be replaced with a loop that has a different sample injection volume SAMPLE IN from door inject port or autosampler 10 uL x SAMPLE LOOP Black Bee 30 c TO INJ Red microbore i w 2 VALVE C Black standard bore TO INJ Lo 4 VALVE W TO INJECT VALVE ai Green Figure 2 18 Injection Valve Plumbing 6 Port Valve 52 Doc 065031 04 1 08 2 DC Description 2 15 CD Conductivity Detector One or two ICS 3000 Conductivity Detectors CDs can be installed in the DC Each CD consists of a heated conductivity cell and the electronics required for collecting the conductivity data and sending it to the computer and the analog output if installed A suppressor optional can be installed on the clips on the lower part of the CD The cell and suppressor are ins
310. torage or disposal of the EluGen cartridge Verify that a 10 32 plug is installed in the EluGen cartridge vent opening This will prevent leakage from the vent opening when you turn over the cartridge Turn the cartridge upside down and place it on the EG drip tray in the service position see Figure 9 14 286 Doc 065031 04 1 08 9 EG Service 4 Remove the 10 32 plugs from the INLET and OUTLET fittings on the eluent generation chamber see Figure 9 15 Locate the yellow 0 5 mL min 7 MPa 1000 psi backpressure coil P N 053765 in the EG Ship Kit P N 062453 Connect one end of the backpressure coil to the EluGen cartridge OUTLET port leave the other end of the coil unconnected see Figure 9 16 1 Figure 9 16 EluGen Cartridge Outlet Connection for Conditioning Procedure NOTE The backpressure coil connection is temporary it is used only for the EluGen cartridge conditioning procedure Connect the EGC IN line from the pump to the EluGen cartridge INLET port While holding the EluGen cartridge right side up with the electrolyte reservoir on top shake the cartridge vigorously and tap it with the palm of your hand 10 to 15 times Make sure any bubbles trapped in the eluent generation chamber are dislodged Slide the EluGen cartridge with the electrolyte reservoir on top into the cartridge holder in the EG Doc 065031 04 1 08 287 ICS 3000 lon Chromatography System
311. tructions Monitoring the Amperometry Cell pH Readout Monitoring the pH readout of a solution with a known composition lets you detect any reference potential shift that may occur over time This allows you to determine when the reference electrode needs regenerating or replacing thus improving the reproducibility of your analyses See Section 4 1 2 for how to monitor the pH readout NOTE Monitor the pH when the reference electrode is used in the Ag mode as well as in the pH mode Doc 065031 04 1 08 59 ICS 3000 lon Chromatography System 2 16 3 DC Amperometric Detection In DC amperometry a constant potential is applied to the working electrode The potential can be entered into a program file PGM see Figure 2 23 or on the Control panel for direct control Program Wizard EDet1 Options oi M M Figure 2 23 DC Amperometry Program Wizard Page The applied voltage can be programmed up to 10 times during the run The actual number of potential changes allowed depends on the available data storage capacity which is determined by the length of the run and the data sampling rate 60 Doc 065031 04 1 08 2 DC Description 2 16 4 Integrated and Pulsed Amperometric Detection Integrated and pulsed amperometric detection are similar to DC amperometry see Section 2 16 3 in that molecules are oxidized or reduced at the surface of an electrode However with these detection modes a series of pote
312. ts cannot be serviced by the user Push here to ensure the detector s electrical connection is secure Figure 8 3 Conductivity Detector Connection Doc 065031 04 1 08 213 ICS 3000 lon Chromatography System CD cell 1 over safe temperature Or CD cell 2 over safe temperature This error occurs when the temperature of the specified conductivity detector is higher than the maximum allowed This error may occur if the ICS 3000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot 1 Refer to Section A 12 for environmental specifications 2 Verify that the compartment setpoint is at least 5 C less than the CD cell setpoint 3 Check the suppressor current setting Running the suppressor at a higher current than is recommended for the application can cause heat up of the CD cell Column open circuit This error may indicate a problem in the detector electronics Contact Dionex for assistance Column over safe temperature This error occurs when the temperature of the column compartment exceeds the maximum allowed This error may occur if the ICS 3000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Section A 12 for environmental specifications 214 Doc 065031 04 1 08 8 DC Troubleshooting Compartme
313. tting and Ferrule Sample Loading Port Green 0 75 mm 0 030 in ID PEEK Tubing Figure 5 4 Sample Loading Port Tubing Connection 6 Thread the free end of the tubing through the sample loading port opening on the DC Insert the port into the opening and turn it until it snaps into place 7 Attach a 10 32 fitting and ferrule to the free end of the tubing and connect it to sample port S 5 on the injection valve Loading the Sample 1 Fill a syringe with a calibration standard or sample 2 Insert the syringe into the sample loading port on the front of the DC 3 Verify that the injection valve is in the Load position If it is not switch the valve by clicking the valve control on the Control panel or pressing the VALVE button on the front of the DC 4 Overfill the sample loop with several sample loop volumes Excess sample will exit through the injection valve waste line 5 Leave the syringe in the port This prevents the sample from exiting the loop before injection 6 Switch the injection valve to the Inject position by clicking the valve control on the Control panel or pressing the VALVE button on the front of the DC 142 Doc 065031 04 1 08 5 Operation 5 3 2 Loading Samples with a Vacuum Syringe Pull Method 1 Make sure the sample loading port on the DC front door is connected to sample port S 5 on the injection valve see Figure 5 5 If the port is not already connected see Se
314. turn it upside down and place it on the drip tray in the service position see Figure 9 14 Disconnect the backpressure coil from the EluGen cartridge OUTLET port Connect the EGC OUT line to the OUTLET port Doc 065031 04 1 08 289 ICS 3000 lon Chromatography System 7 Turn the EluGen cartridge right side up and check for bubbles in the eluent generation chamber If necessary shake and tap the cartridge to remove bubbles Reinstall the EluGen cartridge in the holder Remove the 10 32 plug from the vent opening and reinstall the luer adapter and vent line Push the cartridge s electrical cable connector onto the EGC 1 or EGC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 9 13 Replacing the CR TC Replace the CR TC when the background and drift are not acceptable The CR TC replacement procedure consists of e Removing the old CR TC see Section 9 12 2 e Installing and hydrating the new CR TC see Section 9 13 2 e Completing the plumbing for the new CR TC see Section 9 13 3 Refer to Figure 9 12 for a flow schematic of the EG and CR TC 9 13 1 Removing the Old CR TC 1 On the Pump tab page on the panel tabset click the Motor switch to turn off the pump flow This turns off the power to the EluGen cartridge and the suppressor also Open the front door of the EG Push down on the slide release latch and pull the tray forward until it reaches the stop F
315. u attempt to change column ID properties for a column for which no chip card is installed To troubleshoot Insert a column ID chip card into the appropriate slot see Section 9 26 Raw data file x cannot be created or Raw data file x cannot be created Continuing with network failure protection or Raw data file x cannot be written or Raw data file x cannot be written Continuing with network failure protection If a network failure prevents Chromeleon from creating or writing to a raw data file the corresponding error occurs To troubleshoot Wait until batch processing is complete then reboot the PC and restart the Chromeleon server 244 Doc 065031 04 1 08 TC Troubleshooting Starting data acquisition manually will overwrite any data which has been acquired so far This error occurs if you attempt to start data acquisition manually while a batch is already running To troubleshoot To retain the data already acquired cancel manual data acquisition otherwise go ahead and start data acquisition A The command can format only chip cards with an invalid data structure This error occurs if you select the FormatChipCard command for a column ID chip card that is not defective To troubleshoot Cancel the command Do not attempt to reinitialize a chip card unless it contains invalid or corrupted data A The communication interface is closed Reconnect the instrument This erro
316. ubing is in electrical contact with the counter electrode and through it to ground The working electrode current is processed using low noise analog amplifiers and filters Amperometry Cell Solvent Compatibility The amperometry cell can be used with common reversed phase solvents such as methanol and acetonitrile If a disposable working electrode is used the percentage of methanol should not exceed 30 and the percentage of acetonitrile should not exceed 10 Refer to the disposable electrode manual Document No 065040 for additional eluent compatibility information Because conventional working electrode blocks are made of Kel F and use a gasket made of Ultem there is no restriction on the concentration of organic solvents that can be used with them Combination pH Ag AgCl Reference Electrode The reference electrode is a standard combination pH electrode containing a glass membrane pH half cell and a Ag AgCl half cell The combination pH electrode monitors eluent pH The Ag AgCl half cell is typically used as the cell reference electrode To minimize changes in the baseline the combination pH Ag AgCl electrode can be used as the reference electrode during a pH gradient pH Dependence The potentials at which many redox reactions take place on metallic electrodes are pH dependent with the potential shifting 0 059 V per pH unit This is especially true for metal oxide formation oxidation and oxidative desorption Since the
317. ubleshooting Invalid flow value This error occurs if you enter an invalid value for the DP SP flow rate in Chromeleon or Chromeleon Xpress To troubleshoot Select a flow rate within the DP SP flow rate range 0 001 to 10 0 mL min Leak detected This error occurs if the DP SP leak sensor detects a liquid leak inside the enclosure When this error occurs the pump stops running To troubleshoot To find and eliminate the source of the leak see Section 8 15 Doc 065031 04 1 08 191 ICS 3000 lon Chromatography System Left hand pump block carryover pressure is too high Or Right hand pump block carryover pressure is too high This error occurs if the pressure in the primary pump head exceeds the maximum allowed Right hand refers to the bottom pump left hand refers to the top pump in a dual pump module To troubleshoot 1 Make sure that the tubing between the pump heads and the tubing leading to the priming outlet block is not plugged or blocked Replace tubing connections as needed 2 Inspect the outlet check valve for blockage Replace the check valve cartridge if needed see Section 9 4 Motor malfunction This error occurs if an internal error in the pump drive mechanism occurs To troubleshoot Turn off the DP SP power for 30 seconds and then turn on the power again If the error message appears again contact Dionex for assistance Motor position error The motor is ove
318. uid Line Fittings Document No 031432 The manual is on the Dionex Reference Library CD ROM P N 053891 Use a tubing cutter to cut tubing to the required length Make sure the cut is at a right angle to the length of the tubing and there are no nicks or burrs on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 062614 dual P N 063408 single Refer to the instructions provided with the cutter Cleaning Eluent Reservoirs Before preparing new eluent all eluent reservoirs should be rinsed thoroughly inside and out with ASTM Type I 18 megohm cm filtered and deionized water If a reservoir still appears dirty or has a slimy film on the inside clean it as instructed below 1 2 Dispose of any remaining chemicals according to municipal regulations Rinse the reservoir inside and out with ASTM Type I 18 megohm cm filtered and deionized water Rinse the inside of the reservoir with isopropyl alcohol or methanol 258 Doc 065031 04 1 08 9 DP SP Service 4 Ifalgae or bacteria have left a slimy film on the reservoir use an algicide or disinfectant dilute hydrogen peroxide etc 5 Rinse cleaning chemicals out of the reservoir with ASTM Type I 18 megohm cm filtered and deionized water 6 Dry the reservoir with clean particulate free air 9 3 Priming the DP SP The pump should be primed if the eluent has been changed the eluent line is new empty or the eluent line contains
319. ul not to allow stray strands of wire to short to an adjoining position on the connector 3 Plug the connector into the appropriate 12 pin connector on the DC rear panel 4 Connect the wires from the DC connector plug to the appropriate connector pins on the other modules 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 5 Ifyou connected a TTL input verify that the correct function is assigned to the input and that the correct input control type is selected Select different settings if necessary Input functions and control types are assigned from the Chromeleon Server Configuration program see Section 2 18 4 80 Doc 065031 04 1 08 2 DC Description 2 18 2 Analog Outputs When the I O option is installed two analog outputs one for each detector are installed on the DC rear panel see Figure 2 15 The analog outputs supply a voltage signal proportional to the current measured by the detector cell The outputs can be connected to an analog to digital A D converter such as an integrator or other recording device Refer to Section 2 18 1 and the documentation for the device for connection instructions Several settings are available that allow you to configure the analog output signal for your detector and connected device Table 2 2 describes the settings You select the de
320. ump only pump heads and detector cell Degassing eluents is especially important when combining aqueous and nonaqueous components for example water and acetonitrile The vacuum degassing module is either single channel in an isocratic pump or quad channel in a gradient pump The module consists of e A degas chamber with degassing membranes with internal capacity of 670 uL per channel e A dual stage diaphragm vacuum pump e An on board vacuum sensor e The electronics required to operate the vacuum pump e Tubing fittings and other accessories The vacuum degassing module is automatically activated when the DP SP power is turned on Allow about 10 minutes for the module to equilibrate NOTE Make sure the run time is long enough to ensure that the vacuum degassing module delivers the optimal degassing performance Manual Control of the Vacuum Degassing Module The vacuum degassing module normally remains on continuously To turn it off for example to investigate a leak follow these steps 1 In Chromeleon or Chromeleon Xpress select Command on the Control menu or press the F8 key In the Commands dialog box select the pump name Select the Degasser command Select Off and click the Execute button SR Se D To turn on the degasser again select On and click Execute Doc 065031 04 1 08 21 ICS 3000 lon Chromatography System 2 2 5 2 2 6 Piston Seal Wash System The piston seal wash syste
321. up allows automatic system startup and equilibration The Start up button on the Home tab on the ICS 3000 panel tabset starts the system components pump suppressor eluent generator CR TC detector etc The flow rate suppressor current and other settings that were in effect when the system was shut down are restored 118 Doc 065031 04 1 08 4 Startup 4 3 Preparing Samples This section provides basic information about collecting storing and preparing samples for analysis 4 3 1 4 3 2 NOTE Sample preparation can be performed while the system is equilibrating Collecting and Storing Samples Collect samples in high density polyethylene polystyrene or polycarbonate containers that have been thoroughly cleaned with ASTM Type I 18 megohm cm filtered and deionized water Do not clean containers with strong acids or detergents because these can leave traces of ions on the container walls The ions may interfere with the analysis If samples will not be analyzed on the day they are collected filter them through clean 0 45 micron filters immediately after collection otherwise bacteria in the samples may cause the ionic concentrations to change over time Refrigerating the samples at 4 C 39 F will reduce but not eliminate bacterial growth Analyze samples containing nitrite or sulfite as soon as possible Nitrite oxidizes to nitrate and sulfite to sulfate thus increasing the measured concentrati
322. ure 9 34 on the left and push the cell onto its mounting location in the DC compartment Reconnect the two cables and the liquid lines Start the pump flow Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 9 24 7 Replacing an ED Detector 1 NAP 10 Turn off the pump flow from the Control panel in Chromeleon or Chromeleon Xpress or press PUMP FLOW on the front of the pump Disconnect the ED from the Control panel in Chromeleon or Chromeleon Xpress Press the POWER button on the front of the DC to turn off the DC Open the DC upper door and disconnect the cell see Section 9 24 1 Remove the cell from the detector Press the release lever located below the detector The detector pops out slightly from the DC compartment Grasp the detector and pull outward to remove the detector from the compartment Note the electrical plug on the back of the detector and the receptacle on the inside of the DC Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure Reinstall the cell and reconnect the cell inlet and outlet lines and the cables Turn on the DC power and restart the pump flow 326 Doc 065031 04 1 08 TC Service To avoid injury wait for the TC to cool down before opening the door or performing any maintenance or service procedures CAUTION Afin d viter toute br lure laisser refroidir le c
323. ut 27 Analog to digital converter 81 Annual maintenance DC 160 166 168 355 DP 160 162 350 EG 163 SP 160 162 350 TC 168 357 Application Wizard 148 149 Applications 105 112 AS Autosampler 3 6 Example program 144 Needle seal assembly 297 AS40 Automated Sampler 7 26 Example program 144 Atlas Electrolytic Suppressor AES 39 45 55 Gas separator waste tube 36 55 See also Suppressor Audit Trail 18 31 Error messages 169 Icons 169 Automation Manager AM 2 73 Description 4 44 73 High pressure valves 74 Low pressure valves 75 Ordering 354 RCH 1 Reaction Coil Heater 78 343 Valve specifications 343 Autorecycle mode 56 Autosampler Controlling with relays TTLs 84 Filling vials 118 120 Injecting samples 140 Loading the tray 120 Sample loading 140 See also AS Autosampler AS40 Automated Sampler Autozero 136 146 B Background conductivity High 187 Offsetting 136 Backpressure coil CD 312 Reordering 354 Requirements 312 Backpressure coil EG 34 39 Installation 295 Reordering 351 Backpressure excessive Causes of 186 Problems caused by 113 Backpressure low Causes of 185 How to increase 34 113 178 Problems caused by 178 Baseline Noisy or drifting 178 Oscillations 312 Shift 62 Spikes 180 Stability 53 Batch processing 139 Bromate Post column reagent addition 112 Bubbles Removing from the cell 312 Bulkhead connectors EG
324. ve it Figure 9 33 Disassembling the Amperometry Cell NOTE Handle the cell gasket and the inside surfaces of the cell carefully to prevent scratches which may subsequently cause leaks 6 Carefully separate the parts see Figure 9 34 Working Electrode oa Block Ga PEEK Yoke Block eo Cell Body Cell Gasket Figure 9 34 Amperometry Cell Components 7 Use tweezers to remove the old cell gasket see Figure 9 35 from the cell body Doc 065031 04 1 08 315 ICS 3000 lon Chromatography System Alignment Pins Cell Gasket P N 045972 for conventional non disposable working electrodes 10 11 12 13 14 15 16 17 Figure 9 35 Amperometry Cell Gasket Rinse surface of the cell with ASTM Type I 18 megohm cm filtered and deionized water Clean the polished surface of the cell with a damp soft cloth or tissue Install the new gasket P N 045972 over the alignment pins on the cell body When correctly installed one end of the gasket extends beyond the cell body to facilitate gasket installation and removal Verify that the gasket is flat against the cell body and has no wrinkles Reinstall the working electrode block and the PEEK yoke knob and block Fingertighten the PEEK yoke knob by turning it a full 360 degrees NOTE It is not possible to overtighten the PEEK yoke knob Once the knob clicks into place it does not tighten any furthe
325. vironmental 339 Aco Physical ose LL ag wid eu des eue nt se RAR 339 A 10 EluGen Cartridge 340 DC Specifications ALLL Electrical ste mn es ose les ter re rate ee et Bea tay 341 A12 Environmental 84 pee nn end RA tee ee ea ok 341 A13 Physical gr e r manon nent ea sat Gr el 341 A 14 Lower Compartment Components 342 A 15 Temperature Control 342 A 15 1 Upper Compartment 342 A 15 2 Lower Compartment Optional 343 A 16 ICS 3000 Automation Manager 343 A 16 1 RCH 1 Reaction Coil Heater 343 Al G 20 Valves excite ra ied mes ab Roa ade ra ere nn 343 A 17 ICS 3000 Conductivity Detector 344 A 18 ICS 3000 Electrochemical Detector 345 TC Specifications A 10 Electrical see are cn en Meat onda Atte nares alas alka oy 347 A 20 Environmental 347 A2 Physical sens Re A pee eG See ees 347 A 22 Thermal Compartment 348 B Reordering Information DP SP Reordering Information Doc 065031 04 1 08 xiii ICS 3000 lon Chromatography System EG Reordering Information DC Reordering Information TC Reordering Information xiv Doc 065031 04 1 08 1 1
326. w rate to a value within the allowed range The allowable eluent concentration for a particular application depends on several factors the flow rate suppressor type EluGen cartridge type and cartridge configuration For details refer to Section 4 7 EG1 over current Or EG2 over current This error occurs when the current applied to the EluGen cartridge exceeds the maximum current allowed The EluGen current is automatically turned off to prevent damage to the cartridge This error may also occur if the liquid flow to the cartridge is interrupted Doc 065031 04 1 08 205 ICS 3000 lon Chromatography System To troubleshoot 1 Connect the EluGen cartridge cable connection to the electrical bulkhead see Figure 2 8 2 Refer to Section 8 23 to determine why there is no flow 3 Ifthe error message appears again contact Dionex for assistance The cartridge control electronics may have malfunctioned NOTE The ICS 3000 Ion Chromatography System electronics components cannot be serviced by the user EG1 over power Or EG2 over power This error occurs when in order to maintain the selected current the power supply is required to supply a higher voltage than the EluGen cartridge can support To troubleshoot Replace the EluGen cartridge see Section 9 12 EG1 over voltage Or EG2 over voltage This error occurs when the current applied to the EluGen cartridge exceeds the maximum current allowed
327. wer 2 Download new firmware to the TC as follows a Insert the CD containing the new firmware version into the CD drive b Start the Server Configuration program c Inthe timebase right click the TC for which you want to update the firmware and select Properties on the context menu d On the General tab page in the Properties dialog box click Firmware Download to display a file open dialog box e Select the file the extension is fmw containing the new firmware version and click Open to begin the download Audit Trail messages will inform you of the status of the download 3 Ifthe error occurs again contact Dionex for assistance The firmware cannot be serviced by the user 230 Doc 065031 04 1 08 TC Troubleshooting Can t use device x as a source of the column pressure A Please check the property SystemPressure for a valid device name The device must have the Pressure property available Or Can t use device x as a source of the column pressure Please check the property y for a valid device name The device must have the Pressure property available This error occurs if the device selected to monitor the system pressure is ineligible to do so To troubleshoot 1 In the Commands dialog box in Chromeleon or Chromeleon Xpress click the plus sign beside TC to display the items underneath 2 Click the plus sign beside the column name and select the SystemPr
328. y System Noisy Baseline ED Only DC Amperometry and Integrated Amperometry modes Air bubbles trapped inside cell While wearing gloves and eye protection and with the pump running and all plumbing connected generate a slight temporary backpressure by putting your finger over the end of the cell outlet tubing for 2 to 3 seconds Repeat 2 or 3 times If the baseline does not improve check the other causes of baseline instability described in this section Do not block the end of the cell outlet tubing for longer than the recommended 2 to 3 seconds Doing so creates high backpressure which can break the reference electrode glass membrane NOTE To prevent air from becoming trapped in the cell in the future increase the backpressure on the cell by connecting backpressure tubing to the cell outlet The backpressure limit for the ED cell is 690 kPa 100 psi Do not exceed this limit DC Amperometry and Integrated Amperometry modes Frequent random spikes in the baseline The reference electrode diaphragm is plugged First try regenerating the reference electrode frit by soaking the electrode in a solution of 1 M KCI plus 1 M HCL If this does not eliminate the spiking replace the electrode P N 061879 DC Amperometry and Integrated Amperometry modes Regular baseline oscillation on high sensitivity ranges Reconnect the short length of titanium tubing to the cell inlet see Figure 2 22 DC Amperometry and Integrated A
329. y or TTL connection is required for Chromeleon or Chromeleon Xpress to control sample loading Refer to Installing the ICS 3000 Ion Chromatography System Document No 065032 for relay connection instructions 2 300 Pump Relay 1 Closed Duration 138 00 Notel 0 000 Autozero Note 2 AcgOn sNote 3 InjectValvel InjectPosition Duration 30 00 Note 4 30 00 AcqOff Note 5 1 Close the RELAY OUT 1 which is connected to the AS40 LOAD relay This signals the AS40 to load the sample 2 Zero the baseline 3 Start data acquisition 4 Switch the valve to Inject 5 Stop data acquisition 144 Doc 065031 04 1 08 5 Operation 5 4 3 Commands for a Remote Inject Device If you manually load the sample using a syringe see Section 5 3 you can configure a remote inject device in the same timebase as the DC When Chromeleon or Chromeleon Xpress runs a program and a remote inject device is configured it waits until an inject signal is received before starting data acquisition To trigger the inject signal switch the injection valve to inject by clicking the valve control on the Control panel or pressing the VALVE button on the front of the DC When Chromeleon or Chromeleon Xpress executes the program it runs the commands that occur before the Inject command and then waits for the inject signal During this waiting period the following message is displayed in the Audit Trail Waiting for inject response on InjectValv
330. yclic voltammetry mode the detector measures the current at a rate of 1 KHz i e 1000 raw data points per second are collected The data is compressed before storage to 20 Hz Waveforms A waveform is a series of steps defined as points on a plot of potential vs time Waveforms must be defined for the cyclic voltammetry and integrated amperometry modes Cyclic Voltammetry Waveforms Cyclic voltammetry waveforms consist of three steps each with a time and a potential The waveform forms a triangle with the first step always at time zero and the first and third steps always having the same potential Figure 2 26 shows an example of a triangular waveform used in cyclic voltammetry Volts 0 20 0 80 af 0 00 0 80 28 0 0 80 30 00 Seconds Figure 2 26 Example Cyclic Voltammetry Waveforms Doc 065031 04 1 08 63 ICS 3000 lon Chromatography System In this example the potential is scanned from 0 80 to 0 60 V and then from 0 60 to 0 80 V The total time for one waveform period is 28 s This provides a sweep rate of 0 1 V s as shown in the equation below 2xAV Sweep Rate CV Cycle Time 2x1 4V _ 0 1 y 28s S Cyclic voltammetry waveforms are defined manually on the Chromeleon or Chromeleon Xpress electrochemical detector Control panel Click the CV Mode button to display the following window 1 BE Cyclic Voltammetry Mode ICS 3000 Bek hemical Detector Cyclic
331. zard adding the desired number of samples and standards to the list For help at any time click the Help button on the Sequence Wizard page 148 Doc 065031 04 1 08 5 Operation Using the Application Wizard 1 Click Application Wizard on the Sequence Control panel 2 Select a suppressor type if used and then select an application template from the list NOTE Instead of selecting an application template you can use the Virtual Column Separation Simulator Refer to the Chromeleon Help for details 3 Click Next gt and select the in a new sequence via Sequence Wizard option 4 Click Next gt to go to the Sequence Wizard 5 Complete the steps in the Sequence Wizard adding the desired number of samples and standards to the list For help at any time click the Help button on the Sequence Wizard page After you finish the Sequence Wizard 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 6 2 Starting Batch Sample Processing 1 Click Load Sequence on the Sequence Control panel A dialog box opens 2 Select the sequence from the list and click Open or Load if you are using Chromeleon Xpress 3 Click Start Batch on the Sequence Control panel Doc 065031 04 1 08 149 ICS 3000 lon Chromatography System 150 Doc 065031 04 1 08 6 Shutdown DP SP Shu

ICS-3000 Ion Chromatography System Operator`s Manual

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