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ICS-5000 Ion Chromatography System Operator`s Manual

1. The data format stored on the chip card is Error page 293 unsupported format version x The injections limit for the column has been Warning page 294 exceeded The injections limit will be exceeded for the Warning page 294 column x The nominal temperature must be set within the Error page 294 current limits The nominal temperature value is out of range Error page 294 defined by the active column ID The oven is not fully operable yet Check the Error page 294 values of Standby Ready Door and CardState The primary column ID property x will be Warning page 295 changed The property can t be changed in the future The upper limit must be higher than the lower Error page 295 limit The Warning threshold must be higher than the Error page 296 Limit threshold The Warning threshold must be lower than the Error page 296 Limit threshold There was already an AcqOff command for this Warning page 296 channel before There was already an AcqOn command for this Warning page 296 channel before This function cannot be adjusted by the user Abort page 297 This operation may affect the oven s operation Warning page 297 on timebase x which is currently running a batch Table 8 4 TC Error Messages Continued Doc 065342 06 12 11 213 Dionex ICS 5000 Operator s Manual TC Related Audit Trail Error Message Default
2. 0 0 cece eee eee 65 2 1321 4 Port Valve ci dea is a edie es bee he Geel dae Pe 66 Doc 065342 06 12 11 Contents 2 13 2 6 Port ValVe ui alc tech Saba dale bani fests 67 2 13 3 10 Port Valve 0 0 ili soa ab tat eg bah teas 68 2 14 CD Conductivity Detector 0 eee eee eee 69 2 14 1 Heated Conductivity Cell 0 0 eee eee eee 69 2 142 SUDPIESSOL arri i e 71 2 14 3 System Flow Schematics for Conductivity Detection 72 2 15 ED Electrochemical Detector 75 2 15 1 Electrochemical Detector Cell 75 2 15 2 Combination pH Ag AgCI Reference Electrode 77 2 15 3 Palladium Hydrogen PdH Reference Electrode 79 2 16 DC Rear Panel sifone useable ates 80 21T W O Option eeo i A ies hei eee han Be a es 83 2 17 1 I O Option Connections 84 2 17 2 Analog Outputs LL 85 2 17 3 Power Relay and TTL Outputs 0 87 2 1074 TEE Inputs i diede 89 2 18 Automation Manager 0 eects 94 2 18 1 AM High Pressure Switching Valves 96 2 18 2 AM Low Pressure Valves LL 97 2 18 3 AM High and Low Pressure Valve Control 98 2 18 4 RCH 1 Reaction Coil Heater 0 4 101 2 19 Electrochemical Detection Modes 102 2 19 1 DC Amperometric Detection 0 4 102 2 19 2 Integrated and Pulsed Amperometric Detection 103 2 19 3 Cyclic Voltammetry Li 105
3. Doc 065342 06 12 11 iii Dionex ICS 5000 Operator s Manual 219 4 Waveforms io piu prorina hate deeb Pas dest dee tes 105 2 19 5 Storing and Reprocessing Amperometry Data 109 TC Description crepa reader 115 2 20 FC Front Features ui rai Swe ee belies 115 2 21 TC Interior Components 117 2 22 TC Rear Panel vicine ea 119 223 Inj ction Valvestino eek ota eet es ey cde ahs 122 2 23 1 Injection Valve Operation 0 00 0 eee ee 122 2 23 2 Injection Valve Plumbing 004 124 2 24 Column Identification ID System 125 2 25 Gas and Humidity Sensors LL 126 2 26 TC Theory of Operation 0 0 0 2 eee eee eee 127 2 26 1 Predictive Performance 0 0 0 ee ee eee ee 128 3 Configurations ZL Overview oe Sete Gi Be Ba teed io roi 129 4 Startup 4 1 Operating Precautions 0 eee eee eee eee 141 4 1 1 EG Operating Precautions 00 004 141 4 1 2 ED Cell Operating Precautions 143 4 2 System Startup Checklist 146 4 3 Preparing Samples 147 4 3 1 Collecting and Storing Samples 147 Doc 065342 06 12 11 Contents 4 3 2 Pretreating Samples LL 147 4 3 3 Diluting Samples 148 4 3 4 Filling the Autosampler Vials and Loading the Sample Travis woh ane aaa a bee de Sea i 149 4 4 Starting Chromeleon 7 0 0 cece eee eee 149 4 4 1 Starting the Chrome
4. 7 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 The tubing is included in the pump ship kit Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 063342 Doc 065342 06 12 11 327 Dionex ICS 5000 Operator s Manual 8 Connect the new tubing pieces 10 11 to the seal wash reservoir and pump heads see Figure 9 10 o Push the tubing onto the fitting i EN that was removed in Step 5 Connect the PharMed tubing to the peristaltic pump as follows Tygon 2075 Tubing 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 Secondary d Release the lever La Figure 9 10 Piston Seal Wash Tubing Connections e Pullon the fitting slightly to slide the tubing into the upper notch 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 Push the component mounting panel back into the enclosure Close the DP SP door 12 Turn on the pump flo
5. 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 If you are polishing the electrode before initial installation use only the fine polishing compound If you 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 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 filtered and deionized water that meets the specifications listed in Section 1 5 to make a thick paste 390 Doc 065342 06 12 11 9 DC Service 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 electrode c Use ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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
6. To ov Column Ww c To Waste P From Pump From Pump Sample Eluent Figure 2 24 Injection Valve Flow Schematics 4 Port Valve e In the Load position sample flows from the syringe or autosampler line if installed through the valve and into the internal sample loop where it is held until injection Excess sample flows out to waste Eluent flows from the pump through the valve and to the column bypassing the sample loop e In the Inject position eluent flows from the pump through the internal sample loop and on to the column carrying the contents of the sample loop with it Section 5 3 1 describes how to inject samples with an autosampler and Section 5 3 2 describes how to inject samples manually 66 Doc 065342 06 12 11 2 DC Description 2 13 2 6 Port Valve The 6 port valve P N 061961 is the standard injection valve for analytical IC systems It is installed in the lower compartment of the DC see Figure 2 21 Figure 2 25 shows flow schematics for the 6 port valve LOAD POSITION INJECT POSITION Sample Loop Sample Sample In Loop Sample In To To Column Column We Cc To Ar Waste From Pump From Pump Eluent Sample Figure 2 25 Injection Valve Flow Schematics 6 Port Valve e In the Load position sample flows from the syringe or autosampler line if installed through the valve and into the sample loop where i
7. 272 8 28 3 Shift in ED Cell pH Readout 272 8 28 4 No ED Cell pH Readout or Intermittent Readout 273 Doc 065342 06 12 11 ix Dionex ICS 5000 Operator s Manual 8 28 5 Leak in pH Ag AgCl Reference Electrode Compartment 274 8 28 6 Shift in Ag AgCl Reference Potential 274 TC Troubleshooting 0 0c cece eee eee 275 8 29 Troubleshooting TC Error Messages 000005 275 8 30 TC ALARM LED Is Lighted 00 02 eee 299 8 31 Liquid Leaks from TC Components 008 300 8 32 TC Temperature Does Not Increase 301 8 33 TC Temperature Stabilizer Not Operating Properly 301 9 Service 9 1 Connecting Capillary Tubing LL 303 9 2 Tightening Guidelines for High Pressure Fittings 305 DP SP SEVICE e il SERE eee i 306 9 3 Replacing Tubing and Fittings LL eranu e nee 306 9 4 Cleaning Eluent Reservoirs 0 0 0 0 ee eee eee ees 308 9 5 Priming the DP SP iibic iii pie dob iee neni ine e pee ee 308 9 5 1 Priming with the PUMP PRIME Button 309 9 5 2 Priming from the Chromeleon Panel 310 9 6 Replacing the Check Valves 0 0 eee eee ee eee 312 9 6 1 Removing the Check Valves 0 002000 313 9 6 2 Installing the New Check Valves 00 314 9 7 Replacing Piston Seals 0 0 0 eee eee ee eet 316 9 7 1 Removing the Pump He
8. 750 Curent Om Unknown Flow_detected 1000 0 0 2 5 5 0 7 5 10 0 Figure 4 9 DC Control Panel Chromeleon 7 Version Shown 3 For each of the following temperature control devices installed in the DC Compartment Column Reaction Coil IC Cube enter the preferred Set temperature This turns on the device also If the preferred temperature is already selected but the device is off click the corresponding switch to turn on the device Doc 065342 06 12 11 165 Dionex ICS 5000 Operator s Manual If a suppressor is installed Under Suppressor 1 or Suppressor 2 select the suppressor Type set the Mode to On and enter the Current required for your application If a CD is installed Click the CD tab to open the CD panel Under Cell Heater set the Cell Heater Mode to On and enter the Cell Heater Set Point 4 12 Equilibrating the System and Verifying Operational Readiness NOTE You can also use the Smart Startup feature in Chromeleon to automate system startup and equilibration Refer to the Chromeleon Help for details On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset verify that each device listed below if installed in your system is turned on and the selected setting for the device flow rate eluent concentration temperature and so on is correct for your application e Pump e EGC e CR TC e EPM e Suppressor e Temperature control devices DC compartment
9. MISE EN GARDE VORSICHT Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hlt ist ehe Sie die T r ffnen bzw Wartungs oder Servicearbeiten durchf hren 372 Doc 065342 06 12 11 9 DC Service 3 Open the DC upper door 4 Disconnect each liquid line connected to the IC Cube cartridge to be replaced 5 Loosen the two thumbscrews on the cartridge see Figure 9 40 and pull the cartridge out of the IC Cube 6 Slide the new cartridge into the IC Cube Push the cartridge firmly into the IC Cube and then tighten the thumbscrews Cartridge Thumb screws Figure 9 40 Capillary Cartridge Thumbscrews EG Degas Cartridge Shown 7 Ifyou are installing a suppressor or CRD cartridge hydrate them before use Refer to the instructions in the suppressor or CRD manual The manuals are included on the Thermo Scientific Reference Library DVD P N 053891 8 Reconnect the liquid lines that were disconnected in Step 4 Doc 065342 06 12 11 373 Dionex ICS 5000 Operator s Manual 9 26 2 Replacing Capillary Columns 1 2 3 4 Turn off the pump flow Open the DC upper door Disconnect the line from the ELUENT OUT port of the injection valve and the line from the ELUENT OUT fitting on the column cartridge see Figure 9 41 Disconnect these two lines DEGAS Figure 9 41 Disconnect Capillary Cartridge Eluent Lines Loosen the two thumbscrews on the column cartr
10. 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 To troubleshoot 1 Check all tubing connections for signs of blockage replace as needed see Section 9 3 Be careful not to overtighten fittings 2 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 On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset set the Flow rate to 0 01 mL min for a capillary IC system or 1 0 mL min for an analytical IC system and record the backpressure d Disconnect all components after the injection valve e One at a time reconnect each component of the flow path If reconnecting a component causes an abnormal increase in backpressure replace the component Replace as many components as necessary to resume operation at the standard operating backpressure 3 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 pro
11. 061961 Injection valve head including seal for 2 position 6 port valve 061962 Injection valve head including seal for 2 position 10 port valve 042857 Sample loop 25 uL Consumables 6710 1505 Column ID Kit includes five column ID chip cards 064786 Column Clips Kit includes six column clips 064548 Temperature stabilizer standard bore 0 25 mm 0 010 in ID 064650 Temperature stabilizer microbore 0 125 mm 0 005 in ID Miscellaneous 954776 Fuse IEC 60127 2 time lag rated at 2 A two fuses required 063246 USB cable 1 m 3 ft 6000 1004 6 pin mini DIN signal cable 5 m 16 4 ft 064792 TC VWD PDA Regulator Bracket Kit Maintenance Kit 075041 6 Port High Pressure Valve Preventive Maintenance Kit 075042 10 Port High Pressure Valve Preventive Maintenance Kit Doc 065342 06 12 11 445 Dionex ICS 5000 Operator s Manual 446 Doc 065342 06 12 11 Symbols Offset analog out 86 5V output DC 83 87 Numerics 10 port valve AM 96 DC 65 67 TC 123 See also High pressure valves 2D data Integrated amperometry 107 109 Pulsed amperometry 109 3D amperometry data 111 113 3D plot description 112 113 Chromatogram 111 Definition 110 Displayed in Chromeleon 110 Isoamperometric plot description 112 I t plot 111 3 way low pressure valves See Low pressure valves 4 port valve 66 6 port valve DC 65 96 TC 122 1
12. 22 EG 37 TC 115 C Cables Power cord 357 370 371 413 Signal cable 6 pin mini DIN 121 445 USB 33 46 437 440 444 445 CAES 71 Calibration CD cell 379 381 pH Ag AgCl reference electrode 394 Recorder analog output 86 Capillary IC applications 2 Conductivity detector for 69 CR TC trap column for 42 DC components for 54 Eluent generator cartridges for 41 Injection valves for 65 Replacing capillary columns 374 379 Suppressors for 71 System configurations 129 Tube fitting installation 303 304 Tubing and fittings DC 359 Carbohydrate analysis 140 Carbonate mixer 43 Carbonate bicarbonate eluent 41 43 164 CCES 300 57 CCES 300 Capillary 71 CD cell disconnected error 259 CD cell over safe temperature 260 CE mark 19 cETLus mark 19 Check valve cartridges Replacement procedure 312 Chromatogram Amperometry data 111 Dips instead of peaks 86 Pulsed amperometry example 109 Water dip in 148 Chromeleon 11 Alarm conditions 259 275 Application Wizard 174 176 Audit Trail 22 37 203 Audit Trail error messages 203 Commands dialog box 26 126 156 Connected LED 51 Controlling external valves 82 Controlling high pressure valves 98 Controlling low pressure valves 98 Controlling power relays and TTL outputs 89 Controlling switched AC sockets 81 Creating a sequence 174 ePanel Set 11 149 171 Home panel 11 Installation manual 14 Instrum
13. EDet1 ED_i_Total AcqOn CDeti Autozero CDet1 CD_1 AcgOn CDet1 CD_1_Total AcgOn Figure 2 45 Chromeleon 7 Script Editor 98 Doc 065342 06 12 11 2 DC Description To add AM valve control commands to a Chromeleon 6 8 program use the Relay and State Devices Options page in the Program Wizard see Figure 2 46 Program Wizard Relay and State Devices Options AM_HP1 AM_LP1 9 Closed DC_ACRelay_1 DC_ACRelay_2 DC_LP1 DC_LP2 DC LP3 Figure 2 46 Chromeleon 6 8 Program Wizard Relay and State Devices Options Page Doc 065342 06 12 11 99 Dionex ICS 5000 Operator s Manual For manual control of AM valves execute commands from the DC ePanel in Chromeleon 7 see Figure 2 47 or the DC Control panel in Chromeleon 6 8 ICS 5000 Home AS Pump EG DC CD ED Audit Queue O eevee gt Detector Compartment Compartment Column React e o 7 Serial Number 123456789012 gm Gr Status Ready Set 30 00 C_ Set 130 00 t Set Upper Door Closed 0 a E m 35 10 70 20 15 20 Valves Inj 1 LoadPosition DC_LP1 Closed Ini 2 LoadPosition DC_LP2 Closed Vv DC_LP3 Closed W AM_LPI Closed Y DC_LP4 Closed YW AM_LP2 Closed YW Suppressor 1 Type None Mode Off SS DC_LPS rr Current 0 mA DC_LPE Closed Vv lt Figure 2 47 Valve Control on DC ePanel in Chromeleon 7 100 Doc 065
14. Values Zero Full Scale Normal Description 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 analog 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 4 Analog Output Configuration Settings Continued 86 Doc 065342 06 12 11 2 DC Description ICS 5000 Home Pump EG AS DC CD EDI Audit Queue Detector Settings CD Signal 80 325 Total Signal
15. Waveform 200 Waveform name Download Waveform NP Valtane nanan IS ele I I n rn Pm ne AT n i MI AA i a dr ara errare A RA A A iii A Figure 4 1 Monitoring the pH Ag AgCI Reference Electrode pH 3 Thereafter monitor the pH value to determine whether there is a shift in the pH A shift in the pH reading for the same eluent composition 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 pH Ag AgCI reference electrode see Section 8 28 6 144 Doc 065342 06 12 11 4 Startup To set ED cell pH limits You can set upper and lower pH limits in the Chromeleon 7 Instrument Method Wizard see Figure 4 2 or Chromeleon 6 8 Program Wizard The Audit Trail displays an alarm if the limits are exceeded Instrument Method Wizard Options ED EDet2 EDet2 Options EDet2 Options for Options ED EDet2 Channels ED_2 ED_2 Total Waveform Selector Retention min 1 Initial Time Amperometry Cell On O Off Waveform lt New Waveform gt Autozero O Yes No Data Collection Rate 1 00 Hz Electrode Description pH 10 00 13 00 Lower Limit Upper Limit Figure 4 2 Setting pH Limits in Chromeleon 7 Cancel Help NOTE To disable the alarm set the upper limit to 14 and the lower limit to 0 Doc 065342 06 12 11 145 Dionex ICS 5000 Operator s Manual 4 2 System Startup Checklist
16. r F F r r rF O psi 0 00 1 25 2 50 3 75 5 00 6 25 7 50 8 75 10 00 pp psi ae _ re a EGC Left EGC Right Injection State Off Vial Position RAI Injection Type PushFull 0 00 mM c00mM amp CR TC CR TC TR of J oi Injection Volume 100 0 AS AP Figure 1 2 Chromeleon 7 ePanel Set Dionex ICS 5000 Home Panel Shown 12 Doc 065342 06 12 11 1 Introduction Figure 1 3 Chromeleon 6 8 Panel Tabset Dionex ICS 5000 Home Panel Shown Doc 065342 06 12 11 13 Dionex ICS 5000 Operator s Manual 1 2 Dionex ICS 5000 System Documentation Every effort has been made to provide complete and accurate user documentation for the Dionex ICS 5000 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 Thermo Scientific Dionex ICS 5000 lon 065342 Yes No Chromatography System Operator s Manual Installing the Thermo Scientific Dionex 065343 Yes Yes ICS 5000 lon Chromatography System Dionex AS Autosampler Operator s 065051 Yes No Manual Dionex ICS Series Photodiode Array 065147 Yes No Detector Operator s Manual Dionex ICS Series Variable Wavelength 065141 Yes No Detector Operator s Manual Chromeleon 7 Installation Guide 071686 Yes Yes Chromeleon 7 Quick Start Guide 0
17. 8 EG Troubleshooting EGC cannot be used due to invalid ion count This error occurs if the ion count reported by the EGC is invalid This may indicate a problem with the memory chip in the EGC To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance EGC is either not installed or invalid cartridge number Please install a capillary EGC This error occurs if no EGC cartridge is connected to the EG or an analytical EGC is connected to a capillary IC system To troubleshoot 1 Verify that a capillary EGC is installed 2 Verify that the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened EGC is either not installed or invalid cartridge number Please install an analytical EGC This error occurs if no EGC cartridge is connected to the EG or a capillary EGC is connected to an analytical IC system To troubleshoot 1 Verify that an analytical EGC is installed 2 Verify that the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened Doc 065342 06 12 11 251 Dionex ICS 5000 Operator s Manual EGC is either not installed or invalid cartridge number Please install an EGC This error occurs if no EGC cartridge is connected to the EG or the cartrid
18. CD Only 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 Thermo Scientific Reference Library DVD P N 053891 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 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 Thermo Scientific Reference Library DVD P N 053891 Doc 065342 06 12 11 225 Dionex ICS 5000 Operator s Manual DC Amperometry and Integrated Amperometry modes Amperometric detection cell working electrode shorted to counter electrode Clean 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
19. Capillary tubing fittings incorrectly installed Incorrectly installed fittings on capillary tubing can increase void volumes causing chromatograms with tailing peaks see Figure 8 2 4 50 Sulfate Assymmetry 2 72 Chioride Assymmetry 3 03 Phosphate Assymmetrp 48 300 Nitrite Assymmetry 2 78 Nitrate Aspymmetry 2 68 ps 2 00 Fluoride As 950 pp rr 0 0 5 0 10 0 15 0 20 0 25 0 30 0 Figure 8 2 Tailing Peaks Caused by Incorrectly Installed Capillary Tubing Fittings To correctly install fittings on capillary tubing follow the instructions in Section 9 1 222 Doc 065342 06 12 11 8 Troubleshooting 8 8 Low System Backpressure PEW IC 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 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 16 Internal EGC 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 EGC see Section 9 14 NOTE The EG leak sensor cannot imm
20. Cyclic Voltammetry jnal 7 Cycle Time 10 00 s 2 Elapsed Time CV Mode In Le CV Low Voltage 1 000 V Rise Time o CV High Voltage 100V 3 Start CV T il Close aids pg es Figure 2 53 Cyclic Voltammetry Control Panel Integrated Amperometry Waveforms Integrated amperometry waveforms are included in an instrument method in Chromeleon 7 or a program in Chromeleon 6 8 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 e 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 e 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 e Each waveform can have only one integration interval However 3D amperometric data can be reprocessed after the run with integration intervals at multiple points in the waveform see Section 2 19 5 e The integration interval generates one integrated data point per waveform Doc 065342 06 12
21. DP SP Reordering Information 435 EG Reordering Information 439 DC Reordering Information 441 TC Reordering Information 445 xiv Doc 065342 06 12 11 1 Introduction 1 1 Thermo Scientific Dionex ICS 5000 System Overview 1 Dionex ICS 5000 Dual Pump DP Dionex ICS 5000 Eluent Generator Ec Dionex ICS 5000 Detector Chromatography Module Figure 1 1 Dual Dionex ICS 5000 System with RFIC EG The Thermo Scientific Dionex ICS 5000 Ion Chromatography System offers a full range of Reagent Free IC RFIC components RFIC EG combines automated eluent generation and self regenerating suppression to make IC easier and more powerful than ever 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 Doc 065342 06 12 11 1 Dionex ICS 5000 Operator s Manual results In combination with capillary columns at flow rates of 0 010 mL min the Dionex ICS 5000 system can be used for long periods of continuous operation and minimal eluent consumption The dual analysis capabilities both simultaneous and sequential of the Dionex ICS 5000 system let you maximize efficiency and throughput and m
22. 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 High pressure valves 1 and 2 are the valves installed in the DC lower compartment see Figure 8 5 High pressure valves 3 and 4 are the valves installed on either the IC Cubes or the AM in the upper compartment see Figure 8 6 High Pressure Valve 1 1 High Pressure 2 Valve 2 not j installed in this system Ni r 7 5 ex ro ea Di wi a E Figure 8 5 High Pressure Valves 1 and 2 In DC Lower Compartment High Pressure Valve 3 High Pressure Valve 4 Figure 8 6 High Pressure Valves 3 and 4 On IC Cubes Doc 065342 06 12 11 265 Dionex ICS 5000 Operator s Manual High amp Pressure Valve 3 High Pressure Valve 4 Figure 8 7 High Pressure Valves 3 and 4 On AM To troubleshoot 1 Ifa sequence is being executed terminate the sequence by selecting Stop on the Chromeleon 7 ePanel or Chromeleon 6 8 Control panel 2 Turn off the Thermo Scientific Dionex ICS 5000 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 3 Try to toggle the valve from Load to Inject by pressing the Load and Inject buttons on the front of the DC
23. 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 A check valve may be defective Replace the check valve cartridges see Section 9 6 and then prime the pump see Section 9 5 Doc 065342 06 12 11 231 Dionex ICS 5000 Operator s Manual 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 7 instrument method or Chromeleon 6 8 program but 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 If the 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 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 see Section 9 3 Be careful not to overtighten fittings 232 Doc 065342 06 12 11 8 DP SP Troubleshooting The pressure in the left hand working cylinder exceeded the safety limit
24. s Manual 11 12 13 14 15 16 17 18 Remove the fitting plug from the outlet fitting on the separator column Orient the fitting with a flat side up and push the fitting into the opening at the front of the column cartridge until it stops see Figure 9 44 Coil the separator column tubing inside the cartridge as shown in Figure 9 42 or Figure 9 43 Secure the column and the inlet fitting in the clips on the column cartridge Secure the inlet and outlet fittings on the guard column if used in the column clips on the lid of the column cartridge Route the column inlet tubing from the guard column if used or the separator column through the clip on the top edge of the cartridge lid Close the lid you should hear a click and route the tubing into the slot on the front of the column cartridge see Figure 9 48 NOTE Ifthe columns are installed correctly the cartridge lid snaps closed easily If the lid does not close easily do not force it Open the lid and verify that the columns and tubing are installed correctly and secured in the clips o Separator Column Outlet Column Label Column Inlet Tubing Figure 9 48 Column Cartridge Closed Slide the column cartridge into the IC Cube column oven and tighten the two thumbscrews Turn on the pump flow Wait until liquid is flowing out of the Eluent Out port 3 of the injection valve 378 Doc 065342 06 12 11 9 DC
25. 59 17 11 24 2009 0 00 59 17 11 24 2009 Figure 9 58 Wellness Panel Dionex ICS 5000 Electrochemical Detector Chromeleon 7 Version Shown 5 Follow the instructions on the panel to calibrate the electrode 6 Disconnect the pH Ag AgCl reference electrode cable and the cell cable 7 Grasp the cell body and pull straight out to remove the cell from the detector Be If you are installing the pH Ag AgCl reference electrode in a capillary IC system go on to page 396 If you are installing the pH Ag AgCl reference electrode in an analytical IC IG system go on to page 398 Doc 065342 06 12 11 395 Dionex ICS 5000 Operator s Manual mey Installing the pH Ag AgCl Reference Electrode in the Cell for a Capillary IC System 1 To avoid any hydraulic pressure buildup when inserting the pH Ag AgCl reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings 2 Use a sharp tool for example the tip of a safety pin or a straight pin to remove the pH Ag AgCl reference electrode O ring see Figure 9 59 pH Ag AgCl Reference Electrode O Ring remove for capillary IC Figure 9 59 pH Ag AgCI Reference Electrode O Ring 3 Using tweezers install the reference electrode gasket for capillary IC P N 072162 into the bottom of the reference electrode well see Figure 9 60 Reference Electrode Gasket for Capillary IC Figure 9 60 Reference Electrode
26. 7 10 DC Weekly Maintenance e Check liquid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines e 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 7 11 DC Periodic Maintenance e Inspect the door seal for signs of damage A defective seal impairs the performance of the instrument If the seal is defective contact Technical Support for Dionex products Doc 065342 06 12 11 199 Dionex ICS 5000 Operator s Manual 7 12 DC Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The following kits are available e 0 4 uL Internal Loop High Pressure Valve Preventive Maintenance Kit P N 075040 e 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 e 10 Port High Pressure Valve Preventive Maintenance Kit P N 075042 200 Doc 065342 06 12 11 fa TC Routine Maintenance This section describes routine maintenance procedures for the Dionex ICS 5000 Thermal Compartment TC that users may perform All other maintenance procedures must be performed by Thermo Fisher Scientific personnel 7 13 TC Daily Maintenance e Check the TC components for leaks or spills Wipe up spills Isolate and repair leaks see Sect
27. Ba 7 Ifyou are installing a CR TC in an analytical IC system remove the backpressure tubing from the EGC IN line and use a high pressure blue fitting to connect the EGC IN line to the EGC INLET port 9 15 3 Completing the New CR TC Plumbing 1 Connect the regen out and eluent in lines from the eluent degasser to their respective ports on the CR TC Refer to Figure 9 28 for a capillary IC system or Figure 9 29 for an analytical IC system To EGC OUTLET Port WASTE GAS SEPARATOR To EG Degas Cartridge Regen Out To EG Degas Cartridge Eluent In Figure 9 28 Capillary CR TC Plumbing Diagram Installation Completed Doc 065342 06 12 11 353 Dionex ICS 5000 Operator s Manual To EGC To RFIC Eluent To RFIC Eluent OUTLET Port Degasser Degasser REGEN OUT Port ELUENT IN Port Y To Gas Separator Waste Tube WASTE GAS lt 4 SEPARATOR CR TC Figure 9 29 Analytical CR TC Plumbing Diagram Installation Completed 2 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 3 Push the CR TC electrical cable firmly into the CR TC 1 or CR TC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 4 Push the tray into the module until it locks into p
28. Capillary removes the carbonate peak contributed by the sample in hydroxide eluent chemistries Removal occurs immediately after suppression of the eluent before the sample reaches the detector The CRD 200 Capillary is optimized for operation at the flow rate range typically used with capillary columns The CRD and tubing connections inside the cartridge are not accessible Tubing exits the front of the cartridge to allow connection to other capillary IC components Installation of a CRD 200 Capillary is optional However if one is not used a CRD bypass cartridge P N 072056 must be installed The bypass cartridge 56 Doc 065342 06 12 11 2 DC Description contains the plumbing connections necessary for eluent and waste flow through the system ey Suppressor Cartridge or Suppressor Bypass Cartridge Two versions of capillary suppressor cartridges are available ACES 300 Anion Capillary Electrolytic Suppressor cartridge P N 072052 and CCES 300 Cation Capillary Electrolytic Suppressor cartridge P N 072053 Each cartridge holds a suppressor and the required tubing connections for eluent and regenerant flow to the suppressor The suppressor and tubing connections inside the cartridge are not accessible Tubing exits the front of the cartridge to allow connection to other capillary IC components When the cartridge is installed in the IC Cube pins on the rear of the cartridge connect the suppressor to its power sourc
29. Dionex ICS 5000 Operator s Manual 8 10 11 12 13 Slide the EGC with the electrolyte reservoir on top into the cartridge holder see Figure 9 20 Figure 9 20 Capillary EGC Installed on Holder Push the EGC electrical cable firmly into the EGC 1 or EGC 2 bulkhead connector see Figure 9 14 Twist the ring on the cable connector fingertight to secure it Unscrew the fitting on the top of the EGC a few turns to vent the EGC To ensure proper ventilation always loosen the fitting on the top of the capillary EGC before operation On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset select the following settings a DC panel Verify that the suppressor Mode is off b EG panel Verify that the CR TC is off To avoid damaging the suppressor and CR TC always turn them off before flushing the EGC The pump flow is on during flushing however no flow reaches the suppressor or CR TC c Pump panel Set the flow rate to 0 02 mL min This turns on the pump flow also Flush the capillary EGC for 20 minutes and then turn off the pump flow Disconnect the temporary tubing from the EGC OUTLET port 342 Doc 065342 06 12 11 9 EG Service Bey Conditioning the Capillary EGC 1 Useahigh pressure blue fitting bolt and ferrule to connect the EGC OUT line from the ELUENT IN port of the CR TC to the EGC OUTLET port see Figure 9 21 2 Disconnect the lines from the ELUENT OUT and REGE
30. For more information refer to the CR TC manual The manual is included on the Thermo Scientific Reference Library DVD P N 053891 NOTE Do not install a CR TC in the same channel as an EGC KCO or an EPM III Electrolytic pH Modifier NOTE The Thermo Scientific Dionex IonPac ATC HC Trap Col umn P N 059604 or Thermo Scientific Dionex IonPac CTC 1 Trap Column P N 040192 may be used with the EG However both Dionex IonPac trap columns require off line chemical regeneration Contact Thermo Fisher Scientific for more information 42 Doc 065342 06 12 11 2 EG Description RFIC Eluent Degasser IC For analytical IC systems an RFIC Eluent Degasser P N 062137 is installed on the EG component mounting panel The degasser contains a tubing assembly that purges the electrolysis gas from the freshly generated eluent before it is directed to the separator column Bay For capillary IC systems the degasser is installed in the IC Cube see Section 2 11 2 Backpressure Coil Optional IC For analytical IC systems the EGC 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 injection valve and the EGC OUTLET port For details refer to Section 9 17 EPM Ill Electrolytic pH Modifier and Carbonate
31. Fuse Requirements Two IEC 60127 2 slow blow fuses P N 954773 rated at 2 A 250 V Doc 065342 06 12 11 A EG Specifications ICS 5000 EG Eluent Generator Specifications Continued Physical Dimensions h x w x d 41 x 23 x 56 cm 16 x 8 75 x 21 5 in Weight 25 kg 40 Ib without optional items Flow Path All polymeric PEEK anion or cation configurations Environmental Operating Temperature 4 40 C 40 104 F Operating Humidity 5 95 relative humidity noncondensing ICS 5000 ER Eluent Regeneration Specifications Analytical IC Only Eluents Carbonate and carbonate bicarbonate combinations up to 20 mM MSA up to 34 mM Flow Rates 1 00 2 00 mL min Continuous Operation with 4 L of Eluent Up to 28 days or 2000 samples typically Always On Always Ready Capable Yes standard feature Remains Fully Calibrated for Extended Periods of Time lt 28 Days Yes standard feature Results are traceable to a single calibration System Wellness Consumables usage monitoring for predictive maintenance Maximum Operating Pressure 21 MPa 3000 psi Operating Temperature Range 4 40 C Doc 065342 06 12 11 421 Dionex ICS 5000 Operator s Manual 422 Doc 065342 06 12 11 ICS 5000 aaa DC Specifications Dionex ICS 5000 DC Detector Chromatography Compartment Specifications Dual Te
32. 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 improved performance when dealing with dirty matrices The MS detector is equipped with FastLock probes for two complementary ionization techniques atmospheric pressure chemical ionization APCD and electrospray ionization ESI During a scan ions of selected mass to charge ratios are sequentially transmitted through a quadrupole mass filter analyzer The MS detector can perform both full range scans and selected ion monitoring SIM scans 10 Doc 065342 06 12 11 1 Introduction 1 1 2 Dionex ICS 5000 System Control The Dionex ICS 5000 system is controlled by a PC configured with Thermo Scientific Dionex Chromeleon 7 Chromatography Data System release 7 0 SRI or later or Thermo Scientific Dionex Chromeleon 6 8 Chromatography Data S
33. P N 042772 10 cc syringe P N 054578 Seal insertion tool P N 063675 Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 063342 316 Doc 065342 06 12 11 9 DP SP Service Additional items Cleanroom gloves lint free particle free and oil free Small beaker ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Methanol optional 0 2 micron filtered Class 10 isopropyl alcohol IPA Lint free paper towels KIMWIPES or equivalent Large flat blade screwdriver 0 2 micron filtered canned air duster ITW Chemtronics Ultrajet or equivalent 9 7 1 Removing the Pump Head and Piston 1 2 Turn off the pump flow Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following e Disconnect the pump from the software by clicking Connected on the Pump panel 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 Five red Phillips screws are installed on the component mounting panel before shipment from the factory Remove these screws if present Use the handles on the component mounting panel t
34. Prepare the samples see page 147 Fill the autosampler vials and load the sample tray see page 149 Start Chromeleon see page 149 Set up the eluent reservoirs see page 153 Set up the piston seal wash system see page 154 Start the pump see page 157 Set the pressure limits see page 158 OoOdaaqagzeao go If an EG is installed start the EG and set the eluent concentration see page 161 Start the DC see page 165 or TC see page 169 O oO Equilibrate the system and verify operational readiness DC see page 166 TC see page 170 NOTE You can use the Smart Startup feature in Chromeleon to auto mate system startup and equilibration Refer to the Chrome leon Help for details 146 Doc 065342 06 12 11 4 Startup 4 3 4 3 1 4 3 2 Preparing Samples This section provides basic information about collecting storing and preparing samples for analysis 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 that meets the specifications listed in Section 1 5 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
35. Red microbore Black standard bore Injection Valve Plumbing 6 Port Valve 8 Turnon the pump flow Check for leaks from the valve Tighten fittings as required see Section 9 29 9 Close the TC door 9 32 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 Thermo Fisher Scientific Electronics related repair procedures must be performed by Thermo Fisher Scientific personnel NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product war ranty Doc 065342 06 12 11 411 Dionex ICS 5000 Operator s Manual Turn off the pump flow from the Control panel in Chromeleon 6 8 or Chromeleon 7 or press PUMP FLOW on the front of the pump 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 Disconnect each liquid line connected to the valve 4 Unscrew the black locking ring on the front of the va
36. 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 1 is always installed in the lower half of the DP SP enclosure This button is not present on the SP 22 Doc 065342 06 12 11 2 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 a gradient analytical pump pump 1 and an isocratic capillary pump pump 2 Figure 2 4 identifies the pump components that are unique to a gradient analytical pump Status Bar Priming Valve Secondary Pump Head Primary Pump Head Pressure Transducer Priming Waste Line Peristaltic Pump for seal wash system Vacuum Degas Chamber one channel Eluent Supply On Off Valve isocratic pumps only Tubing Chase 2 e n F avan es eeee 8 8 000000000 Pulse Damper Outlet capillary pumps only Handle 2 Piston Seal Wash Reservoir 14 Leak Sensor Figure 2 3 Example DP Interior Components Pump 1 Analytical Gradient Pump Pump 2 Capillary Isocratic Pump Doc 065342 06 12 11 23 Dionex ICS 5000 Operator s Manual 2 2 1 Vacuum Degas Chamb
37. 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 Thermo Scientific Reference Library DVD 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 Doc 065342 06 12 11 289 Dionex ICS 5000 Operator s Manual 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 changing a secondary column property For a list of primary and secondary properties refer to the Chromeleon Help A Properties cannot be changed A chip card has not
38. egen Out Eluent Out Eluent Eluent gt qu q Eluent Eluent ou VY kdn cu VVAAT Wy gt Regen To inject valve 2 port P 2 In Out In Out Effignt Out gt lt Eluei S I Regen In CR TC 4 w A Fi AS B A trom To the degasser 1 R ge In via the EG rear chase t o Pe To AS Waste 4 Po e m terso gt ae f lt Cantos doe System 1 System 2 To waste es Figure 3 6 Analytical IC Dual RFIC EG System CD CD Doc 065342 06 12 11 135 Dionex ICS 5000 Operator s Manual Pump front view To pump 2 inlet via the pump rear chase DP To pump 1 inlet via the pump rear chase Eluent Deionized Water To waste gt From suppressor 1 Regen Out via the DC rear chase MMI From the ED cell out via the DC rearchase iiaii DC front view From pump 2 EG left side view right side view System 1 System 2 RFIC Eluent Degasser RFIC EGC Eluent Degasser o Fa 3 a a D A 2 N a a Regen Regen Regen Regen Out In Out in 5 D n Eluent Eluent S out Y VA Am Ej m 0 Regen To inject valve 8 Out 2portP 2 3 Out Elug Separator 2 A In 8 Separator 1 To inject valve 1 Regent Eluent port P 2 CR TC Out Stabilizer To the degasser 1 Regen In via the EG rear chase To waste To AS Waste To waste System 1 System 2 Figure 3 7 Analytical IC Dual RFIC EG System
39. installed Analytical Dione ICS 5000 Automation Manager AM IC 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 Dionex ICS 5000 Thermal Compartment TC IC The TC provides a temperature controlled environment for Dionex ICS 5000 chromatography components The TC is intended for applications that do not require conductivity or electrochemical detection The TC is available in four configurations With one 2 position 6 port high pressure injection valve With two 2 position 6 port high pressure injection valves With one 2 position 6 port high pressure injection valve and one 2 position 10 port high pressure injection valve 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 Dionex AS AP Autosampler AS AP The AS AP provides high performance automated sample processing for ion chromatography applications Key features of the AS AP include Excellent reproducibility with RSDs less than 0 3 for full loop injections All PEEK flow paths compatible
40. reagent addition 139 140 Index 16 Doc 065342 06 12 11 Index Capillary IC RFIC EG dual CD and EG system 131 Capillary IC RFIC EG dual CD system 130 Hybrid RFIC EG dual CD analytical and CD capillary system 132 Matrix elimination 137 138 System Wellness 128 T TC VWD PDA Regulator Bracket Kit 35 Temperature calibration DC 64 Temperature control CD 69 Minimizing the effect of variations 70 Temperature compensation 70 Temperature control DC 63 Cell heater 70 Temperature control TC 118 127 Temperature stabilizer TC 8 118 Liquid leaks 300 Operating problem 301 Thermal Compartment TC 3 8 Alarm LED is lighted 115 Digital I O connectors 120 Front description 115 Maintenance 201 202 Moduleware update 278 Oven LED is flashing 116 Oven LED is lighted 116 Rebuilding the injection valve 410 Regulator Bracket Kit 35 Replacing the injection valve pod 411 Service procedures 407 Shutdown procedure 189 Signal cable 121 445 Specifications 433 Theory of operation 127 Trace analyses 9 Trap column 5 Tray autosampler Loading 146 149 Triangle waveform 106 Troubleshooting DC Alarm conditions DC 259 Amperometry cell 271 Error messages DC 259 Liquid leaks DC 270 pH readout always at 7 0 271 pH readout cannot be set to 7 0 272 pH readout nonexistent 273 Reference electrode leaks 274 Reference potential shifts 274 VALVE button not working
41. 0 ee eee eee 349 9 15 1 Removing the Old CR TC o 350 Doc 065342 06 12 11 xi Dionex ICS 5000 Operator s Manual 9 15 2 Installing and Flushing the New CR TC 350 9 15 3 Completing the New CR TC Plumbing 353 9 16 Replacing the RFIC Eluent Degasser 0 355 9 17 Installing a Backpressure Coil 0 000002 ee eae 355 9 18 Changing the EG Main Power Fuses 000 4 357 DG Service ccc het eee inner eR ve Whee ed lai 359 9 19 Replacing Tubing and Fittings LL 359 9 19 1 Tubing and Fittings for Capillary IC Systems 359 9 19 2 Tubing and Fittings for Analytical IC Systems 362 9 20 Connecting a Sample Loading Port to the Injection Valve 363 9 21 Replacing the Leak Sensor 364 9 22 Rebuilding a High Pressure Injection Valve 366 9 23 Replacing a High Pressure Injection Valve Pod 367 9 24 Installing or Replacing an I O Option Board 369 9 25 Changing the DC Main Power Fuses 000 4 371 9 26 IC Cube Service Procedures 00 eee ee eee 372 9 26 1 Replacing an IC Cube Cartridge 372 9 26 2 Replacing Capillary Columns 374 9 27 CD Service Procedures 0 eee eee 379 9 27 1 Calibrating the CD Cell 0 04 379 9 27 2 Replacing an Analytical Suppressor 381 9 27 3 Replacing a CD rnst ieni sac
42. 0 35 Potential Volts 0 10 ee 0 60 Integration 0 0 0 2 0 4 0 6 0 8 Time Seconds E su i Ei i Positive Cleaning Potential E1 E2 Jes E4 E4 Negative Cleaning Potential Figure 2 51 Example Integrated Amperometry Waveform With the example waveform shown in Figure 2 51 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 Doc 065342 06 12 11 2 DC Description 2 19 3 2 19 4 Cyclic Voltammetry 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 Chromeleon 6 8 supports cyclic voltammetry 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
43. 11 107 Dionex ICS 5000 Operator s Manual Chromeleon provides several pre programmed waveforms 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 54 Waveform Editor fx Waveform Gold IPAD 2 v Description Amino Acids Ag AgCl R ef _ Reference Electrode Mode pH s Waveform No Time s Yoltage GainRegion Ramp Integration Append 1 0 0000 0 1300 off Ramp Off 2 0 0400 0 1300 Off Ramp Off 3 0 0500 0 3300 off Ramp off 4 0 2100 0 3300 On Ramp on 5 0 2200 0 5500 On Ramp On 6 0 4600 0 5500 On Ramp On 7 0 4700 0 3300 On Ramp On 8 0 5600 0 3300 Off Ramp off 9 0 5700 1 6700 off Ramp Off 10 0 5800 1 6700 off Ramp Off 11 0 5900 0 9300 off Ramp Off 12 0 6000 0 1300 off Ramp Off Apply Exit Figure 2 54 Waveform Editor in Chromeleon 7 To view the Waveform Editor click Edit on the ED Options page in the Instrument Method Wizard Chromeleon 7 or Program Wizard Chromeleon 6 8 Analytical vs Scanning Waveforms The pre programmed analytical waveforms supplied with Chromeleon 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 50 or while a series of step
44. 115 126 285 Humidity sensor 126 285 Hybrid system configuration 129 132 I T O option DC 82 83 444 5V output 83 Analog outputs 83 Connections 84 Power output 87 Relay outputs 83 TTL inputs and outputs 83 IC Cube 55 Cartridge replacement procedure 372 373 Column cartridge 58 Column heater 58 CRD bypass cartridge 56 CRD cartridge 56 EG degas cartridge 58 Flow schematic for conductivity detection 59 Flow schematic for electrochemical detection 60 Suppressor bypass cartridge 57 Suppressor cartridge 57 Tubing and fittings 360 ICS 5000 Automation Manager AM See Automation Manager AM ICS 5000 Conductivity Detector CD See Conductivity Detector CD ICS 5000 Detector Chromatography Module See Detector Chromatography Module DC ICS 5000 Dual Pump DP See Dual Pump DP ICS 5000 Electrochemical Detector ED Doc 065342 06 12 11 Index 9 Dionex ICS 5000 Operator s Manual See Electrochemical Detector ED ICS 5000 Eluent Generator EG See Eluent Generator EG ICS 5000 Eluent Organizer EO See Eluent Organizer EO ICS 5000 IC System Overview 1 2 11 Software control 11 User manuals 14 15 ICS 5000 Single Pump SP See Single Pump SP ICS 5000 Thermal Compartment TC See Thermal Compartment TC Injecting samples 180 Injection ports Loading with a syringe 179 Injection valves DC 65 Flow schematics 10 port valve 68 Flow schematics 4 port valve 6
45. 16 DC Rear Panel Figure 2 31 illustrates the rear panel of the DC om Cae TIMI MNI a III IITITTITMIIK SE LULA RIN IMM nen Tubing Chase 2 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 Drain Port O O 6 8 O86 Figure 2 31 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 80 Doc 065342 06 12 11 2 DC Description Switched AC Sockets The two AC receptacles can be used to control the power to external devices Use Chromeleon to switch the power on and off TTL inputs can also be used to control the AC sockets see Section 2 17 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 22 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 o
46. 196 437 EG 197 SP 193 196 437 TC 202 Application Wizard 174 176 Applications 129 139 AS Autosampler 3 9 Example program instrument method 182 Needle seal assembly 359 362 AS AP Autosampler 8 Example program instrument method 181 AS DV Autosampler Example program instrument method 181 ASRS 300 71 Atlas Electrolytic Suppressor AES 62 Gas separator waste tube 72 Audit Trail 22 37 Error messages 203 Icons 203 Automation Manager AM 3 94 Description 8 94 High pressure valves 96 Low pressure valves 97 Ordering 443 RCH 1 Reaction Coil Heater 101 Autorecycle mode 73 74 Autosampler Controlling with relays TTLs 87 Filling vials 146 149 Injecting samples 178 Loading the tray 146 149 Sample loading 178 Autozero 167 B Background conductivity High 225 Offsetting 167 Backpressure coil CD Reordering 442 Requirements 384 Backpressure coil EG 43 47 Installation 355 Reordering 439 Backpressure excessive Causes of 223 Problems caused by 141 Backpressure low Causes of 223 How to increase 43 141 215 Problems caused by 215 Baseline Noisy or drifting 215 Oscillations 383 Shift 104 Spikes 217 Stability 69 Bottles See Reservoirs eluent Bromate Post column reagent addition 139 Bubbles Removing from the cell 383 Bulkhead connectors EG 44 Index 2 Doc 065342 06 12 11 Index Button descriptions DC 51 DP SP 21
47. 20 Doc 065342 06 12 11
48. 267 Reaction coil over safe temperature 268 Suppressor over current 268 Suppressor over power 268 Suppressor over voltage 269 Upper leak sensor wet 269 Error messages DP SP 227 234 Abnormal drive current 227 Camshaft index too early 228 Camshaft index too late 228 Camshaft sensor always alight 228 Degasser malfunction 228 Excessive drive current 229 Function cannot be adjusted by user 234 Invalid flow value 229 Leak detected 229 Maximum purge pressure exceeded 232 Motor malfunction 230 Motor position error 230 Pressure fallen below lower limit 231 Pressure in working cylinder exceeded safety limit 233 Program with this name already exists 227 Pump block carryover pressure too high 230 Relay 4 configured for inject synchronization 232 System pressure exceeded safety limit 233 Upper pressure limit exceeded 234 Error messages EG 241 253 CR TC mode is off for a virtual pump 243 CR TC over current 242 CR TC stopped due to zero flow 243 EG cartridge disconnected 244 EG invalid concentration 245 EG invalid flow 246 EG invalid flow rate concentration 246 EG over current 247 EG over power 248 EG over voltage 248 249 Leak sensor wet 252 Error messages TC AcqOff with previous AcqOn 275 Acquisition still on at program end 275 All samples must specify same value 275 Can t execute Disconnect command 276 Can t execute Standby comm
49. 3 4 Analytical IC Single System with no EG CD Doc 065342 06 12 11 133 Dionex ICS 5000 Operator s Manual Pump front view SP Seal Wash Pump To the pump inlet via the pump rear chase pump not to scale D Fi Deionized Water Vz eg S j 4 Valve gt From the suppressor Regen Out via the DC rear chase To waste DC front view EG left side view RFIC EGC Eluent Degasser Regen Regen Cell In Cell Out Regen Out Eluent Out p 5 Sam l 4 emp wl i A tabilizer 6 3 Backpressure Device From AS gt ml Pe To AS Waste co lt To Waste dd Figure 3 5 Analytical IC Single RFIC EG System CD 134 Doc 065342 06 12 11 3 Configurations Pump front view To pump 2 inlet via the pump rear chase To pump 1 inlet via the pump rear chase System 2 To waste pump not to scale Ti Piston Seal System 1 Wash Deionized Deionized Water Water 00 DO Oc To waste E From suppressor 1 Regen Out via the DC rear chase NR p gt From suppressor 2 Regen Out via the DC rear chase i DC front view ce left side view EG System 1 System 2 right side view y RFIC EGC Eluent Degasser RFIC Eluent Degasser 4 Regen Regen Out In Regen Regen Out In Cell In Cell Out Cell In Cell Out sey 1e 1 DI au EIA uj UaBay z JesseBap ay OL
50. 4 Ifthe problem persists contact Technical Support for Dionex products for assistance A IC Cube 1 heater over safe temperature Or A IC Cube 2 heater over safe temperature This error occurs when the temperature of the IC Cube heater exceeds the maximum allowed This error may occur if the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Appendix A for environmental specifications 266 Doc 065342 06 12 11 8 DC Troubleshooting Lower door opened This message occurs when the door to the lower compartment is opened during a run To troubleshoot 1 Verify that the door is fully closed 2 Check for and remove any obstruction 3 If the door is fully closed and the error persists contact Technical Support for Dionex products 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 33 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 2 Tighten fittings or replace tubing and fittings as required Refer to Section 8 26 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray thoroughly to p
51. Amperometry and Integrated Amperometry modes Dirty or pitted conventional nondisposable working electrode Polish the working electrode see Section 9 28 4 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 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 Doc 065342 06 12 11 217 Dionex ICS 5000 Operator s Manual 8 3 Repeat two or three 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 pH Ag AgCl reference electrode glass membrane NOTE To prevent air from becoming trapped in the cell in the future increase the backpressure on the cell by con necting 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 may contain trace contaminants Remake the eluent using ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Poor Retention Time Reproduc
52. Analytical EGC Conditioning EGC Pump at 1 0 mL min for 30 min EGC concentration at 50 mM y To Waste 0 5 mL min 7 MPa 1000 psi backpressure coil Inlet Outlet VA P N 053765 na Temporary connection y To Waste Figure 9 25 Flow Schematic for Conditioning an Analytical EGC 1 Set a small temporary waste container for example a beaker next to the EG Direct the yellow backpressure coil from the EGC OUTLET port to the waste container The backpressure must be at least 1 4 MPa 200 psi 2 On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset select the following settings a DC panel Verify that the suppressor Mode is off b EG panel Verify that the CR TC is off IMPORTANT To avoid damaging the suppressor and CR TC always turn them off before conditioning the EGC The pump flow is on during conditioning however no flow reaches the suppressor or CR TC c Pump panel e Gradient pump only Select the correct eluent channel A B C or D e All pumps Set the flow rate to 1 0 mL min This turns on the pump flow also 348 Doc 065342 06 12 11 9 EG Service 3 4 d EG panel Enter 50 mM in the Target Concentration field This turns on the power to the EGC also e Condition the analytical EGC for 30 minutes Turn off the EGC and CR TC power Turn off the pump flow Completing the Analytical EGC Installation IC 1 Twist the ring on the EGC electrical cable coun
53. CD ED 136 Doc 065342 06 12 11 3 Configurations Sy WOIH BISEMVSV OL To AS Waste lo pump 2 inlet via the pump rear chase Pump front view To pump 1 inlet A via the pump rear chase DP Seal A p Deionized Deionized Water Water carrier From the suppressor Regen Out via the DC rear chase DC front view 4 172 Regen Out luent In 5 O Large Loop he To inject valve sample port Cell In Cell Out Eluent Out lt Backpressure Device S C I e pump not to scale Oa Pistoni lo B Seal Ol Wash lo D Pump 1 a _ Oe o to c To waste EG left side view RFIC Eluent Degasser Out Eluent y y A A Eluent In Figure 3 8 Analytical IC Single RFIC EG System with Matrix Elimination Using a DP and a 6 Port Valve Doc 065342 06 12 11 137 Dionex ICS 5000 Operator s Manual To pump 2 inlet via the pump rear chase Pump front view Injection Valve To pump 1 inlet A via the pump rear chase DP Connections Key ae o Wash Concentrator E y E To column E Pump 2 2 a Sample in Eluent in ER Mixer lt a Nave To waste To waste pump not to scale Piston Carrier pump in To waste Deionized Deionized Pump 1 Water Water carrier A E Mixer Y DO Oc UE css To waste From the suppressor Reg
54. Chromeleon 6 8 2 Check the sample loop for blockage Clean or replace the loop if needed 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 e ED Verify that the signal cables from the cell are connected to the detector block 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 see Figure 8 1 Push here to ensure that the detector s electrical connection is secure Figure 8 1 Detector Connection ED Only e Cell is off Turn on the cell from the detector ePanel in Chromeleon 7 or Control panel in Chromeleon 6 8 Doc 065342 06 12 11 221 Dionex ICS 5000 Operator s Manual 8 7 Tailing Peaks IE IC Excess tubing void volumes Check tubing connections for void volumes CD Long tubing lengths connecting Minimize all tubing lengths between the injection valve and the detector 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 28 4 If you are using a disposable electrode replace it
55. Column over safe temperature This error occurs when the temperature of the column compartment exceeds the maximum allowed This error may occur if the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Appendix A for environmental specifications 260 Doc 065342 06 12 11 8 DC Troubleshooting Column temperature calibration error To troubleshoot Repeat the calibration procedure Follow the instructions provided in the DC Temperature Calibration Kit P N 063782 If the error appears again contact Technical Support for Dionex products for assistance Compartment temperature open circuit This error may indicate a problem in the detector electronics Contact Technical Support for Dionex products 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 Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Appendix A for environmental specifications Compartment temperature calibration error To troubleshoot Repeat the calibration procedure following the instructions provided in the DC Temperature Calibration Kit P N 063782 If
56. Conductivity Detector and Accessories for Analytical IC 061716 Dionex ICS 5000 Conductivity Detector Analytical 056116 AAES Anion Atlas Electrolytic Suppressor 056118 CAES Cation Atlas Electrolytic Suppressor 064555 ASRS 300 2 mm Anion Self Regenerating Suppressor 064556 CSRS 300 4 mm Cation Self Regenerating Suppressor 064557 CSRS 300 2 mm Cation Self Regenerating Suppressor 045460 Suppressor gas separator waste tube 045877 Backpressure coil for 4 mm suppressor 045878 Backpressure coil for 2 mm suppressor Electrochemical Detector and Accessories for Capillary and Analytical IC 072042 Dionex ICS 5000 Electrochemical Detector ED without cell 072044 ED cell 061879 pH Ag AgCl reference electrode 014067 O ring for pH Ag AgCI reference electrode for analytical 072162 Gasket for pH Ag AgCl reference electrode for capillary 072075 PdH reference electrode 072214 Gasket for PdH reference electrode 061749 ED gold conventional working electrode with gasket and polishing kit 061751 ED platinum conventional working electrode with gasket and polishing kit 061753 ED glassy carbon conventional working electrode with gasket and polishing kit 061755 ED silver conventional working electrode with gasket and polishing kit 045972 Gasket PTFE 0 001 in for conventional working e
57. DC column compartment IC Cube CD cell heater reaction coil heater Click Monitor Background on the toolbar above the Chromeleon 7 ePanel Set or on the Home panel of the Chromeleon 6 8 panel tabset Chromeleon begins plotting the detector signal and pump pressure readings 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 Thermo Scientific Reference Library DVD P N 053891 166 Doc 065342 06 12 11 4 DC Startup 4 Offset the detector background and zero the reading by clicking the Autozero button 5 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 6 Monitor the DP SP pressure and make sure it is at the expected reading for the installed column and it is stable 7 Verify that all installed temperature control devices are at their set points and are stable The system is now ready for operation Be Because capillary IC systems use low flow rates and consume very little eluent you can leave a capillary IC system on at all times allowing it to remain equilibrated and always ready to run the next sample Doc 065342 06 1
58. DP SP B Reordering Information DP SP Reordering Information Part Number Item Pump Head Components 074447 capillary 062083 analytical Primary pump head 074240 capillary 062079 analytical Secondary pump head 044541 capillary 045722 analytical Inlet check valve assembly for primary pump head includes inlet nut and 1 8 in cartridge 044520 capillary 045721 analytical Outlet check valve assembly for primary pump head includes outlet nut and 1 8 in cartridge 075493 capillary 064946 analytical Main piston seal 074371 Backup ring for capillary pumps 040695 O ring for capillary or analytical pump 074446 capillary 062064 analytical Seal wash body 068628 capillary 063382 analytical Piston seal wash seal 068627 capillary 062092 analytical Retainer for piston seal wash seal 068646 capillary 062082 analytical Piston 063968 Priming valve for secondary pump head for capillary or analytical pump 063382 Priming valve knob seal for secondary pump head for capillary or analytical pump Doc 065342 06 12 11 435 Dionex ICS 5000 Operator s Manual Part Number Item Piston Seal Wash System 064155 Piston seal wash reservoir 063268 PharMed tubing 0 159 cm 0 0625 in ID Note Order 12 in of tubing for replacement of piston seal wash tubing 064079 Tygon 2075 tubi
59. Detector Chromatography Module DC 2 7 Alarm LED is lighted 51 Automation Manager AM 94 Electrochemical Detector ED 75 Flow schematics 73 74 Front description 51 T O option 83 Maintenance 199 Rebuilding the injection valve 366 Service procedures 359 Spare parts 441 Specifications 423 System configuration 129 Temperature control 63 Disposable working electrodes 75 Reordering 443 Drain port TC 121 Drifting baseline 215 Dual Pump DP 2 3 Analog pressure output 32 Digital I O port 31 Fuse replacement 330 Fuses 31 Maintenance annual 196 Maintenance daily 195 Maintenance periodic 196 Maintenance weekly 195 Operating humidity 417 Operating temperature 417 Piston replacement procedure 323 Piston seal replacement procedure 316 321 323 324 Piston seal wash tubing replacement procedure 326 Pressure limit tripped 223 255 256 Pressure limits for EG 158 Priming procedures 308 311 Priming valve knob seal replacement 329 Product warranty 303 Pulse damper for capillary pump 27 Selecting pressure limits 158 Shutdown procedure 183 Spare parts 435 Specifications 415 Start up procedures 153 Static mixer 27 Status bar buttons and LEDs 21 System configurations 129 137 USB connections 33 Waste lines 33 Dual system configuration 132 135 136 E EC cell See Amperometry cell ED cell See Amperometry cell ED cell disconnected error 261 264 EGC
60. EGC power supply for the second channel Thus the EG can accommodate only one such configuration 44 Doc 065342 06 12 11 2 EG Description 2 8 EG Rear Panel Figure 2 12 illustrates the rear panel of the Dionex ICS 5000 Eluent Generator EG Exhaust Fan Gas Vent Lines USB Receptacle B Connector o ce USB Ports 2 A Connectors Fuse Holder Main Power Switch and Power Receptacle Tubing for Connecting to Suppressors Tubing Chase O Drain Port Figure 2 12 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 is installed e Two USB Universal Serial Bus ports A type connectors are provided for connections to other Dionex ICS 5000 modules Doc 065342 06 12 11 45 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT One 1 8 m 6 ft USB cable P N 960777 is provided in the EG Ship Kit P N 072047 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 18 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 o
61. For conventional nondisposable electrodes clean the working electrode with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Dry with pressurized air or nitrogen If the electrode is pitted polish the electrode see Section 9 28 4 Check the value of the reference potential shift see Using a Digital Voltmeter to Determine Reference Potential Shift on page 274 If the value fluctuates by more than 30 mV electrode passivation may occur because potentials that are too high are being applied Recalibrate the pH Ag AgCl reference electrode see Section 9 28 6 If the problem persists replace the pH Ag AgCl reference electrode see Section 9 28 5 Analog Output Option e Analog output range set too high Select a more sensitive analog output range 224 Doc 065342 06 12 11 8 Troubleshooting 8 11 High Background CR TC is contaminated Clean the trap column as instructed in the CR TC manual The manual is included on the Thermo Scientific Reference Library DVD P N 053891 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 Background signal not offset from detector signal Before injecting sample allow the background signal to equilibrate and then press Autozero on the detector ePanel in Chromeleon 7 or Control panel in Chromeleon 6 8
62. Gasket for Capillary IC 396 Doc 065342 06 12 11 9 DC Service 4 Make sure the gasket is centered in the bottom of the well and that it does not block the inlet and outlet of the well The inlet and outlet are small round openings in the bottom of the well see Figure 9 61 Reference Electrode Well Inlet Reference Electrode Well Outlet Figure 9 61 Reference Electrode Well with Reference Electrode Gasket for Capillary IC Installed 5 Verify that the reference electrode O ring has f been removed and the reference electrode gasket is correctly installed in the bottom of the well 6 Screw the pH Ag AgCl reference electrode into the reference electrode well and tighten it fingertight see Figure 9 62 Figure 9 62 Installing the pH Ag AgCI Reference Electrode In the Reference Electrode Well 7 Orient the cell assembly with the yoke knob on the left and then push the cell onto its mounting location on the ED 8 Connect the reference electrode cable and the cell cable 9 Reconnect the cell inlet and outlet lines Doc 065342 06 12 11 397 Dionex ICS 5000 Operator s Manual 10 11 12 Analytical l 7 Analytical IC System a SN OY 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 Installing the pH Ag AgCl Reference Electrode in the Cell for an To avoid any hydraulic pressure buildup w
63. IC Shown 4 Grasp the cell by the cell body and pull straight out to remove it from the detector Doc 065342 06 12 11 385 Dionex ICS 5000 Operator s Manual 9 28 2 Replacing an ED Cell Disposable Working Electrode Gasket For installation instructions for disposable working electrodes refer to the installation guide shipped with the electrodes see below or to Product Manual for Disposable Electrodes Document No 065040 which is included on the Thermo Scientific Reference Library DVD P N 053891 e Disposable Silver Electrode Installation Guide for ED Document No 065137 e Disposable Platinum Electrode Installation Guide for ED Document No 065139 e Disposable Gold Electrode Installation Guide Document No 065191 When you install a disposable electrode make sure that you install IMPORTANT the correct gasket for your system e Fora capillary system use a 0 001 in PTFE gasket P N 072117 Pkg of 2 e For an analytical system with a gold silver or platinum disposable electrode use a 0 002 in PTFE gasket P N 069141 Pkg of 4 e Foran analytical system with a carbon disposable electrode use a 0 001 in Ultem gasket P N 069339 9 28 3 Replacing an ED Cell Conventional Working Electrode Gasket 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 ED cell gasket for conventional working electrode
64. Mixer IC The EGC II KCO can be used with an EPM III Electrolytic pH Modifier P N 080135 and a carbonate mixer P N 061686 4 mm P N 063443 2 mm to produce a carbonate bicarbonate mixture for use with anion exchange separations on carbonate based Dionex IonPac columns After the cartridge generates potassium carbonate eluent the EPM adjusts the eluent concentration to produce the carbonate bicarbonate mixture The carbonate mixer provides mixing necessary to produce a homogenous solution of electrolytically generated KxCO3 and KHCO eluent For more information about these products refer to the EGC manual EGC manuals are included on the Thermo Scientific Reference Library DVD 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 and an error message is displayed in the Audit Trail In addition the Alarm LED on the EG front panel lights Doc 065342 06 12 11 43 Dionex ICS 5000 Operator s Manual 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 EGCs or one EGC and one EPM and e Two CR TCs When operating with an EGC II K CO3 and the EPM III the EGC is connected to the EGC power supply for one channel and the EPM is connected to the
65. N o OH COM Dee n c O Non Energized Relay N O COM N C ollo lo Da Energized Relay NOTES 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 35 Relay Output Configuration 88 Doc 065342 06 12 11 2 DC Description You can control the power relays and TTL outputs from the DC ePanel in Chromeleon 7 see Figure 2 36 or the DC Control panel in Chromeleon 6 8 ICS 5000 Home AS Pump DC CD ED EG Audit Queue a Ocoee Detector Compartment Compartment Column Reaction Coil J a m e m Serial Number 123456789012 i 7 i g Statue Heat Set 00t E se foot set 350 C 5 Lower Door Closed Upper Door Closed Ooo OOO O M Dutput Relays and TTLs Input TTLs Inj 1 Load bem TTL Ov Inj 2 LoadPosition pc TT By a TUE NY a ee TTL3 Ov Suppressor 1 DC_RELAY_1 Open Ov Type None v DC_RELAY_2 Open TS Ov TITLE Ov Mode Off v DC_AC_RELAY_1 Open TU ov Current 0 m E DC_AC_RELAY 2 Open 4 TTL Ov Flow_detected 250 Suppressor 2 Tune None v ran v Figure 2 36 Output Relays and TTL Control on DC ePanel in Chromeleon 7 NOTE Itis possible to change the settings for the power relays and TTL outputs while a Chromeleon 7 instrument
66. Operator s Manual 9 7 2 Cleaning the Piston 1 Place the piston in a beaker containing either ASTM Type I 18 megohm cm filtered and deionized water or methanol Sonicate for several minutes After cleaning rinse the piston thoroughly with ASTM Type I 18 megohm cm filtered and deionized water 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 8 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 9 7 3 Removing the Main Piston Seal 1 5 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 and into the piston cavity in the pump head Reinsert the piston 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 If the piston seal w
67. P N 053891 3 Create a sequence in Chromeleon that specifies the vials from which to take sample injections and the order in which the injections should be run 4 Specify a Chromeleon 7 instrument method or Chromeleon 6 8 program that includes the appropriate load and inject commands for the autosampler See the examples in Section 5 4 Loading Samples with a Syringe This section describes two methods for using a syringe to load sample into the DC injection valve sample loop e Loading sample with a syringe through the sample loading port on the front of the DC push method e Loading sample with a vacuum syringe through the sample loading port on the front of the DC pull method Loading Samples with a Syringe Push Method 1 Verify that a luer adapter fitting is installed on the sample loading port on the front of the DC and that tubing is connecting the sample loading port 178 Doc 065342 06 12 11 5 Operation to the sample port on the injection valve If not refer to Section 9 20 for connection instructions Fill a syringe with a calibration standard or sample Insert the syringe into the sample loading port on the front of the DC Verify that the injection valve is in the Load position If it is not switch the valve by clicking the valve control on the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset or by pressing the VALVE button on the front of the DC Overfill the sample loop with severa
68. See also Reference electrode Photodiode Array Detector 3 9 Regulator Bracket Kit 35 Piston seal wash solution 26 183 Piston seal wash system 26 154 Activation 26 Dual pump seal wash option 27 154 436 Replumbing the DP connections 154 Setup 156 Piston seals Replacement procedure 316 Pistons Replacement procedure 323 Platinum working electrodes 75 Plot I t 111 Plumbing Replacing DC tubing and fittings 359 Replacing DP SP tubing and fittings 306 Replacing EG tubing and fittings 333 Replacing TC tubing and fittings 407 Plumbing configuration drawings 129 139 Polarity Analog output 86 Polishing kit ED Reordering 443 Polishing working electrodes 389 Post column reagent addition 61 94 139 Potassium carbonate eluent 41 43 Potassium hydroxide eluent 41 Index 12 Doc 065342 06 12 11 Index Potential shifting 77 274 Power cord 357 370 371 413 Power LED DC 52 Power LED DP SP 22 Power LED EG 38 Power LED TC 116 Power output DC T O option 82 83 87 Power receptacle DC 81 DP SP 30 EG 46 TC 119 Power switch rear panel DC 81 DP SP 30 EG 46 TC 119 Pre concentration 61 94 Predictive Performance 128 Pressure limit settings 158 Pressure limits tripped 223 Pressure transducer 25 Pressurizable eluent reservoirs Installation 35 Priming procedures DP SP 308 309 From the Control panel 310 Priming with a syringe 310 311 Priming with th
69. Service 19 Connect the tubing from the Eluent In port of the column cartridge to the Eluent Out port 3 of the injection valve 20 Wait until liquid is flowing out of the Eluent Out port of the column cartridge 21 Reconnectthe line to the Eluent Out fitting on the column cartridge that was disconnected in Step 3 see Figure 9 41 22 Close the DC upper door 9 27 CD Service Procedures 9 27 1 Calibrating the CD Cell NOTE Do notuse 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 KCI in 1 liter of 18 megohm cm DI water Backpressure tubing to Use 0 25 mm 0 010 in ID black PEEK provide at least 7 MPa tubing P N 042690 1000 psi 1 On the Chromeleon 7 ePanel Set click the CD tab On the Chromeleon 6 8 panel tabset click the CD tab Doc 065342 06 12 11 379 Dionex ICS 5000 Operator s Manual 2 Under Detector Settings click Calibration The Wellness panel opens 10 11 see Figure 9 49 Ss Conductivity Detector Wellness External Conductivity Cell Calibration Update Wellness Database Press forinstructions Instructions Press for instructions Instructions Cond Cell Calibration Calibrate Settings to Download Current gt Log Cell 1 Cal Value Log Download in Process Log Cell 2 Cal Value Log Cell Serial Number Current Calibration D
70. Shift 1 For each pH Ag AgCl reference electrode the unexposed electrode and the electrode being tested use a straightened paper clip or short piece of wire of a suitable diameter to connect the voltmeter s voltage inputs to pin on the reference electrode s cable connector To identify the cable connector pins refer to Product Information Update for the Electrochemical Detector PIU_ED_1 The document is included on the Thermo Scientific Reference Library DVD P N 053891 Immerse both 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 30 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 28 7 274 Doc 065342 06 12 11 fa TC Troubleshooting 8 29 Troubleshooting TC Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon Audit Trail AcqOff without previous AcqOn This error occurs if the Chromeleon 7 instrument method or Chromeleon 6 8 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 7 instrument method or Chromeleon 6 8 pr
71. Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 270 Doc 065342 06 12 11 8 DC Troubleshooting 8 27 VALVE Button Not Working The VALVE 1 and VALVE 2 buttons on the front of the DC must be enabled in Chromeleon 6 8 or Chromeleon 7 in order to use them to manually switch the inject valves To enable a button open the Commands dialog box and select the Valve1 Button or Valve2Button command in the list of commands for the DC 8 28 ED Cell Troubleshooting 8 28 1 ED Cell pH Readout Always 7 0 The pH reading of the pH Ag AgCl reference electrode is displayed on the Chromeleon 7 ED ePanel or the Chromeleon 6 8 EC Detector panel e Disconnected pH Ag AgCl reference electrode Verify that the reference electrode cable is securely connected see Figure 8 8 Check the cable connection Figure 8 8 ED Cell Electrical Connections e Reference electrode short circuit Replace the reference electrode see Section 9 28 5 e pH Ag AgCl reference electrode glass membrane broken or cracked Replace the pH Ag AgCl reference electrode see Section 9 28 5 Doc 065342 06 12 11 271 Dionex ICS 5000 Operator s Manual 8 28 2 Cannot Set ED Cell pH Readout to 7 0 8 28 3 The pH reading of the pH Ag AgCl reference electrode is displayed on the ED ePanel in Chromeleon 7 or the EC Detector Control panel in Chromeleon 6 8 e Inaccurate calibration buffer Use a pH met
72. The TC is at its set The TC is transitioning to temperature 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 Does not flash LED 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 62 116 Doc 065342 06 12 11 2 TC Description 2 21 TC Interior Components Figure 2 61 illustrates the interior of the TC The components installed in your TC may vary depending on your application Slots for Column ID Chip 1 Cards A B C and D 4 Guard Column 2 Injection Valves O Column Brackets Separator Column O Temperature Stabilizer Figure 2 61 TC Interior View Dual System Configuration Shown 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 23 for details about the injection valves Column Brackets The column brackets are installed in the TC at the factory The TC can hold up to thre
73. Type I 18 megohm cm filtered and deionized water 6 Dry the reservoir with clean particulate free air 9 5 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 air This section describes two methods for priming the pump e To prime the pump with the PUMP PRIME button see Section 9 5 1 e To prime the pump from the Pump panel in Chromeleon see Section 9 5 2 Although a 10 cc syringe P N 054578 can be used with either priming procedure using a syringe only if eluent lines are 100 empty or if the pump is dry is recommended 308 Doc 065342 06 12 11 9 DP SP Service 9 5 1 Priming with the PUMP PRIME Button 1 On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab Gradient pump only Enter 100 for the channel A B C or D to be primed Set the priming flow rate to the desired rate The default rate for a capillary IC pump is 3 0 mL min The default rate for an analytical IC pump is 6 0 mL min Disconnect the DP SP from the software by clicking Connected on the Pump panel NOTE When the pump is connected to Chromeleon the PUMP PRIME buttons are disabled Open the priming valve on the secondary pump head see Figure 9 2 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
74. USB Receptacle 0 B Connectors USB Ports 3 A 6 Connectors Exhaust Port from Vacuum Degas Module Drain Port Figure 2 7 DP SP Rear Panel Tubing Chases The tubing chases route tubing 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 30 Doc 065342 06 12 11 2 Description 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 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 11 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
75. Using IPA rinse inside the pump head cavity where the seal will be installed Blow inside the cavity to dry it using the 0 2 micron filtered canned air duster Inspect the cavity for any particulate matter If necessary rinse and dry again until the cavity is clean Fill the cavity with ASTM Type I 18 megohm cm filtered and deionized water Place the components on the pump head and gently press the housing until the piston seal snaps into place When pressing the seal in place ensure that the piston is free to move out to relieve the pressure in the pump head during seal installation 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 Remove the 10 32 fitting plugs from the pump head 322 Doc 065342 06 12 11 9 DP SP Service 9 7 6 9 8 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 the piston should extend from the head 2 Place the pump head back on the pump 3 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 4 Reconnectall tubing connections to the pump head Tighten connectio
76. VALVE W from door inject port or autosampler 25 pL SAMPLE LOOP Orange TO INJECT VALVE P TOINJ _ Red microbore VALVE C Black standard bore Figure 2 66 Injection Valve Plumbing 6 Port Valve 124 Doc 065342 06 12 11 2 TC Description 2 24 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 67 osi e _ mii nie Column Identification System i Ww Column ID Chip Card Figure 2 67 Column ID Identification System The columns to be monitored are selected in the TC Properties dialog box in the Chromeleon 7 Instrument Configuration program or the Chromeleon 6 8 Server Configuration program To select column properties see below for storage and to review the stored information at any time use the TC ePanel in Chromeleon 7 or the TC Control panel in Chromeleon 6 8 The properties are also available in the Chromeleon Commands dialog box 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 pr
77. a new gasket see Section 9 28 3 Turn the yoke knob see Figure 9 53 a full 360 degrees to completely engage the knob 226 Doc 065342 06 12 11 ICS 5000 DP SP 8 12 DP SP Troubleshooting Troubleshooting DP SP Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon Audit Trail A program with this name already exists This error occurs if you attempt to save a modified Chromeleon 7 instrument method or Chromeleon 6 8 program under the name of an existing instrument method or program To troubleshoot Enter a new name for the modified instrument method or program or select Save to save your changes under the existing instrument method or 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 see Section 9 3 Be careful to not overtighten fittings If the message appears again contact Technical Support for Dionex products for assistance Doc 065342 06 12 11 227 Dionex ICS 5000 Operator s Manual Camshaft index too early Or Camshaft index 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
78. 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 concentrations of these ions in the sample In general samples that do not contain nitrite or sulfite can be refrigerated for at least one week with no significant 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 Low Volume High Pressure Inline Filter P N 074505 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 065342 06 12 11 147 Dionex ICS 5000 Operator s Manual 4 3 3 Before injection pretreat samples that may contain high concentrations of interfering substances by putting them through Thermo Scientific Dionex OnG
79. been 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 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Under TC select the column name and select the CardState property 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 A 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 290 Doc 065342 06 12 11 8 TC Troubleshooting 3 Ifthe door is fully closed but the error persists contact Technical Support for Dionex products for assistance A Properties cannot be changed there is no card in the card reader This error occurs if you 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 30 A Raw data file x can
80. before beginning an analysis This allows the DP SP to stabilize the flow rate Enter the minimum and maximum pressure limits Setting pressure limits ensures that the DP SP will automatically stop if a system malfunction occurs Table 4 1 lists the default pressure limits for capillary and analytical pumps Pump Configuration Capillary pump not linked to an EGC Default Low Pressure Limit 0 Default High Pressure Limit 41 MPa 6000 psi Capillary pump linked to an EGC 1 4 MPa 200 psi 35 MPa 5000 psi Analytical pump not linked to an EGC 35 MPa 5000 psi Analytical pump linked to an EGC 1 4 MPa 200 psi 21 MPa 3000 psi Table 4 1 Default Pressure Limits for DP SP Pumps a Capillary IC pumps shipped before February 17 2011 were rated for lower operating pressures than the pumps currently being shipped Refer to the im portant note on the next page for details b If the installed version of EG degas capillary cartridge is not rated for 35 MPa 5000 psi change the default high pressure limit to 21 MPa 3000 psi Refer to the important note on the next page for details 158 Doc 065342 06 12 11 4 DP SP Startup Be IMPORTANT Capillary IC pumps shipped before February 17 2011 were rated for lower operating pressures than the pumps currently being shipped The older pumps can be operated at pressures up to 35 MPa 5000 psi without RFIC and
81. defective Replace both check valve cartridges see Section 9 6 Fluent proportioning valve leaks gradient pump only Tighten loose fittings If there are no loose fittings the proportioning valve assembly should be replaced Contact Technical Support for Dionex products for assistance Doc 065342 06 12 11 237 Dionex ICS 5000 Operator s Manual 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 10 If leaks occurs when the priming valve knob is closed either the pump head or the knob is damaged and should be replaced Contact Technical Support for Dionex products 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 Refer to the troubleshooting steps for the Audit Trail message The system pressure exceeded the safety limit on page 233 8 16 Vacuum Degassing Module Low Vacuum Leak in the vacuum degassing module Check all tubing connections for leakage tighten loose fitting connections 8 17 Vacuum Degassing Module Does Not Run Electrical connections incorrectly installed There may be a problem with the connections from the v
82. 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 Iftheerror persists there may be a problem in the detector electronics Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the user Push here to ensure the detector s electrical connection is secure Doc 065342 06 12 11 259 Dionex ICS 5000 Operator s Manual CD cell over safe temperature This error occurs when the temperature of the conductivity detector is higher than the maximum allowed This error may occur if the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot 1 Refer to Appendix A 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 temperature open circuit This error may indicate a problem in the detector electronics Contact Technical Support for Dionex products for assistance
83. eluent produced by the car tridge A system backpressure of 16 MPa 2300 psi is ideal Analytical IC only 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 analytical IC system RFIC Eluent Degasser has ruptured Replace the degasser see Section 9 16 Doc 065342 06 12 11 255 Dionex ICS 5000 Operator s Manual 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 5 and resume operation DP SP pressure limit tripped Verify that the Current Pressure reading on the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset is between the high and low limits displayed on the panel For details see Section 4 8 NOTE The analytical EGC 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 For a capillary IC system select a flow rate between 0 001 and 0 100 mL min For an analytical IC system select a flow rate between 0 100 and 3 000 mL min Electrical error detected ALARM LED is lighted To prevent dama
84. er Z A To Waste GLI OO renali To Waste ample ample tile y Carrier y Carrier To Waste Pump in To Waste Pump In Sample Eluent se Carrier Figure 2 26 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 26 the flow occurs as follows 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 68 Doc 065342 06 12 11 2 DC Description 2 14 2 14 1 e In the Inject position carrier liquid flows through the sample loop and on 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 CD Conductivity Detector Each Dionex ICS 5000 Conductivity Detector 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 The CD is installed in the upper
85. installable with pre formed tubing and color coded labeling Capillary column heater 15 to 80 C Doc 065342 06 12 11 423 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 DC Detector Chromatography Compartment Specifications Flow Path Plumbing configurations for 4 mm 2 mm and 0 4 mm columns fully inert PEEK Detectors Any combination of two conductivity or electrochemical detectors upgradeable and field installable Dual detectors can be operated simultaneously or independently Optional remote operation up to 3 m from instrument Analog Signal Output Two analog output channels two 24 V relays two TTL Out and eight TTL In lines upgradeable and field installable optional Leak Detection Optical leak sensor standard Application Control Automation Yes standard All DC modules come equipped with two switched AC controllers built in to automate external devices and the ability to control up to six low pressure 2 way or 3 way valves for fluidic automation Suppression Non suppressed conductivity Yes supported Suppressor wear parts None No valves pumps peristaltic pump tubin g or inline filters required Chemical Suppression 2mm and 4 mm anion and cation membrane suppression available Displacement Chemical Suppression 2 mm and 4 mm anion and cation membrane suppression available Electrolytic Suppression Self Regenerating 0 4 mm with o
86. integrated pulsed amperometric detection IPAD see Section 2 19 2 e Cyclic voltammetry see Section 2 19 3 2 19 1 DC Amperometric Detection In DC amperometry a constant potential is applied to the working electrode The potential can be entered into a Chromeleon 7 instrument method see Figure 2 49 or Chromeleon 6 8 program amp Instrument Method Wizard Options ED EDet1 EDet1 Options EDet1 Options for Options ED EDet1 Channels Amperometry Cell Data Collection Rate Autozera v de Di Total On 1 00 KS He O Yes DI O Off No Voltage V Retention min Yoltage Y 1 Initial Time 0 0000 2 0 000 0 0000 Insert Delete All ARE I Asa ondino sitter draft Figure 2 49 DC Amperometry Instrument Method Wizard Page in Chromeleon 7 The applied voltage can be changed up to 10 times during the run The actual number of potential changes allowed depends on the available data storage 102 Doc 065342 06 12 11 2 DC Description 2 19 2 capacity which is determined by the length of the run and the data sampling rate For direct control enter the potentials on the DC ePanel in Chromeleon 7 or the Control panel in Chromeleon 6 8 Integrated and Pulsed Amperometric Detection Integrated and pulsed amperometric detection are similar to DC amperometry see Section 2 19 1 in that molecules are oxidized or reduced at the surface of an electrode However with these detection modes a series o
87. line 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 Doc 065342 06 12 11 113 Dionex ICS 5000 Operator s Manual 114 Doc 065342 06 12 11 Ea TC Description 2 20 TC Front Features A status bar on the front of the Dionex ICS 5000 Thermal Compartment TC includes LEDs light emitting diodes that indicate the status of several TC components and functions see Figure 2 60 LOAD INJECT LOAD INJECT e e e e e e e CONNECTED ALARM VALVE 1 VALVE 2 Figure 2 60 TC Status Bar LED Label If the LED Is On If the LED Is Flashing CONNECTED The TC is connected to a Does not flash Chromeleon 7 instrument or a Chromeleon 6 8 timebase ALARM A sensor detected the Does not flash presence of a gas or humidity leak inside the TC ora valve or oven error was detected Check the Chromeleon Audit Trail for the cause VALVE 1 LOAD Indicates whether the Valve error See VALVE 2 LOAD injection valve is in the Section 8 30 for VALVE 1 INJECT Load or Inject position troubleshooting VALVE 2 INJECT Doc 065342 06 12 11 115 Dionex ICS 5000 Operator s Manual LED Label If the LED Is On If the LED Is Flashing OVEN
88. listed in Section 1 5 Removing the Pump Head and Piston When disassembling and reassembling the pump head refer to Figure 9 6 primary pump head or Figure 9 7 secondary pump head 1 Turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following e Disconnect the pump from the software by clicking Connected on the Pump panel 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 4 Five red Phillips screws are installed on the component mounting panel before shipment from the factory Remove these screws if present 5 Use the handles on the component mounting panel to pull the panel forward until it reaches the stop 324 Doc 065342 06 12 11 9 DP SP Service 6 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 7 Disconnect all tubing connections to the pump head with the damaged piston 8 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 th
89. 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 Technical Support for Dionex products 7 16 TC Annual Maintenance e Thermo Fisher Scientific recommends performing preventive maintenance annually The following kits are available e 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 e 10 Port High Pressure Valve Preventive Maintenance Kit P N 075042 202 Doc 065342 06 12 11 8 Troubleshooting This chapter is a guide to troubleshooting minor issues that may arise during operation of the Dionex ICS 5000 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 Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office Please have this chapter at hand when talking with Technical Support personnel 8 1 Audit Trail Error Messages The instrument control firmware installed in each Dionex ICS 5000 module periodically checks the status of certain parameters If a problem is dete
90. 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 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 There was already an AcqOff command for this channel before Or There was already an AcqOn command for this channel before Or A Two AcqOn commands for the same channel The second chromatogram will overwrite the first A Chromeleon 7 instrument method or Chromeleon 6 8 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 instrument method or program 296 Doc 065342 06 12 11 8 TC Troubleshooting This function cannot be adjusted by the user This error occurs if you attempt to change the setting for a read only parameter To troubleshoot Do not attempt to reset read only parameters This operation may affect the oven s operation on timeb
91. port analytical EGC This will prevent the evaporation of water in the electrolyte reservoir 2 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 Section 9 14 4 for a capillary EGC or Section 9 14 5 for an analytical EGC Ba If you are replacing a capillary EGC go on to Section 9 14 4 If you are replacing an analytical EGC go on to Section 9 14 5 IC Doc 065342 06 12 11 339 Dionex ICS 5000 Operator s Manual aay 9 14 4 Installing and Conditioning a New Capillary EGC Figure 9 18 shows the EG flow schematic for a capillary IC system Refer to this figure when performing EGC and CR TC service procedures in a capillary IC system Tubing Assembly Key 1 0 25 mm 0 010 in ID Black PEEK 86 cm 34 in P N 068658 0 062 mm 0 0025 in ID Blue 47 Vent PEEK 18 cm 7 in P N 072204 A 0 062 mm 0 0025 in ID Blue Capillary PEEK 61 cm 24 in P N 072203 0 25 mm 0 010 in ID Black PEEK 64 cm 25 in P N 072224 1 58 mm 0 062 in ID Clear ETFE 2 1 m 7 ft P N 072225 TO PUMP DAMPER WASTE GAS B SEPARATOR EG Degas Cartridge inside DC To inject Gm Valve Figure 9 18 EG Flow Schematic Example for Capillary I
92. required to compress eluent in the pump head During the pre compression phase pulsation is minimized 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 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 Proportioning Valves Gradient pump only In the gradient pump which is available for analytical IC applications only eluent flows from the eluent reservoirs through the vacuum degas chambers and into a four way proportioning valve assembly see Figure 2 4 Programmed percentages of each eluent are proportioned by the four valves 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 pump only pump heads and detector cell Degassing eluents is especially important when combining aqueous and nonaqueous components for example water and acetonitrile The vacuum dega
93. short between the working electrode contact and the cell body If the conventional nondisposable working electrode becomes discolored or if you notice a degradation in performance baseline noise tailing peaks etc polish the electrode as instructed in Section 9 28 4 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 see Section 9 28 4 To help determine when the pH Ag AgcCI reference electrode needs regenerating or replacing monitor the pH value displayed on the detector panel in Chromeleon see page 144 To have an alarm displayed in the Audit Trail if the pH exceeds certain values set pH limits in Chromeleon see page 145 Doc 065342 06 12 11 143 Dionex ICS 5000 Operator s Manual To monitor the pH Ag AgCl reference electrode pH 1 At installation calibrate the pH electrode see Section 9 28 6 2 When you run your first chromatographic instrument method or program note the pH value displayed on the Chromeleon panel see Figure 4 1 ICS 5000 Home AS Pump DC CD ED Audit Queue Detector Settings DCAmp 600 Mode 400 Ref Electrode pH Rise Time zoo Data Collection Rate 1 00 Hz 2 o Reference Electrode AgCI
94. 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 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 On the 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 37 Save the screws Remove two screws Figure 9 37 DC Rear Panel Removing the I O Option Cover Plate 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 370 Doc 065342 06 12 11 9 DC Service Figure 9 38 shows the I O option installed I PAS IIITINIIKIKI IHU e IIITIITIKINI MALANIN TITTI TINI ees INI a mim CI 1 0 Option Figure 9 38 DC Rear Panel I O Option Installed 7 Reconnect the main power cord and turn on the power 9 25 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 31 3 Disconnect the main power cord from both its source and from the DC rear panel HIGH VOLTAGE Disconnect the ma
95. 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 removes any liquid that collects in the drip tray in the bottom of the TC A clear corrugated drain hose P N 055075 is connected to this port during installation Place the drain hose into a waste container To maintain a positive siphon position the waste container below the level of the TC For correct drainage make sure the drain hose is not bent pinched or elevated at any point Do not allow the end of the hose to be submerged in waste liquid Doc 065342 06 12 11 121 Dionex ICS 5000 Operator s Manual 2 23 Injection Valves The TC is available in the following configurations TC Description Part Number TC with no injection valves 074108 TC with one 2 position 6 port high pressure injection valve 074109 TC with two 2 position 6 port high pressure injection valves 074112 TC with one 2 position 6 port high pressure injection valve 074113 and one 2 position 10 port high pressure injection valve The 6 port valve is installed on the left side of the module 2 23 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 64 shows flow schematics for the 6 port val
96. the instrument queue and a Ready Check is performed If the Ready Check passes and the instrument is not currently running another sequence the sequence is started Running Anions ics 5000 o Running Studio 4 Print Insert Row GH Fil Down SZ Filtering On Grouping On B Up Pump_1_Pressurh Name 2 Positio Volume Instrument Meth Processi i 5 Injection 3 Unknown 3 20 0 AnionMethod AS124 i 3 Injection 4 Unknown 4 20 0 AnionMethod ASIT2A if Injection 5 Unknown 5 20 0 AnionMethod AS12A 6 None HB Injection 6 Unknown 6 20 0 AnionMethod ASIT2A oe a MOS ns amma DEI E eo on A a A Y LUPO RR NE y E Ea ILLE Figure 5 6 Running Sequence in Chromeleon 7 Starting a Sequence in Chromeleon 6 8 1 On the Sequence Control panel click Load Sequence see Figure 5 7 2 to the Sequence table Click Start Batch see Figure 5 7 33 Panel Tabset1 Select the sequence from the list and click Open The sequence is added ICS 5000 22 Home Sequence Control Status Gradient Pumps Eluent Generator Detector Compartment AS DV Cond Detector System Log Audit Trail 2 33 45 AM Manually acquired samples will be stored temporarily in sequence SEQ AMARQUARDT2_localilCS 5000 manual 9 33 45 AM Chromeleon server version 6 80 SR8 Build 2598 Beta 154575 started serial number 39 2 34 07 AM User AMarquardt from AMARQUARDT2 has acquired cont
97. this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scientific Inc makes no representations that this document is complete accurate or error free and assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this document even if the information in the document is followed properly Revision history Revision 01 released May 2010 Revision 02 released June 2010 Revision 03 released February 2011 Revision 04 released June 2011 Revision 05 released September 2011 Revision 06 released December 2011 For research use only Not for use in diagnostic procedures Contents 1 Introduction 1 1 Thermo Scientific Dionex ICS 5000 System Overview 1 1 1 1 Dionex ICS 5000 System Components 2 1 1 2 Dionex ICS 5000 System Control 11 1 2 Dionex ICS 5000 System Documentation 14 1 3 The Dionex ICS 5000 System Operator s Manual 15 1 4 Safety and Regulatory Information 16 1 4 1 Safety Messages and Notes 00 16 1 4 2 Safety Symbols LL 18 1 4 3 Declaration of Conformity 00005 19 1 5 Deionized Water Requirements for IC 20 2 Description DP SP Desceriplioni colileallo gela aa 21 2 1 DP SP Front Features LL 21 2 2 D
98. uS cm stop the pump 13 Reconnectthe pump to the injection valve and reconnect the line from the suppressor to the cell inlet 9 27 2 Replacing an Analytical Suppressor IC Refer to the suppressor manual for guidance about when to replace a suppressor and for instructions on preparing a new suppressor before initial use Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 1 Stop the pump flow 2 Press the POWER button on the front of the DC for 2 seconds 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 hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the DC upper door 4 Disconnect the four liquid lines from the suppressor see Figure 9 50 Doc 065342 06 12 11 381 Dionex ICS 5000 Operator s Manual 5 Unplug the suppressor cable from the detector aciamtinie Pn C8 NERO SCIENTIFIC CSAS 300 2 mm P N 064557 er e ere Figure 9 50 Disconnecting the Suppressor Liquid Lines and Cable 6 Remove the suppressor from the detector by sliding it to the left a few millimeters to detach it from the mounti
99. up to 21 MPa 3000 psi with RFIC Before operating at pressures above these limits verify that you have the appropriate pump e HPC is stamped on the secondary pump heads of the older lower pressure rated capillary IC pumps e HPC 2 is stamped on the secondary pump heads of the newer higher pressure rated capillary IC pumps A Capillary Pump High Pressure Upgrade Kit P N 075994 is available for converting a lower pressure rated capillary IC pump to a higher pressure rated pump IMPORTANT If your system includes a capillary pump linked to an EGC check the label on the EG degas capillary cartridge in the IC Cube and verify that 5000 psi is printed on the label see the figure on the right If 5000 psi is not on the label you must change the high pressure limit to 21 MPa 3000 psi or replace the cartridge with an EG degas capillary cartridge that is rated for 35 MPa 5000 psi P N 074459 5000 psi Doc 065342 06 12 11 159 Dionex ICS 5000 Operator s Manual 160 Doc 065342 06 12 11 Es EG Startup 4 9 Entering the Eluent Concentration 1 Press the POWER button on the front of the EG 2 Onthe Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the EG tab to display the EG panel see Figure 4 8 ICS 5000 Home Pump EG AS DC CD EDI Audit Queue Q EG1 Control o e Lr Target Concentration 0 00 mM z Status Off Applied Concentration
100. using an autosampler are included in a Chromeleon 7 instrument method or Chromeleon 6 8 program When you create an instrument method or program with the Chromeleon software wizard the specific autosampler commands required for your model of autosampler and the type of injection to be performed are added automatically An Inject command to switch the injection valve to the Inject position is always included The Inject command occurs at time 0 00 This is when the sample enters the high pressure side of the system and defines the beginning of a chromatogram Wait commands to pause the instrument method or program while the autosampler is performing the injection are also included For Dionex AS DV and AS autosamplers a Load command is required to switch the injection valve to the Load position A separate Load command is not needed for the Dionex AS AP 180 Doc 065342 06 12 11 5 Operation Figure 5 9 shows the basic Chromeleon commands for controlling sample injection with a Dionex AS AP Autosampler Time Command Yalue 59 DP Pump_2 Curve 5 60 EDet1 CellControl off 61 EDet1 DC_Voltage OM Pi Wait Sampler CycleTimeState Hold Wait Sampler Ready Hold Timeoul Sampler Inject DP Pump_i Pump_i_Pressure AcqOn DP Pump_2 Pump_2_Pressure AcqOn HE S aa Figure 5 9 Commands for Loading and Injecting a Sample with a Dionex AS AP Chromeleon 7 Script Editor Shown Figure 5 10 shows the basi
101. waste line q 3 PUMF ANA Priming valve Secondary Pump Head ocak Priming Waste Line ma Figure 9 2 DP SP Priming Valve Doc 065342 06 12 11 309 Dionex ICS 5000 Operator s Manual 6 10 11 Press PUMP PRIME 1 or PUMP PRIME 2 on the front of the DP SP The pump will begin pumping at the priming flow rate selected on the Chromeleon panel Prime the pump until all air is purged and no air bubbles can be seen exiting the waste line Gradient pump only To prime additional eluent lines select another eluent channel and repeat the priming procedure After priming all eluent lines press PUMP PRIME 1 or PUMP PRIME 2 to stop priming and return to the flow rate last selected 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 destroy the cap seal Open or close the priming valve only when the system pressure is down Reconnect the pump to the software by clicking Connected on the Pump panel 9 5 2 Priming from the Chromeleon Panel 1 Open the priming valve on the secondary pump head see Figure 9 2 by turning it one half turn counterclockwise NOTE Ifthe priming valve is opened too much air is drawn through the valve and air bubbles can be seen exiting the waste line On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab Gradient pum
102. water 4 If you used the coarse polishing compound in Step 3 repeat the step with the fine compound 5 Using a moist piece of polishing cloth with no polishing compound added rub the polished surface free of residual polishing compound particles 6 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 pol ishing compound from the pads After initial use add only enough polishing compound to maintain the coat ing on the pad 7 Replace the working electrode block and yoke knob Fingertighten the knob by turning it a full 360 degrees NOTE Itis not possible to overtighten the yoke knob Once the knob clicks into place it does not tighten any fur ther The yoke knob ensures constant pressure is applied to the cell 8 Orient the cell assembly with the yoke knob on the left and push the cell onto its mounting location in the DC compartment 9 Reconnect the cell s inlet and outlet lines 10 Reconnect the electrical cables 11 Start the pump flow Doc 065342 06 12 11 391 Dionex ICS 5000 Operator s Manual 12 Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 13 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 9 28 5 Replacing a pH Ag A
103. zu vermeiden warten Sie bitte bis der DC abgek hlt ist ehe Sie die T r ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the DC lower door 4 Loosen the screw on the front of the leak sensor P N 062437 see Figure 9 33 Note The screw remains attached to the sensor eak Sensor Loosen this screw Figure 9 33 Leak Sensor 5 Pull out the leak sensor from the e n x component panel and continue Co pulling until the attached cable wp is also out of the opening Disconnec 6 The cable attached to the leak cables 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 34 i L l Figure 9 34 Leak Sensor Cable 7 Disconnect the two cables 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 065342 06 12 11 365 Dionex ICS 5000 Operator s Manual 9 22 Rebuilding a High Pressure Injection Valve Thermo Fisher Scientific recommends rebuilding the injection valve annually The Injection Valve Rebuild Kit P N 074698 4 port valve P N 057896 6 port valve P N 061759 10 port valve contains all required replacement parts This procedure also applies to high pressu
104. 0 00 a a Information Serial Number 123456789012 v Expiration Date Remaining lon Count N A Date Time fleteniion Device a 1 14 2010 10 24 48 AM EluentGenerator EGC_1 NIN an ANN PP aa AEN mandan MBA on hie nina ah AN ANA nn Mn Figure 4 8 Example EG Panel Chromeleon 7 Version Shown 3 Enter a value in the Target Concentration box For help in selecting an eluent concentration see Section 4 10 If the pump flow is on entering a new Target Concentration value automatically turns on the power to the EGC also 4 If the pump flow is off first turn on the flow and then click the switch under EG1 Control or EG2 Control This turns on the power to the EGC at the selected Target Concentration value 5 Ifthe CR TC switch is off click the switch to turn on the power to the CR TC Doc 065342 06 12 11 161 Dionex ICS 5000 Operator s Manual 4 10 Selecting an Eluent Concentration The allowable eluent concentration depends on several factors the flow rate suppressor type EGC type and cartridge configuration For details refer to Table 4 2 and Table 4 3 Single Cartridge or Independent Dual Cartridge Configuration In the single cartridge configuration the EG contains one EGC In the independent dual cartridge configuration the EG contains two EGCs operating independently on separate systems each cartridge is linked to a different DP SP For details refer to the EGC manual Cartridge manuals are included
105. 0 psi For details see page 5 Doc 065342 06 12 11 1 Introduction Analytical IC Analytical IC pumps operate at flow rates ranging from 0 00 to 10 0 mL min and operating pressures up to 35 MPa 5000 psi without RFIC and up to 21 MPa 3000 psi with RFIC Both microbore and standard bore IC applications are supported Dionex ICS 5000 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 e A high precision programmable current source power supply For each channel the following options must be ordered separately for installation inside the EG e A disposable eluent generator cartridge EGC Each cartridge contains an electrolyte concentrate solution appropriate for the eluent being generated 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 e A high pressure gas removal device that removes electrolysis gases created during eluent generation Two versions of EGC and CR TC are available one for capillary IC systems and one for analytical IC systems IMPORTANT If your system includes a capillary pump linked to an EGC check the label on the EG degas capillary cartridge in t
106. 06 12 11 131 Dionex ICS 5000 Operator s Manual To pump 2 inlet via the pump rear chase Pump front view To pump 1 inlet via the pump rear chase Deionized Deionized Water Water o DO Oc y To waste To EGC 1 In From the suppressor Regen Out via the DC rear chase From the IC Cube EG Degas Regen Out DC front view To the IC Cube EG Degas Eluent In EG EG left side view System 1 System 2 right side view From autosampler i To waste RFIC Eluent Degasser y Cell In Cell Out Y A jen Out Eluent Out 0 Regen Regen luent In Regen I Y Regon gut System 1 Regen In Separator DD es lt 4 A gt Eluent In luent S L Guard J emp W A tabilizer 6 Backpressure i Device GG ere e e AA 6 WA From autosampler ff mL p To the degasser Regen In via the EG rear chase x To waste To waste C ssa To waste us am Figure 3 3 Hybrid System Dual RFIC EG System CD Analytical CD Capillary 132 Doc 065342 06 12 11 3 Configurations To the pump inlet via the pump rear chase DL Eluent DC front view Pump front view Seal Wash Pump E Cell In Cell Out Eluent Out Regen Out 9 Piston A Seal O Wash D Ss 3 3 3 g f Mixer RI On Off Valve D From A i To waste To AS Waste I Figure
107. 1 V Vacuum degassing module 25 Daily maintenance 195 On off control 26 Vacuum is low 238 VALVE buttons DC 52 Enabling disabling 52 Troubleshooting 271 Valve LEDs DC LED is flashing 52 LED is lighted 52 Valve LEDs TC LED is flashing 115 299 LED is lighted 115 Valves See High pressure valves Injection valves Low pressure valves Variable Wavelength Detector 3 10 Regulator Bracket Kit 35 Vials 146 149 Filling 146 149 Virtual Column Separation Simulator 172 176 Voltammetry 105 See also Cyclic voltammetry VP Vacuum Pump 140 W Waste container EG Preventing gas buildup 142 Waste disposal 201 Waste lines CD Gas separator waste tube 72 Waste lines DC 82 Blocked 270 Waste lines DP SP 33 Waste lines EG 46 47 Blocked or incorrectly installed 253 254 Waste lines TC Blocked 300 Water dip 148 Water samples 147 Waveform Editor 108 Index 18 Doc 065342 06 12 11 Index Waveforms 105 Cyclic voltammetry 105 Defining 108 Integrated amperometry 107 Integrated amperometry example 104 Maximum length 107 Pre programmed 108 Pulsed amperometry example 103 Weekly maintenance DC 199 DP SP 195 EG 197 TC 201 Wellness 128 Wireframe plot 112 Working electrodes 75 Maintenance 143 Materials 75 Polishing 389 Z Zero position analog out 86 Doc 065342 06 12 11 Index 19 Dionex ICS 5000 Operator s Manual Index
108. 193 Dionex ICS 5000 Operator s Manual 194 Doc 065342 06 12 11 rae DP SP Routine Maintenance This section describes routine maintenance procedures that users may perform for the Dionex ICS 5000 Dual Pump DP or Dionex ICS 5000 Single Pump SP All other maintenance procedures must be performed by Thermo Fisher Scientific personnel 7 2 DP SP Daily Maintenance PVE IC 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 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 Check the liquid level in the seal wash reservoir The liquid level should remain between the Min and Max markers on the reservoir label Check eluent reservoirs for microbial growth clean reservoirs and replace eluent as needed Rinse each eluent reservoir thoroughly inside and out with ASTM filtered Type I 18 megohm cm deionized water that meets the specifications listed in Section 1 5 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 4 Check the liquid level in each eluent reservoir and refill as required 7 3 DP SP Weekly
109. 2 11 167 Dionex ICS 5000 Operator s Manual 168 Doc 065342 06 12 11 C TC Startup 4 13 Starting the TC 1 Press the POWER button on the front of the TC 2 On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the TC tab to display the TC panel see Figure 4 10 4 ICS 5000Home TE Audi Queue Temperature Control m a NotReady Oven gt ee Door Closed Nominal Temperature 20 0 C 3 Temp NotReady Actual Temperature i O Retention Time e a D a 9 i a pr T a Device Message S Date Time i 1 14 2010 5 15 32 PM User NA AMarquardt AMar m 1 14 2010 5 11 59 PM TC Column_B Chip card detected i 1 14 2010 5 11 59 PM TC Column_A Chip card detected 1 14 2010 5 11 59 PM TC TC 3000 Serial Demo F 1 14 2010 5 11 57 PM Chromeleon instrument cont 1 14 2010 5 11 57 PM Initializing driver Dionex AS Figure 4 10 TC Panel Chromeleon 7 Version Shown 3 Click the Oven switch Chromeleon 7 or the Oven on button Chromeleon 6 8 to turn on the oven 4 Set the temperature required for the application Doc 065342 06 12 11 169 Dionex ICS 5000 Operator s Manual 4 14 Equilibrating the System and Verifying Operational Readiness NOTE You can also use the Smart Startup feature in Chromeleon to automate system startup and equilibration Refer to the Chromeleon Help for details 1 On the Chromeleon 7 ePanel Set o
110. 2 11 363 Dionex ICS 5000 Operator s Manual 4 Attach the luer adapter fitting to the front of the port see Figure 9 32 1 Luer Adapter Fitting Sample Loading Port 3 1 4 28 Fitting and Ferrule Green 0 75 mm 0 030 in 4 ID PEEK Tubing Figure 9 32 Sample Loading Port Connection Cut a 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 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 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 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 9 21 Replacing the Leak Sensor 1 CAUTION MISE EN GARDE Turn off the pump flow from the ePanel in Chromeleon 7 or the Control panel in Chromeleon 6 8 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 To avoid injury wait for the DC to cool down before opening the door or performing any maintenance or service procedures Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance 364 Doc 065342 06 12 11 9 DC Service Um Verletzungen
111. 2 19 4 In the cyclic 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 are defined by three points each with a time and a potential The waveform forms a triangle with the first point always at time zero and the first and third points always having the same potential Doc 065342 06 12 11 105 Dionex ICS 5000 Operator s Manual Figure 2 52 shows an example of a triangular waveform used in cyclic voltammetry 0 60 14 0 0 60 Volts 30 00 Seconds Figure 2 52 Example Cyclic Voltammetry Waveforms 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 2x AV Sweep Rate CV Cycle Time 2x 14V _ 0 1 V 285 S 106 Doc 065342 06 12 11 2 DC Description Cyclic voltammetry waveforms are defined manually on the Chromeleon 6 8 electrochemical detector Control panel Click the CV Mode button to display the following window hemical Detector Ex EEN _ E T
112. 2 44 OFF POSITION kon f ON POSITION N C normally closed N O normally open COM common flow Note When the valve is off i e it is not energized port 0 is open N O and port 1 is closed N C Conversely when the valve is on port 1 is open and port 0 is closed Figure 2 44 Three Way Low Pressure Valve Flow Schematics 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 see Section 2 18 3 Doc 065342 06 12 11 97 Dionex ICS 5000 Operator s Manual 2 18 3 AM High and Low Pressure Valve Control IC Chromeleon is used to control the high and low pressure valves For automated control commands for valve control can be included in a Chromeleon 7 instrument method or a Chromeleon 6 8 program To add AM valve control commands to a Chromeleon 7 instrument method use the Script Editor see Figure 2 45 E 9 pd test Instrument Method Chromeleon Chromatography Studio Ox Home Instrument Method en Command Sampler DP Pump_2 Curve AS Sampler i Options Column TC CD CDet1 Ch Onti 000 State pions 4 Open ED EDet1 9 Closed Ji Options AM_LP2 DC DC ae DC_LP1 e DC_LP2 5 peo i e DELPI a DC_LP4 K System amp E DC_LP5 z amp E DC_LP6 7 Script Editor ae
113. 21 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 High Pressure High Pressure Valve 1 Valve 2 Figure 2 39 Dionex ICS 5000 Automation Manager NOTE Because the AM requires the full width of the DC upper com partment an IC Cube cannot be installed in the DC when an AM is installed e AM is available in the following configura tions Components Included 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 Figure 2 40 AM Configurations 94 Doc 065342 06 12 11 2 DC Description Components Included Part Number One 6 port high pressure valve 061740 One low pressure 3 way valve AutoPrep configuration 066343 10 port high pressure valve AutoPrep sample loop AutoPrep standard loops AM tray with no valves 061734 Figure 2 40 AM Configurations Continued 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 0
114. 21 323 324 Piston seal wash tubing replacement 326 Priming 310 311 Priming valve knob seal replacement 329 Service procedures EG CR TC replacement 349 354 Eluent generator cartridge replacement 336 349 Fuse replacement 357 Service procedures TC Column ID system setup 408 409 Fuse replacement 413 Injection valve pod replacement 411 Injection valve rebuilding 410 Tubing and fittings replacement 407 Shift in reference potential 274 Ship Kit DC 81 Ship Kit DP SP 33 Ship Kit EG 46 Ship Kit TC 121 Shutdown DC 187 DP SP 183 EG 185 TC 189 Silver electrodes 75 Single Pump SP 2 3 Analog pressure output 32 Digital I O port 31 Fuse replacement procedure 330 Fuses 31 Maintenance annual 196 Maintenance daily 195 Maintenance periodic 196 Maintenance weekly 195 Operating humidity 417 Operating temperature 417 Piston replacement procedure 323 Doc 065342 06 12 11 Index 15 Dionex ICS 5000 Operator s Manual Piston seal replacement procedure 316 321 323 324 Piston seal wash tubing replacement procedure 326 Pressure limit tripped 223 255 256 Pressure limits for EG 158 Priming procedures 308 311 Priming valve knob seal replacement procedure 329 Product warranty 303 Pulse damper for capillary pump 27 Selecting pressure limits 158 Shutdown procedure 183 Spare parts 435 Specifications 415 Start up procedures 153 Static mixe
115. 24 See also High pressure valves Injection valves A AAES 71 AC sockets DC 81 ACES 300 57 ACES 300 Capillary 71 Acetonitrile 76 Index Ag AgCl half cell 77 Air bubbles conductivity cell 383 Air particulate samples 147 Air pressure requirements 146 154 Alarm conditions See Error messages Alarm LED DC 51 Alarm LED DP SP 22 Alarm LED EG 256 LED is lighted 253 Troubleshooting 253 Alarm LED TC 115 Amperometry cell Cell design 76 Cell gasket replacement 386 Description 75 Electrodes 75 Maintenance 143 Monitoring the pH readout 78 Operating precautions 143 pH cannot be set to 7 0 272 pH limits 145 Polishing the working electrode 389 Reordering 442 Solvent compatibility 76 Storage 187 Troubleshooting 271 Amperometry detection See Cyclic voltammetry See DC amperometry See Integrated amperometry See Pulsed amperometry Analog output 85 Connection instructions 84 Connectors 82 83 Description 85 Full scale 86 Mark 86 Doc 065342 06 12 11 Index 1 Dionex ICS 5000 Operator s Manual Offset level 86 Polarity 86 Range 85 Recorder calibration 86 Selecting settings 85 Analog pressure output 32 Analog to digital converter 85 Analytical IC applications Conductivity detector for 69 CR TC trap column for 42 Eluent generator cartridges for 41 Suppressors for 71 System configurations 129 Annual maintenance DC 193 200 202 444 445 DP 192
116. 25 0 50 0 75 1 Create Application 2 Prepare System 3 Execute Application System Maintenance Create Program Application Wizard Hold Continue Daily Audit Trail Run Time Elapsed Create Sequence Acq On Acq Off Start Batch Consumable Change Edit Program Load Sequence Abort Batch Eluent Change rSequence Noj Po Inj Vol Program Status Inj Date Time Sequence Figure 5 4 Sequence Control Panel in Chromeleon 6 8 2 Complete the steps in the Sequence Wizard specifying the number of samples and standards that you want and the program and quantitation method to use For help at any time click the Help button on the Sequence Wizard page NOTE If preferred you can create the sequence first and then specify the program and quantitation method later You can also edit other details of the sequence for example add or remove samples after you finish the wizard 3 After you finish the Sequence Wizard the new sequence is displayed in the Chromeleon 6 8 Browser Doc 065342 06 12 11 175 Dionex ICS 5000 Operator s Manual Using the Application Wizard Chromeleon 6 8 only 1 Click Application Wizard on the Sequence Control panel see Figure 5 4 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 6 8 He
117. 271 Troubleshooting DP SP Chromatographic reproducibility 218 Digital I O port not operating 239 Leak alarm 237 Liquid leaks 237 Pump does not start 235 Pump stops unexpectedly 236 Vacuum degassing module low vacuum 238 Troubleshooting EG Alarm LED is lighted 253 EG stops operation 256 Error messages 241 Leaking fittings 253 Liquid leaks 254 No flow 255 Power LED does not light 254 Troubleshooting system wide 203 High background 225 Low detector output 224 Noisy baseline 215 Retention times too early 220 Retention times too late 220 Tailing peaks 222 Troubleshooting TC Alarm conditions TC 275 Alarm LED is lighted 299 Liquid leaks 300 Temperature does not increase 301 Temperature stabilizer not operating 301 Doc 065342 06 12 11 Index 17 Dionex ICS 5000 Operator s Manual TTL and relay connectors DC 82 83 Installation instructions 84 TTL inputs DC 82 Control types 92 Functions available 89 TTL outputs DC 82 Controlling 87 TTL Relay control DC Control panel 87 DC relay output configuration 87 Operating failure 239 Tubing Replacing DC 359 Replacing DP SP 306 Replacing EG 333 Replacing TC 407 U Upper compartment DC Description 61 Upper oven LED 51 USB cables DC 81 DP SP 33 EG 46 Reordering DC 444 Reordering DP SP 437 Reordering EG 440 Reordering TC 445 TC 121 USB connections DC 81 DP SP 33 EG 257 TC 12
118. 342 06 12 11 2 DC Description Tex 2 18 4 RCH 1 Reaction Coil Heater IC 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 For automated control of the heater commands can be included in a Chromeleon 7 instrument method see Figure 2 48 or Chromeleon 6 8 program Instrument Method Wizard Options DC DC Temperature Options Temperature Options for Options DC DC Column Use On Temperature 30 00 amp 10 00 70 00 C C Wait Ready O Dif Compartment Use On Temperature 30 00 15 00 35 00 C O Wait Ready O of Reaction Coil Heater Use On 1 Temperature 35 00 20 00 80 00 C O Wait Ready Off TT sides setta stabia si gman dedite mant Ae Mia Ae a Aim Bat msde mth neared py adio ob pen Mets oti Figure 2 48 Instrument Wizard DC Options Page in Chromeleon 7 For direct control of the heater use the controls on the DC ePanel in Chromeleon 7 or the Control panel in Chromeleon 6 8 Doc 065342 06 12 11 101 Dionex ICS 5000 Operator s Manual 2 19 Electrochemical Detection Modes The Dionex ICS 5000 Electrochemical Detector can perform the following electrochemical detection modes e DC amperometry see Section 2 19 1 e Integrated amperometry includes pulsed amperometric detection PAD and
119. 4 illustrates the liquid flow path through an EG configured for an analytical IC system Doc 065342 06 12 11 47 Dionex ICS 5000 Operator s Manual EG Degas Cartridge inside DC To Inject Ga Valve 4 Vent EGC Capillary TO PUMP DAMPER WASTE GAS SEPARATOR Figure 2 13 EG Flow Schematic Example for Capillary IC 48 Doc 065342 06 12 11 2 EG Description EGC VENT age RFIC Eluent y Degasser Regen Regen To Waste Inlet Outlet EGC IN EGC TO PUMP TO INJ VALVE P Coupler Coupler TO SRS AES REGEN OUT WASTE GAS SEPARATOR CR TC Figure 2 14 EG Flow Schematic Example for Analytical IC NOTE Refer to the EGC CO Mixer manual for a flow schematic showing the components required to generate a carbon ate bicarbonate mixture The manual is included on the Thermo Scientific Reference Library DVD P N 053891 Doc 065342 06 12 11 49 Dionex ICS 5000 Operator s Manual 50 Doc 065342 06 12 11 ICS 5000 sam DC Description 2 10 DC Front Features The status bar on the front of the Dionex ICS 5000 Detector Chromatography Module DC see Figure 2 15 includes buttons for controlling certain DC functions as well as LEDs that indicate the status of several DC components and functions e 9 CONNECTED AL
120. 4 x 8 25 x 19 in Weight SP 20 4 kg 45 Ib DP 24 1 kg 55 Ib Flow Path All polymeric PEEK anion or cation configurations Environmental Operating Temperature 4 40 C 40 104 F Operating Humidity 5 95 relative humidity noncondensing Doc 065342 06 12 11 417 Dionex ICS 5000 Operator s Manual 418 Doc 065342 06 12 11 a EG Specifications ICS 5000 EG Eluent Generator Specifications Minimum and Maximum Eluent Concentrations 0 1 100 mM Analytical 0 1 200 mM Capillary Flow Rates 0 100 3 000 mL min Analytical 0 001 0 030 mL min Capillary Eluent Types Analytical KOH LiOH NaOH Carbonate Carbonate Bicarbonate Carbonate with pH modifier MSA Eluent Types KOH Capillary MSA Maximum Operating Pressure 21 MPa 3000 psi Analytical 35 MPa 5000 psi Capillary Maximum Solvent Concentration Analytical and Capillary Cations None Anions 25 methanol Gradient Profiles Standard any combination of an unlimited number of linear convex and concave positive and negative gradient profiles Number of Cartridges Supported Two dual cartridge support RFIC Eluent Degasser Analytical Only Eluent degasser housed in the EG module System Software Software Chromeleon Chromatography Data System supports Microsoft Windows XP and Vista Automated Procedure Wizards Yes standard
121. 5000 system Introduction includes a brief description of the Dionex ICS 5000 modules the software required for Dionex ICS 5000 operation and the Dionex ICS 5000 user manuals Chapter 2 Detailed descriptions of Dionex ICS 5000 system Description components and important operating features includes an introduction to Chromeleon software Chapter 3 Detailed illustrations of component plumbing for System several Dionex ICS 5000 system configurations Configurations Chapter 4 Tasks to be performed before beginning operation of Getting Started the Dionex ICS 5000 system Chapter 5 Instructions for routine operation of the Dionex ICS Operation 5000 system Chapter 6 Short term and long term shutdown procedures for Shutdown the Dionex ICS 5000 system Chapter 7 Routine preventive maintenance procedures for the Maintenance Dionex ICS 5000 system Doc 065342 06 12 11 15 Dionex ICS 5000 Operator s Manual 1 4 1 4 1 DANGER Chapter 8 List of Chromeleon Audit Trail error messages and a Troubleshooting list of minor problems that may occur during operation of the Dionex ICS 5000 system The possible cause of each message or problem and the corrective action to take is included Chapter 9 Instructions for routine service and parts Service replacement procedures the user can perform for the Dionex ICS 5000 system Appendix A Specifications and installation site requirements for Speci
122. 6 Flow schematics 6 port valve 67 Leaking 270 Operation 65 68 Rebuilding 366 Reordering 441 Replacing mechanical parts Pod 367 Types available 62 Injection valves TC 122 Flow schematics 10 port valve 123 Flow schematics 6 port valve 122 Leaking 300 Operation 122 123 Plumbing 6 port valve 124 Rebuilding 366 410 Replacing mechanical parts pod 411 Types available 117 Inline filter 36 Instrument method Chromeleon 172 Integrated amperometry 103 3D data 109 Data storage 109 Integration interval 104 107 Waveform characteristics 107 Waveform example 104 Interior components DC 53 Analytical IC components 61 Conductivity Detector CD 54 61 Electrochemical Detector ED 54 61 IC Cube 55 Lower compartment description 62 Suppressor types 62 Upper compartment description for analytical IC 61 Upper compartment description for capillary IC 54 Inverted edge TTL input control DC 93 Inverted pulse TTL input control DC 93 IonPac ATC HC Trap Column 42 IonPac CTC 1 Trap Column 42 IPAD See Integrated amperometry I t plot 111 L Leak sensor EG 43 252 Leak sensors DC Lower leak sensor wet alarm 267 Replacement 364 Upper leak sensor wet alarm 269 Leak sensors TC Gas 126 285 Humidity 126 285 Leaks Conductivity cell 270 DC 270 EG 43 252 Gas 115 126 285 299 Humidity 115 126 285 299 Injection valve DC 270 Injection valve TC 300 Re
123. 61745 RCH 1 Reaction Coil Heater 061746 Temperature stabilizer standard bore 0 25 mm 062561 0 010 in ID Temperature stabilizer microbore 0 125 mm 062562 0 005 in ID Figure 2 41 AM Components Available Separately Doc 065342 06 12 11 95 Dionex ICS 5000 Operator s Manual Analytical 2131 AM High Pressure Switching Valves IC Up to two high pressure switching valves can be installed 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 42 and Figure 2 43 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 42 High Pressure Switching Valve Flow Schematics 6 Port Valve POSITION A POSITION B Figure 2 43 High Pressure Switching Valve Flow Schematics 10 Port Valve 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 see Section 2 18 3 96 Doc 065342 06 12 11 Analytical IC 2 DC Description 2 18 2 AMLow 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
124. 71679 Yes Yes Chromeleon 7 online Help N A N A N A Chromeleon 6 8 Software User s Guide 4829 5060 Yes No Installing the Chromeleon 6 8 031883 Yes No Chromatography Management System with a Dionex lon Chromatograph IC Chromeleon 6 8 online Help N A N A N A All Adobe PDF files listed above are shipped on the Thermo Scientific Reference Library DVD P N 053891 which is included in the ship kit of each Dionex ICS 5000 system module In addition the software manuals are provided as PDF files on the Chromeleon DVD A printed copy of the software installation instructions is provided in the software ship kit 14 Doc 065342 06 12 11 1 Introduction Consumables documentation For complete information about columns suppressors eluent generator cartridges etc refer to the appropriate product manual These manuals are provided on the Reference Library DVD 1 3 The Dionex ICS 5000 System Operator s Manual The electronic version i e PDF file of the Dionex ICS 5000 system operator s manual contains numerous links that you can click to go to other locations within the manual 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 An overview of the Dionex ICS
125. 75 Suppressor eluent out 10 32 ferrule double Tan 043276 CRD eluent in cone e CD cell inlet and outlet e ED cell outlet e Injection valve sample in and sample out Table 9 6 Tubing and Fittings for a Capillary IC DC System Doc 065342 06 12 11 359 Dionex ICS 5000 Operator s Manual rus Table 9 7 lists the tubing and fittings in the IC Cube Tubing Kit P N 072186 Part Length Part Used To Connect Quantity Number Precision cut 0 062 mm 65 mm 072188 50 mm guard column 0 0025 in ID PEEK 2 56 in outlet to 250 mm tubing blue separator column inlet Precision cut 0 062 mm 115 mm 072189 Guard column inlet to 0 0025 in ID PEEK 4 53 in injection valve tubing blue labeled VALVE PORT 3 Precision cut 0 062 mm 75 mm 074603 35 mm guard column 0 0025 in ID PEEK 2 93 in outlet to 150 mm tubing blue separator column inlet Precision cut 0 062 mm 210 mm 072187 Separator column inlet to 0 0025 in ID PEEK 8 27 in injection valve if a guard tubing blue labeled column is not present VALVE PORT 3 0 25 mm 0 010 in ID 610 mm 042690 EG degas cartridge PEEK tubing black 24 in REGEN OUT to waste if an EG is not present 0 125 mm 0 005 in ID 610 mm 044221 Inject valve waste to AS PEEK tubing red 24 in waste High pressure 10 32 7 074449 e EG degas cartridge fitting bolt blue ELUENT OUT to injection valve e Injection valve to guard or separator c
126. 75 and ferrule P N 043276 refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 Doc 065342 06 12 11 361 Dionex ICS 5000 Operator s Manual 9 19 2 Tubing and Fittings for Analytical IC Systems IC Table 9 8 lists the tubing and fittings used to plumb a DC system for analytical IC Tubing Size and Type Color P N Used to connect 0 75 mm 0 030 in ID Green 044777 Injection valve to waste PEEK 1 in AS needle seal White 057301 AS normal and assembly 46 cm 18 in 1 in concentrate modes only with 10 32 ferrule fitting Injection valve to the AS inject port 0 33 mm 0 013 in ID Light Blue 049714 AS sequential modes only PEEK 1 in Injection valve to AS diverter valve 0 51 mm 0 020 in ID Orange 042855 AS simultaneous mode PEEK 1 in only Each injection valve to the AS simultaneous injection tee 1 58 mm 0 062 in ID Colorless 014157 Suppressor REGEN OUT PTFE 1 in 0 125 mm 0 005 in ID Red 044221 Microbore systems PEEK 1 in Connections between other system components 0 25 mm 0 010 in ID Black 042690 Standard bore systems PEEK 1 in Connections between other system components 1 8 in fitting bolt Tan 052267 Suppressor REGEN OUT 1 8 in ferrule Yellow 048949 fitting 10 32 Fitting bolt Black 043275 All other tubing fittings 10 32 Ferrule double Ta
127. 8 Camshaft sensor missing or dark Abort page 228 Degasser malfunction Warning page 228 Excessive drive current Camshaft x x Abort page 229 Invalid flow value Abort page 229 Leak detected Flow stopped Abort page 229 Left hand pump block carryover pressure is too Abort page 230 high Motor malfunction Abort page 230 Motor position error The motor is overloaded Abort page 230 Pressure fallen below lower limit Abort page 231 Relay 4 is configured for inject synchronization Abort page 232 Please change pump configuration Right hand pump block carryover pressure is Abort page 230 too high The maximum purge pressure was exceeded Abort page 232 The pressure in the left hand working cylinder Abort page 233 exceeded the safety limit The pressure in the right hand working cylinder Abort page 233 exceeded the safety limit Table 8 1 DP SP Error Messages 204 Doc 065342 06 12 11 8 Troubleshooting DP SP Related Audit Trail Error Message Default Severity Level The system pressure exceeded the safety limit Abort page 233 This function cannot be adjusted by the user Abort page 234 Upper pressure limit exceeded Abort page 234 Table 8 1 DP SP Error Messages Continued 8 1 2 EG Error Messages Table 8 2 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 Tra
128. 9 rd e Check the liquid level in each eluent reservoir and refill as required 7 4 DP SP Periodic Maintenance e Make fresh eluent as needed e Replace piston seals every 6 to 12 months see Section 9 7 Be e Clean eluent reservoirs every 3 months with methanol or isopropyl alcohol as instructed in Section 9 4 7 5 DP SP Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The following kits are available e ICS 5000 Analytical Pump Preventive Maintenance Kit P N 075038 ICS 5000 Capillary Pump Preventive Maintenance Kit P N 075039 196 Doc 065342 06 12 11 feel EG Routine Maintenance This section describes routine maintenance procedures for the Dionex ICS 5000 Eluent Generator EG that users may perform All other maintenance procedures must be performed by Thermo Fisher Scientific personnel For information about maintenance procedures for the EGC CR TC trap column or suppressor refer to the appropriate product manual These manuals are included on the Thermo Scientific Reference Library DVD P N 053891 7 6 EG Daily Maintenance e Locate and repair leaks inside the EG see Section 9 13 and wipe up liquid Rinse dried eluents off components with deionized water e 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 ac
129. 9 23 leave the other end of the coil unconnected This is a temporary connection oT Figure 9 23 Analytical EGC Outlet Connection for Conditioning Procedure 8 While holding the EGC 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 346 Doc 065342 06 12 11 9 EG Service 9 Slide the EGC with the electrolyte reservoir on top into the holder in the EG see Figure 9 24 Figure 9 24 Analytical EGC Installed on Holder 10 Push the EGC electrical cable firmly into the EGC 1 or EGC 2 bulkhead connector see Figure 9 14 Twist the ring on the cable connector fingertight to secure it 11 Remove the 10 32 plug from the EGC 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 16 13 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 To ensure proper ventilation always connect the vent line to the IMPORTANT analytical EGC before operation Doc 065342 06 12 11 347 Dionex ICS 5000 Operator s Manual Conditioning the Analytical EGC IC EGC VENT
130. ARM 2 UPPER LOWER SUPPRESSOR OVEN VALVE 1 LOAD INJECT LOAD INJECT CORONE VALVE 2 Figure 2 15 DC Status Bar Button LED If the LED Is On If the LED Is Flashing Label CONNECTED The DC is connected to a Does not flash Chromeleon 7 instrument or Chromeleon 6 8 timebase ALARM The leak sensor is wet or there Does not flash was a valve or suppressor error Check the Chromeleon Audit Trail for the cause SUPPRESSOR 1 The suppressor is on and Does not flash set temperature SUPPRESSOR 2 current is being applied OVEN UPPER The upper compartment is at The upper compartment its set temperature is transitioning to the set temperature The compartment is not ready for operation OVEN LOWER The lower compartment is at its The lower compartment is transitioning to the set temperature The compartment is not ready for operation Doc 065342 06 12 11 51 Dionex ICS 5000 Operator s Manual Button LED If the LED Is On If the LED Is Flashing Label VALVE 1 LOAD Use the VALVE 1 and VALVE 2 Valve error See VALVE 2 LOAD buttons to manually switch the Section 8 25 for VALVE 1 INJECT position of the DC injection troubleshooting VALVE 2INJECT valves The LEDs indicate whether the valve is in the Load or Inject position Use this POWER button for Does not flash POWER routine on off control of the DC When the power is on this LED is lighted To turn
131. C Systems Ber Flushing the Capillary EGC 1 Remove the new EGC from the shipping container NOTE Save the shipping container it may be required for storage or disposal of the EGC 340 Doc 065342 06 12 11 9 EG Service 2 Verify that the vent fitting on top of the EGC is tightened Turn the cartridge upside down and place it on the EG drip tray 4 Remove the plugs from the INLET and OUTLET fittings on the eluent generation chamber 5 Locate the 38 cm 15 in piece of 0 025 mm 0 001 in ID tan PEEK tubing P N 074582 in the EG Ship Kit P N 072047 6 Connect this line to the EGC INLET port and connect the other end to the EGC IN line from the pump pulse damper see Figure 9 19 This is a temporary connection to provide backpressure during the EGC setup procedure 7 Connect a piece of 0 25 mm 0 010 in ID black PEEK tubing to the EGC OUTLET port Direct the other end of the tubing to waste This is a temporary connection Capillary EGC Flushing Pump at 0 02 mL min for 20 min EGC Capillary Electrolyte Reservoir f EGC Electrolyte Generation IN 38 cm 15 in of 0 025 mm Chamber 0 001 in ID tan PEEK tubing Temporary connection for backpressure EGC 0 25 mm 0 010 in ip OUT Pump Outlet PERSI Tubing Assembly connection P N 068658 To Waste TO PUMP DAMPER Figure 9 19 Flow Schematic for Flushing the Capillary EGC Doc 065342 06 12 11 341
132. CS 5000 Operator s Manual 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 78 Use a small screwdriver to remove the fuse cartridge Fuse Cartridge Figure 9 78 TC Fuse Cartridge 4 Replace the two fuses with new 2 A IEC 60127 2 time lag fuses P N 954776 Thermo Fisher Scientific recommends always replacing both fuses 5 Reinstall the fuse cartridge 6 Reconnect the main power cord and turn on the power 414 Doc 065342 06 12 11 A Specifications 8 DP SP Specifications ICS 5000 SP Single Pump and DP Dual Pump Specifications Type Dual piston in series microprocessor controlled constant stroke variable speed patented Isokinetic Eluent Precompression Construction Chemically inert metal free PEEK pump heads and flow path compatible with aqueous eluents from pH 0 14 and reversed phase solvents Pressure Range 0 35 MPa 0 5000 psi Analytical 0 41 MPa 0 6000 psi Capillary Flow Rate Range e 0 000 10 000 mL min with settable flow increments at 0 001 mL min Analytical e 0 001 3 000 mL min with settable flow increments at 0 0001 mL min Capillary Flow Rate Precision lt 0 1 Analytical Flow Rate Ac
133. Description 119 Digital I O connectors 120 Fuses 119 Power switch 119 USB connections 121 Waste line 121 Rear seal wash See Piston seal wash system Recorder Analog output setting 86 Calibrating 86 Recycle mode 73 Redox reactions 77 Reference electrode 75 Contaminated 272 Faulty 274 Leaking 274 Preventing from drying out 78 Reordering information 442 Shutdown procedure 187 Reference potential shift 78 274 Regulator Bracket Kit TC VWD PDA 35 Regulator Kit EO 35 Relay connectors DC 82 84 Configuring 87 Relay outputs DC 82 Controlling 89 Reordering information DC 441 DP SP 435 EG 439 TC 445 Reprocessing amperometry data 109 Reproducibility Affected by amperometry cell pH 78 Affected by temperature changes 70 Reproducibility is poor 218 Reservoirs eluent 34 Cleaning 214 219 308 Installation in EO 6 34 35 Pressurizing 34 Retention time Troubleshooting 220 Variations 118 Reversed phase solvents 76 RFIC Eluent Degasser 43 47 Leaks 253 254 Pressure requirements 141 Replacement procedure 355 Tubing rupture 141 223 255 RFIC ER 6 RFIC ESP 6 Running samples 172 See also Sample processing S Safety icons 35 Safety messages 16 35 Salt crystals preventing 197 Sample analysis overview 172 Sample loading With a syringe 179 With an autosampler 178 Sample loop DC Injecting 66 67 69 Loading 68 178 179 Reordering 441 Sample loop
134. Dionex ICS 5000 lon Chromatography System Operator s Manual Document No 065342 Revision 06 December 2011 2011 Thermo Fisher Scientific All rights reserved AES Atlas Chromeleon IonPac OnGuard and SRS are registered trademarks of Thermo Fisher Scientific Inc in the United States Adobe Acrobat and Adobe Reader are registered trademarks of Adobe Systems Incorporated in the United States and other countries Windows is a registered trademark of Microsoft Corporation in the United states and other countries The following are registered trademarks in the United States and possibly other countries Kel F is a registered trademark of 3M Company Inc KIMWIPES is a registered trademark of Kimberly Clark Corporation PharMed and Tygon are registered trademarks of Saint Gobain Performance Plastics Ultrajet is a registered trademark of ITW Chemtronics PEEK is a trademark of Victrex PLC TitanHP is a trademark of Rheodyne L L C All other trademarks are the property of Thermo Fisher Scientific and its subsidiaries Thermo Fisher Scientific Inc provides this document to its customers with a product purchase to use in the product operation This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific Inc The contents of this document are subject to change without notice All technical information in
135. Figure 9 12 Carefully slide the seal onto the knob avoid scratching or nicking the sides 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 Seal P N 063382 Insert seal with groove facing away from knob Figure 9 12 Replacing the Priming Valve Seal 9 Insert the priming valve knob into the secondary pump head turn the knob clockwise and tighten fingertight 10 Push the component mounting panel back into the enclosure Close the DP SP door 11 Press the POWER button on the front of the DP SP to turn on the pump 12 Reconnect the pump to the software by clicking Connected on the Pump panel 13 Turn on the pump flow 9 11 Changing the DP SP Main Power Fuses 1 Turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following e Disconnect the pump from the software by clicking Connected on the Pump panel 330 Doc 065342 06 12 11 9 DP SP Service DANGER DANGER ACHTUNG 5 10 11 12 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 7 Disconnect the m
136. ICS 5000 Operator s Manual 2 Check the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the pump and EGC are linked EG mode will be turned off for invalid flow Flow range for analytical EGC 0 100 3 000 mL min capillary EGC 0 001 0 100 mL min This error occurs when the flow to the EGC is out of range or there is no pumped linked to the EGC To troubleshoot 1 Set the flow rate to a value within the allowed range Refer to Appendix A for flow rate specifications 2 Check the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the pump and EGC are linked EGC 1 is not linked to a compatible pump Or EGC 2 is not linked to a compatible pump This error occurs if the type of pump linked to the EGC does not match the EGC type A capillary EGC can only be used with a capillary pump and an analytical EGC can only be used with an analytical pump To troubleshoot 1 Install the correct type of EGC for the pump type 2 Fora hybrid system a dual system with both an analytical and a capillary pump check the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the correct pump is linked to the EGC 250 Doc 065342 06 12 11
137. Installing and Conditioning a New Analytical EGC NEMI Figure 9 22 shows the EG flow schematic for an analytical IC system Refer ie to this figure when performing EGC and CR TC service procedures in an analytical IC system EGC VENT Pi EGC To Waste Eluent Inlet Outlet EGC IN E To PUMP 50 Coupler TO INJ VALVE P Coupler TO SRS AES REGEN OUT WASTE GAS SEPARATOR m sy ol CR TC Figure 9 22 EG Flow Schematic Example for Analytical IC Systems Installing the Analytical EGC 1 Remove the new EGC from the shipping container NOTE Save the shipping container it may be required for storage or disposal of the EGC Doc 065342 06 12 11 345 Dionex ICS 5000 Operator s Manual 2 Verify that a plug is installed in the vent port This will prevent leakage from the vent opening when you turn over the cartridge 3 Turn the cartridge upside down and place it on the EG drip tray in the service position see Figure 9 17 4 Remove the plugs from the INLET and OUTLET fittings on the eluent generation chamber 5 Connect the EGC IN line from the pump to the EGC INLET port 6 Locate the yellow 0 5 mL min 7 MPa 1000 psi backpressure coil P N 053765 in the EG Ship Kit P N 072047 7 Connect one end of the backpressure coil to the EGC OUTLET port see Figure
138. Kit P N 074422 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 When the TC VWD or PDA is installed as the topmost module in the system the TC VWD PDA Regulator Bracket Kit P N 074424 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 074423 For instructions on installing the regulator kits refer to Thermo Scientific Dionex ICS 5000 Ion Chromatography System Installation Instructions Document No 065343 The manual is included on the Thermo Scientific Reference Library DVD P N 053891 Doc 065342 06 12 11 35 Dionex ICS 5000 Operator s Manual 2 5 3 Filtering Eluent e Install an end line filter P N 045987 on the end of each reservoir s eluent line End line filters are provided in the pump ship kit e 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 36 Doc 065342 06 12 11 E EG Descriptio
139. Maintenance 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 EGC to generate carbonate bicarbonate eluent When the end line filters are new they are pure white Replace the filters whenever they become discolored if bacterial buildup is evident or if eluent flow is blocked Doc 065342 06 12 11 195 Dionex ICS 5000 Operator s Manual NOTE Itis especially important to regularly replace end line filters when using aqueous eluents Aqueous eluents may contaminate the filters with bacteria or algae causing cause flow restrictions to the pump End line filters are provided in the pump ship kit Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 063342 Before installation thoroughly rinse the end line filter with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 to remove any loose particles e Replace the seal wash solution ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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
140. Manual 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 5 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 A J 0 5 10 Retention Time Minutes Figure 2 56 Example Chromatogram for a Pulsed Amperometry Application For 3D 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 are collected Displaying and Reprocessing 3D Data This section describes how to display and reprocess 3D amperometry data using Chromeleon 6 8 If you are using Chromeleon 7 the features described here are available by displaying the data in a contour plot For details refer to the Chromeleon 7 Help In Chromeleon 6 8 you can display and reprocess 3D amperometry data in the 3D Amp
141. N IN port of the CR TC 3 Connect a piece of 0 25 mm 0 010 in ID PEEK tubing between the ports This is a temporary connection Capillary EGC Conditioning Pump at 0 02 mL min for 15 min EGC concentration at 50 mM 0 062 mm 0 0025 in ID PEEK Tubing Assembly P N 072204 TO PUMP DAMPER To Waste gt N 1 58 mm 0 062 in ID Tefzel Tubing Assembly P N 072225 0 25 mm 0 010 in ID PEEK Tubing Temporary connection Figure 9 21 Flow Schematic for Conditioning the Capillary EGC 4 Verify that the suppressor Mode is off Doc 065342 06 12 11 343 Dionex ICS 5000 Operator s Manual 5 10 11 12 13 Set the pump flow rate to 0 02 mL min To avoid damaging the suppressor always turn it off before conditioning the EGC The pump flow is on during conditioning however no flow reaches the suppressor Set the EGC concentration to 50 mM and turn on the EGC and CR TC power Condition the EGC for 15 minutes Turn off the EGC and CR TC power Turn off the pump flow Remove the backpressure tubing from the EGC IN line Use a high pressure blue fitting to connect the EGC IN line to the EGC INLET port Disconnect the temporary tubing from the ELUENT OUT and REGEN IN ports of the CR TC Reconnect the lines to the ELUENT OUT and REGEN IN ports of the CR TC that were disconnected in Step 2 344 Doc 065342 06 12 11 9 EG Service 9 14 5
142. P SP Interior Components LL 23 2 2 1 Pump Heads 0 cee eee ee 24 2 2 2 Pressure Transducer 0 0 eee eee eee eee 25 2 2 3 Proportioning Valves Gradient pump only 25 2 2 4 Vacuum Degassing Module 0005 25 2 2 5 Piston Seal Wash System 26 Doc 065342 06 12 11 i Dionex ICS 5000 Operator s Manual 2 2 6 Static Mixer Analytical IC only LL 27 2 2 7 Pulse Damper Capillary IC only 27 2 3 DP SP Flow Schematics i 28 2 3 1 Isocratic Pump Flow Schematic 28 2 3 2 Gradient Pump Flow Schematic 29 24 DP SP Rear Panels ii e A 30 2 5 Eluent Reservoirs urti on nits naa is weds wel 34 2 5 1 EO Optional 00 cee eee eee 34 2 5 2 Pressurizing Eluent Reservoirs LL 34 2 5 3 Filterin Bluent oro ire boa e Aaa laut 36 EG Description inor o Per Rs 37 2 60 EG Front Features iii amener fee ae PE i 37 2 7 EG Interior Components 38 2 8 EG Rear Panel corriere et 45 2 9 EGFlowSchematics Sres ruen ani cece eee eee eee 47 DC Description tints sees es Ai tee beds ia 51 2 10 DC Front Features ili dad tea eta ees 51 2 11 DC Interior Components 53 2 11 1 DC Interior Components for Capillary IC 54 2 11 2 IC Cube for Capillary IC 55 2 11 3 DC Interior Components for Analytical IC 61 2 12 DC Temperature Control Zones 00 0 eee eee eee 63 2 13 High Pressure Valves
143. Periodic Maintenance 0 e eee eee eee 196 7 5 DP SP Annual Maintenance 196 EG Routine Maintenance 004 197 7 6 EG Daily Maintenance LL 197 7 7 EG Weekly Maintenance 0 0 eee eee eee 197 7 8 EG Annual Maintenance 197 DC Routine Maintenance 00 199 7 9 DC Daily Maintenance 199 7 10 DC Weekly Maintenance LL 199 Doc 065342 06 12 11 vii Dionex ICS 5000 Operator s Manual 7 11 DC Periodic Maintenance 00 cece eee eee 199 7 12 DC Annual Maintenance 0 0 eee eee 200 TC Routine Maintenance 0 201 7 13 TC Daily Maintenance LL 201 7 14 TC Weekly Maintenance 0 eee eee eee eet 201 7 15 TC Periodic Maintenance LL 201 7 16 TC Annual Maintenance 202 8 Troubleshooting 8 1 Audit Trail Error Messages 0 0 cece eee eee eee 203 8 1 1 DP SP Error Messages 00 00 e eee ee eee 204 8 1 2 EG Error Messages 205 8 1 3 DC Error Messages scs ocras 00 eee eee ee eee 207 8 1 4 TC Error Messages 0 eee ee eee eee 209 82 Noisy Baseline va seedless oa eat 214 8 3 Poor Retention Time Reproducibility 0 218 8 4 Peak Retention Times Are Too Early 220 8 5 Peak Retention Times Are Too Late 220 8 07 No Peaks dics pose cigar scotia eee wis Vins ane Mage WES Ms 220 8 7 Tailing Peaks
144. Piston a a Seal Wash System 1 Y Deionized Water From IC Cube 2 EG Degas Regen Out EG System 1 From autosampler System 1 a System 2 Ne autosampler Tewm To waste From IC Cube 1 EG Degas Regen Out a Regen In Y To IC Cube 1 Eluent In EG Degas a Eluent In Regen Out Eluent Out To waste gt To IC Cube 2 EG Degas Eluent In EG System 2 right side view Regen Out gt Regen In gen In J gt Eluent In Eluent Out To waste 130 Figure 3 1 Capillary IC Dual RFIC EG System CD CD Doc 065342 06 12 11 3 Configurations Pump front view To pump 2 inlet via the pump rear chase To pump 1 inlet via the pump rear chase System 2 To waste pump not to scale To EGC g 2 In Piston Seal System 1 Pj Y Deionized Deionized Water Water Os To waste DC front view Fia Ibs Rube fz ie Reges Hog ee Fo IC Cube 2 EG Degas Eluent In EG left side view System 1 System 2 right side view From autosampler System 1 gt autosampler ToiWacte To waste EG Degas Regen Out Regen Out Regen Out Yy gt E Regen In egen ni Eluent isf To IC Cube 1 NEREO Eluent In luent Out EG Degas Eluent In lai Eluent Out _ __ _ TE 33 N TO waste To waste aw Eas Figure 3 2 Capillary IC Dual RFIC EG System CD ED Doc 065342
145. R button on the front of the DP SP to turn on the pump 6 Reconnect the pump to the software by clicking Connected on the Pump panel 7 Turn on the pump flow 9 9 Replacing the Piston Seal Wash Tubing Check the piston seal wash tubing weekly for crimping or blockage and replace as needed 1 Turn off the pump flow 2 Five red Phillips screws are installed on the component mounting panel before shipment from the factory Remove these screws if present 3 Open the DP SP door and then use the handles on the component mounting panel to pull the panel forward until it reaches the stop 4 Remove the old tubing from the peristaltic pump see Figure 9 9 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 326 Doc 065342 06 12 11 9 DP SP Service d Pull on the fitting slightly to remove the PharMed tubing from the upper notch on the pump mounting plate PharMed Tubing P N 063268 Rotor Lever Mounting Plate Tygon 2075 Tubing P N 064079 0000 0 Fitting Figure 9 9 Peristaltic Pump for Seal Wash System 5 Pull off the PharMed and Tygon 2075 tubing from the fitting Save the fitting 6 Pull off all seal wash tubing from the seal wash reservoir and the primary and secondary pump heads see Figure 9 10
146. Rise Time 0 50 Data Collection Rate 5 0 Autozero Calibration Cell Heater Cell Heater Mode On Cell Heater Set Point 35 00 C a v x 2004 Cell Heater Temp Cell Heater Status I aa Analog Out 1 Range 1 00 s Full Scale 1 00 800 Offset Level 0 n Unknown Polarity Negative v S 0 0 2 5 5 0 7 5 10 0 Figure 2 34 Conductivity Detector Control Panel Chromeleon 7 Version Shown 2 17 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 35 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 Doc 065342 06 12 11 87 Dionex ICS 5000 Operator s Manual 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 17 1 and the documentation for the external device for connection instructions RELAY OUTPUT CONFIGURATION Rear Panel Relay Output Pins on DC Electronics
147. See Eluent generator cartridges Electrochemical detection DC amperometry 102 Integrated amperometry 103 Pulsed amperometry 103 Electrochemical Detector ED 3 7 75 429 3D data 111 113 Amperometric cell description 75 Data storage 109 Description 61 75 Detection modes 75 102 Palladium hydrogen PdH reference electrode 79 pH Ag AgCl reference electrode 77 Reordering information 442 Replacement procedure 404 Doc 065342 06 12 11 Index 5 Dionex ICS 5000 Operator s Manual Shutdown procedure 187 Working electrodes 75 See also Amperometry cell Electrodes 76 Reference 75 Working 75 Electrolysis gases Purging from eluent 43 58 141 Venting from system 46 Eluemt generator cartridges 5 Eluent concentration 161 163 Eluent generation Electrolysis gases 43 58 Eluent Generator EG 2 5 Alarm LED is lighted 253 256 Analytical IC systems 40 Backpressure 43 Backpressure coil 215 Capillary IC system 39 Component description 38 41 43 Degas cartridge for IC Cube 58 Electrical connections consumables 44 Eluent concentration ranges 161 163 Eluent generator cartridges 5 Fuse cartridge 46 Fuses 46 Gas vent line 46 Leak sensor 43 252 Liquid flow path 47 49 Liquid leaks 253 254 Main power switch 46 Maintenance 197 Operating precautions 141 Power LED does not light 254 Pump pressure limits 256 Rear panel description 45 46 Selecting the eluent co
148. Severity Level Two AcqOn commands for the same channel Error page 296 The second chromatogram will overwrite the first Unknown error code Warning page 297 Unknown format of the card data Error page 297 USB LAN communication error Please check Abort page 283 communication cable and instrument s power Value for name parameter is not within valid Warning page 289 range Value passed x will be substituted by y Value x replaced by valid table entry y Warning page 289 X position error Abort page 298 You do not have the privilege to approve the Error page 298 module s qualification You do not have the privilege to change the Error page 298 performance limits You do not have the privilege to change the Error page 298 qualification intervals Table 8 4 TC Error Messages Continued 8 2 Noisy Baseline e Fluent is contaminated 1 Clean all eluent reservoirs thoroughly inside and out with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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 4 2 Flush the system with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 3 Replace all end line filters P N 045987 See Section 4 6 for instructions 4 Prepare new stock solut
149. Steckdose nahe am Ger t befindet und leicht zuganglich ist VORSICHT Digital I O Port The digital I O port provides a connection to auxiliary devices The connector includes three TTL inputs and four relay outputs Table 2 1 indicates the functions assigned to the connector pins 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 rr Not used 2 e 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 7 Relay 1 Out Potential free Common Table 2 1 25 Pin D Sub I O Port Female Doc 065342 06 12 11 31 Dionex ICS 5000 Operator s Manual Pin Number Signal Name Signal Level Description 8 Relay 2 Out Potential free Common 9 Gnd Ground Ground 10 Gnd Ground Ground 11 Gnd Ground Ground 12 Gnd Ground Ground 1300 e Not used 14 Relay 4 Out Potential free Normally open 15 Relay 4 Out Potential free Common 16 Relay 4 Out Potential free Normally closed 1700 e Not used 18 Relay 3 Out Potential free Common 19 Relay 1 Out Potential free Normally open 20 Relay 2 Out Potential free Normally open 21 Vcc Out 5V 5V 500 mA 22 TTL Input 1 TTL Hold Run 23 TTL Input 2 TTL Stop 24 TTL Input 3 TTL Sta
150. TC Injecting 123 Injection valve connections 124 Loading 122 123 Reordering 445 Sample processing 172 Index 14 Doc 065342 06 12 11 Index Sample tray Loading 146 149 See Tray Samples Collecting and storing 147 Diluting 148 Filtering 147 Loading 178 179 Pretreating 147 See also High pressure valves Injection valves Self Regenerating Suppressor SRS 47 62 Gas separator waste tube 72 Hydrating 185 186 Start up procedure 185 186 See also Suppressor Sensor gas 115 126 285 Sensor humidity 115 126 285 Sequence Wizard 173 176 Service procedures DC Amperometry cell gasket replacement 386 Capillary column replacement 374 CD cell air removal 383 CD cell calibration 379 Conductivity detector replacement 382 Electrochemical detector replacement 404 Fuse replacement 371 IC Cube cartridge replacement 372 Injection valve Pod replacement 367 Injection valve rebuilding 366 410 Leak sensor replacement 364 PdH reference electrode replacement 400 pH Ag AgcCI reference electrode O ring replacement 399 pH Ag AgCl reference electrode replacement 392 Replacing capillary columns 375 379 Suppressor replacement 38 1 Tubing and fittings replacement 359 Working electrode polishing 389 Service procedures DP SP Check valve cartridge replacement 312 Eluent reservoir cleaning 308 Fuse replacement 330 Piston replacement 323 Piston seal replacement 316 3
151. Tab Page 408 Doc 065342 06 12 11 9 TC Service 4 Select the check box for the column to be monitored A B C or D and click OK 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 73 Figure 9 73 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 74 When the chip card is installed correctly the LED next to the slot is green Figure 9 74 Inserting a Column ID Chip Card 3 Installa 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 065342 06 12 11 409 Dionex ICS 5000 Operator s Manual 9 31 Rebuilding an Injection Valve Thermo Fisher Scientific 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 requir
152. 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 3 Be careful not to overtighten fittings 2 Ifthe Upper pressure limit exceeded message is also displayed refer to page 234 for additional troubleshooting steps 230 Doc 065342 06 12 11 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 To troubleshoot 1 6 The eluent supply may be depleted Check the Eluent Level Display on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset 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 5 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 6 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 5 Eluents may be insufficiently degassed Check the vacuum degassing module Check all tubing connections for leaks tighten loose fitting connections Be careful not to overtighten fittings Make sure the priming valve is closed see Figure 2 3
153. Troubleshooting 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 e Find and eliminate any liquid leaks or blockages in tubing connections see Section 8 31 Adjust the flow rate accordingly 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_ LowerLimit commands To troubleshoot Select a valid temperature setting Data buffer overrun This error occurs in Chromeleon 6 8 if the system cannot write incoming data to disk fast enough To troubleshoot Increase the buffer size 1 Start the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program 2 Right click the computer name and select Properties on the menu 3 Click the Advanced tab and enter a new value in seconds in the Buffer field Click OK 4 If the error occurs again contact Technical Support for Dionex products for assistance Doc 065342 06 12 11 281 Dionex ICS 5000 Operator s Manual 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 s
154. Try to toggle the injection valve from Load to Inject by clicking the Load and Inject buttons on the TC ePanel or Control panel 4 Ifthe error occurs again contact Technical Support for Dionex products for assistance A You do not have the privilege to approve the module s qualification Or A You do not have the privilege to change the performance limits Or A 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 298 Doc 065342 06 12 11 8 TC Troubleshooting To troubleshoot The Chromeleon 6 8 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 8 30 TC ALARM LED Is Lighted If the ALARM LED lights red check the Chromeleon Audit Trail for the cause e Gas leak inside the TC 1 Find and eliminate the leak 2 If you are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Humidity le
155. Yes optional Electrical Main Power Requirements 90 265 VAC 47 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Typical input power 200 W Maximum line draw 9 2 A at 110 VAC Fuse Requirements Two IEC 60127 2 slow blow fuses P N 954772 rated at 10 A 250 V Doc 065342 06 12 11 A DC Specifications Dionex ICS 5000 DC Detector Chromatography Compartment Specifications Physical Specifications Dimensions 44 5 x 42 x 57 cm 17 5 x 16 5 x 22 5 in h x w x d Weight 38 kg 84 Ib Flow Path All polymeric PEEK anion or cation configurations Environmental Operating Temperature 4 40 C 40 104 F Operating Humidity 5 95 relative humidity noncondensing Dionex ICS 5000 Conductivity Detector Specifications Electronics Type Microprocessor controlled digital signal processing autoranging Cell Drive 8 kHz square wave Linearity 1 Resolution 0 00238 nS cm Output Range Digital Signal Range 0 15 000 uS cm Analog Signal Range 0 15 000 uS cm Noise Wet lt 0 2 nS at 23 uS cm background lt 0 1 nS at 1 uS cm background Filter Rise times 0 to 10 s programmable Sampling Rate 1 to 100 Hz user settable or automatic Cell Temperature 5 C above DC upper zone temperature to 60 C maximum User settable working range is identical to settable range Cell Temp
156. _ gt gt ML Pe Device To the degasser Regen In via the EG rear chase To AS Waste A 4 To Waste ly Figure 3 10 Analytical IC Single RFIC EG System with Post Column Reagent Addition Bromate Doc 065342 06 12 11 139 Dionex ICS 5000 Operator s Manual Pump front view SP To the pump inlet via the pump rear chase Seal Wash Pump pump not to scale Deionized Water fa l To waste Lv 1 Ballast o i Bottle i To the oO Oc VP lt j CS DC front view EG left side view gt To the CR TC Regen In ino uabay JasseBap y WoJH dm A gt Y 5S Lia emp Amino Trap or PA20 Guard Be W S Backpressure Y CE jE Pa Device a From AS gt 1 2 a From the degasser Eluent Out To the CR TC Regen In via he se chase To AS Waste To Waste D Figure 3 11 Analytical IC Single RFIC EG System with ED and VP for Carbohydrate Analysis 140 Doc 065342 06 12 11 4 Startup This section is an overview of the steps required to start up the Dionex ICS 5000 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 a
157. a different type of Error page 252 cartridge Pump is disconnected The EG mode is off Warning page 253 Table 8 2 EG Error Messages Continued 8 1 3 DC Error Messages Table 8 3 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 Level CD cell option disconnected Abort page 259 CD cell over safe temperature Abort page 260 Column temperature open circuit Abort page 260 Column over safe temperature Abort page 260 Column temperature calibration error Warning page 261 Table 8 3 DC Error Messages Doc 065342 06 12 11 207 Dionex ICS 5000 Operator s Manual DC Related Audit Trail Error Message Default Severity Level Compartment temperature open circuit Abort page 261 Compartment over safe temperature Abort page 261 Compartment temperature calibration error Warning page 261 ED cell current exceeds limits error Warning page 261 ED cell option disconnected Abort page 262 ED cell working electrode disconnected Abort page 263 ED pH offset calibration failed Warning page 263 ED pH slope calibration failed Warning page 264 ED reference electrode disconnected Warning page 264 High pressure valve 1 error Abort page 265 High pressure valve 2 error High pressure valve 3 error High pressure valve 4 err
158. acuum degassing module to the CPU board Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the user 238 Doc 065342 06 12 11 8 DP SP Troubleshooting 8 18 DP SP Digital I O Port Inoperative 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 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 The device being triggered may require a TTL not a relay Connect the device to a pump TTL output Doc 065342 06 12 11 239 Dionex ICS 5000 Operator s Manual 240 Doc 065342 06 12 11 Bae EG Troubleshooting 8 19 Troubleshooting EG Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon Audit Trail A Concentration out of range The maximum value is 1 Or A Concentration out of range The maximum value at time 1 is 2 The allowable eluent concentration depends on the flow rate and the EGC type Th
159. ad and Piston 317 9 7 2 Cleaning the Piston 0 0 0 0c eee ee eee 320 x Doc 065342 06 12 11 Contents 9 7 3 Removing the Main Piston Seal 320 9 7 4 Removing the Piston Seal Wash Seal 321 9 7 5 Installing the Piston Seals and O Ring 321 9 7 6 Reinstalling the Piston and Pump Head 323 9 8 Replacing the Piston 0 eee eee eee eee 323 9 8 1 Removing the Pump Head and Piston 324 9 8 2 Reinstalling the New Piston 325 9 8 3 Reinstalling the Pump Head 325 9 9 Replacing the Piston Seal Wash Tubing 326 9 10 Replacing the DP SP Priming Valve Knob Seal 329 9 11 Changing the DP SP Main Power Fuses 330 EG SEVICE oil eee lea 333 9 12 Replacing Tubing and Fittings LL 333 9 12 1 Tubing and Fittings for Capillary IC EG Channels 333 9 12 2 Tubing and Fittings for Analytical IC EG Channels 335 9 13 Isolating a Restriction in the Liquid Lines 336 9 14 Replacing the EGC voir ada aa Aunt 336 9 14 1 Removing the Old EGC 0 004 337 9 14 2 Disposing of the Old EGC 339 9 14 3 Storing an Old EGC 0 eee eee 339 9 14 4 Installing and Conditioning a New Capillary EGC 340 9 14 5 Installing and Conditioning a New Analytical EGC 345 9 15 Replacing the CR TC 0
160. ain 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 The fuse cartridge is located next to the main power switch see Figure 9 13 Use a small screwdriver to remove the fuse cartridge Replace the two fuses with new 2 A IEC 60127 2 slow blow fuses P N 954773 Thermo Fisher Scientific recommends always replacing both fuses Fuse Cartridge Reinstall the fuse cartridge Reconnect the main power cord to its source and to the DP SP Figure 9 13 DP SP Fuse Cartridge Turn on the main power switch Press the POWER button on the front of the DP SP to turn on the pump Reconnect the pump to the software by clicking Connected on the Pump panel Turn on the pump flow Doc 065342 06 12 11 331 Dionex ICS 5000 Operator s Manual 332 Doc 065342 06 12 11 feel EG Service 9 12 Replacing Tubing and Fittings Ea 9 12 1 Tubing and Fittings for Capillary IC EG Channels Table 9 4 lists the tubing and fittings used to plumb an EG channel for capillary IC Tubing Fitting Size Color P N Use to connect and Type Tubing assembly Blue 072203 CR TC ELUENT OUT to EG precisio
161. ak inside the TC 1 Findandeliminate the leak 2 Ifyouare using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Failure of a mechanical component If a VALVE LED is flashing a mechanical component in the TC injection valve has failed Replace the injection valve pod see Section 9 32 If you are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the Doc 065342 06 12 11 299 Dionex ICS 5000 Operator s Manual ClearAlarmLED button If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button If the OVEN LED is flashing a mechanical component in the TC has failed These parts are not user serviceable Contact Technical Support for Dionex products for assistance 8 31 Liquid Leaks from TC Components Leaking fitting Locate the source of the leak Tighten or if necessary replace the liquid line connection see Section 9 29 Broken liquid line Replace the line with tubing of the same length and internal diameter see Section 9 29 Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked Also make su
162. als or well plates and load them into the sample tray or carousel The autosampler manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Starting Chromeleon 7 Starting the Chromeleon 7 Instrument Controller Service To start the Chromeleon 7 Instrument Controller Service right click the Chromeleon tray icon X which is crossed out in red and click Start Chromeleon Instrument Controller The icon changes to gold to indicate that the Instrument Controller Service is starting When the Instrument Controller Service is running idle the icon changes to gray W 4 If the Chromeleon Tray Icon is not on the taskbar click Start gt All Programs gt Chromeleon 7 gt Services Manager to open the Services Manager and click Start Instrument Controller Starting the Chromeleon 7 Client 1 To start the Chromeleon 7 client click Start gt All Programs gt Chromeleon 7 gt Chromeleon 7 2 To display the Chromeleon 7 ePanel Set click the Instruments category bar on the Console Click your instrument in the Navigation Pane Chromeleon 7 connects to the instrument and displays the ePanel Set see Figure 4 3 The ePanel Set opens to the Home panel by default This panel displays basic status information for each instrument in the system Doc 065342 06 12 11 149 Dionex ICS 5000 Operator s Manual In addition a limited number of device functions can be controlled directly from this panel You can a
163. alue within the allowed range Refer to Appendix A for flow rate specifications 2 Check the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the pump and EGC are linked Doc 065342 06 12 11 243 Dionex ICS 5000 Operator s Manual Current linked pump is capillary Please install a capillary EGC Or Current linked pump is analytical Please install an analytical EGC This error occurs if the type of pump linked to the EGC does not match the EGC type A capillary EGC can only be used with a capillary pump and an analytical EGC can only be used with an analytical pump To troubleshoot 1 Install the correct type of EGC for the pump type 2 Fora hybrid system a dual system with both an analytical and a capillary pump check the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the correct pump is linked to the EGC EG1 cartridge disconnected Or EG2 cartridge disconnected This error occurs if Chromeleon sends a command to set an EG parameter when the EGC is disconnected To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance The EGC con
164. alve assembly on the top of the pump head Tighten the check valves fingertight and then use the 1 2 inch wrench to tighten an additional one quarter to one half turn Overtightening may damage the pump head and check valve housing and crush the check valve seats 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 Reconnect the pump to the software by clicking Connected on the Pump panel Doc 065342 06 12 11 315 Dionex ICS 5000 Operator s Manual 9 7 Replacing Piston Seals 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 Removing the pump head and piston Section 9 7 1 Cleaning the piston Section 9 7 2 Removing the main piston seal Section 9 7 3 Removing the piston seal wash seal Section 9 7 4 Installing new seals Section 9 7 5 Reinstalling the piston and pump head Section 9 7 6 NOTE Capillary IC pumps and analytical IC pumps use different main piston seals and piston seal wash seals Before continu ing verify that you have the correct seal for your pump type Part numbers are shown on Figure 9 6 and Figure 9 7 Before beginning locate the following items in your pump ship kit 3 0 mm hex key P N 062338 10 32 fitting plugs
165. and 276 Can t find TC3000 HEX image 276 Can t start acquisition 277 Can t start TC firmware 277 Can t use device x 278 Card data checksum error 279 Command unavailable in demo mode 279 Communication error 279 Communication interface is closed 292 Communication time out 280 Compartment door is open 293 Configuration doesn t match 280 Configuration mismatch 280 Counter x exceeded its limit 293 Current flow out of limits 280 Current pressure out of limits 281 Current temperature out of limits 281 Data buffer overrun 281 Data format on chip card unsupported 293 Device control feature not available 282 Device is not remote 282 Device not found on USB 283 Either the current date is 283 Error deleting flash memory 283 Error during storing of card data 284 Error finishing download 277 Error programming flash memory 284 Executing this command will reset 284 Firmware download in progress 285 Doc 065342 06 12 11 Index 7 Dionex ICS 5000 Operator s Manual Gas leak detected 285 Humidity leak detected 285 Illegal parameter 286 Injections limit has been exceeded 294 Injections limit will be exceeded 294 Invalid date time format 286 Invalid enumerated value 286 Next qualification is due 286 Next qualification is overdue 287 Next qualification was due on 287 Next service is due in 287 Next service is overdue 287 No chi
166. ard feature System Wellness and Predictive Performance Yes standard feature Application Templates Yes standard feature Automation Support of 3rd Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Customizable System Control Panels Yes standard feature Signal Channels Pump pressure Data Trending Plots Yes all device numerical parameters System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature Doc 065342 06 12 11 A Specifications ICS 5000 SP Single Pump and DP Dual Pump Specifications Continued System Trigger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory present and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks Requirements GLP Compliance Yes optional Electrical Main Power 90 264 VAC 47 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 Fuse Requirements Two IEC 60127 2 slow blow fuses P N 954773 rated at 2 A 250 V Physical Dimensions h x w x d 36 x 21 x 48 cm 1
167. are installing an ED detector in a system that previ ously was set up for conductivity detection remove the sup pressor cartridge from the IC Cube and replace it with a suppressor bypass cartridge P N 072055 For IC Cube car tridge installation instructions see Section 9 26 1 Doc 065342 06 12 11 405 Dionex ICS 5000 Operator s Manual 406 Doc 065342 06 12 11 fa TC Service CAUTION MISE EN GARDE VORSICHT 9 29 To avoid injury wait for the TC to cool down before opening the door or performing any maintenance or service procedures Afin d viter toute br lure laisser refroidir le compartiment thermique avant d ouvrir la porte ou d effectuer des op rations de maintenance 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 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
168. artment Specifications Temperature Range 5 85 C max 18 C below ambient in 0 1 C increments Temperature Accuracy 0 5 C Performance Stability 0 1 C Precision 0 1 C Heat up Cool down Time Typically 15 min 20 C to 50 C and 50 C to 20 C High Pressure Valve 6 port 2 position Rheodyne PEEK injection valve Types 10 port 2 position Rheodyne PEEK switching valve Column Capacity Three column sets 1 9 mm Maximum Column 300 mm 50 mm guard column Length Precolumn Heat Two low delay volume exchangers Exchangers optional Leak Detection Humidity and vapor sensors TTL and Relay Inputs Two digital inputs outputs and Outputs Two relay outputs Control Chromeleon Chromatography Data System Computer Connection USB Electrical Main Power 90 264 VAC 47 63 Hz Auto sensing power Requirements supply no manual voltage or frequency adjustment required Power limit 150 W Fuse Requirements Two IEC 60127 2 time lag fuses P N 954776 rated at 2 A 250 V Physical Dimensions 17 4 x 44 4 x 50 3 cm 6 8 x 17 5 x 19 8 in Weight 15 4 kg 34 Ib Doc 065342 06 12 11 433 Dionex ICS 5000 Operator s Manual ICS 5000 TC Thermal Compartment Specifications Continued Environmental Operating Temperature 10 35 C 50 95 F Operating Humidity 5 80 relative noncondensing 434 Doc 065342 06 12 11 ICS 5000
169. as 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 repeat Step 4 320 Doc 065342 06 12 11 9 DP SP Service 9 7 4 Removingthe Piston Seal Wash Seal 1 Remove the O ring P N 040695 from the seal wash body If this is a capillary pump also remove the backup ring 2 Follow these steps to remove the piston seal wash seal 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 7 5 Installing the Piston Seals and O Ring 1 Follow these steps to reassemble the seal wash body a Place the seal wash body on a clean work surface b Slide the new seal wash seal with the open side of the seal facing upward onto the seal insertion tool P N 063675 see Figure 9 8 Piston Seal Wash Seal P N 068628 Capillary P N 063382 Analytical Seal Insertion Tool P N 063675 Figure 9 8 Piston Seal Wash S
170. ase 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 Unknown error code This error occurs if Chromeleon does not recognize the error code sent by the TC firmware To troubleshoot The firmware cannot be serviced by the user Contact Technical Support for Dionex products for assistance A Unknown format of the card data This error occurs if Chromeleon does not recognize the format of data stored on the column ID chip card To troubleshoot 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box Doc 065342 06 12 11 297 Dionex ICS 5000 Operator s Manual 3 Under TC select the column name and select the FormatChipCard command 4 For Chromeleon 6 8 click Execute 5 If the error occurs again insert a new column ID chip card see Section 9 30 X position 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 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
171. asured 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 17 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 4 describes the settings You select the preferred settings on the detector panel on the Chromeleon 7 ePanel Set see Figure 2 34 or Chromeleon 6 8 panel tabset Analog Output Values Description Setting 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 1 V select a full scale voltage output of 1 V Range Conductivity Sets the full scale detector 0 01 to 15 000 uS response value The range to use DC Amperometry depends on the detector readings 50 pA to 300 uA expected for the application For Integrated example selecting a range of Amperometry 20 micro Siemens uS will limit 50 pC to 200 uC you to viewing conductivity readings of 20 uS or less Table 2 4 Analog Output Configuration Settings Doc 065342 06 12 11 85 Dionex ICS 5000 Operator s Manual Analog Output Setting Recorder calibration
172. ate 4 22 2010 Last Calibration Date 4 22 2010 Dummy Cell Control Cell Control Normal gt Service Wellness Figure 9 49 Wellness Panel Dionex ICS 5000 Conductivity Detector Chromeleon 6 8 Version Shown 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 inlet Verify that backpressure at the pump is at least 7 MPa 1000 psi at 0 01 mL min for capillary or 1 00 mL min for analytical Set the cell heater to 35 C Allow the cell to reach this temperature the LED stops blinking Begin pumping 1 0 mM KCI through the cell at 0 01 mL min for capillary or 1 0 mL min for analytical Wait until the total conductivity reading stabilizes 15 to 30 minutes On the Wellness panel click Calibrate After calibration the conductivity reading should be 147 00 2 uS If this is not the case repeat the calibration To record the new calibration value in the Audit Trail click Log 380 Doc 065342 06 12 11 9 DC Service 12 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
173. ator Accessory and Stand P N 074423 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 074422 Reagent Free IC with Electrolytic Sample Preparation RFIC ESP RFIC ESP systems enable a range of automated sample preparation techniques which use proprietary electrolytic devices to provide reduced cost and higher value analyses RFIC ESP devices and techniques can be used for removing cations from an anion sample before analysis by using a Dionex CR TC device or neutralizing a strongly acidic or basic solution 25 phosphoric acid or sodium hydroxide solutions for example with an AutoNeutralization device An Electrolytic Water Purifier is available which provides water of extremely high purity backgrounds below sub ng L levels are possible for use in trace level analytical work where use of a concentrator column is necessary 6 Doc 065342 06 12 11 1 Introduction Dionex ICS 5000 Detector Chromatography Module DC The DC provides a temperature controlled environment for Dionex ICS 5000 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 detectors e Electrochemical de
174. ble removal 383 Analytical IC system version 69 Capillary IC system version 69 Cell calibration 379 Cell description 69 Cell temperature control 69 Description 69 Effect of temperature on conductivity 69 Leaking 270 Replacement procedure 382 Specifications 427 Temperature compensation 70 Configuration drawings 129 139 Connected LED DC LED is lighted 51 Connected LED DP SP LED is lighted 22 Connected LED EG LED is lighted 37 115 Connected LED TC LED is lighted 115 Counter electrode 75 76 CRD bypass cartridge for IC Cube 56 CRD cartridge for IC Cube 56 CR TC trap column 5 42 Contamination 225 Hydration procedure 351 Replacement procedure 349 354 CSRS 300 71 Cyclic voltammetry 105 Data collection rate 105 Example 106 Sweep rate 106 Triangle waveform 106 Waveforms 105 107 D Daily maintenance DC 199 DP SP 195 EG 197 TC 201 Data Displaying 3D amperometry data 110 Reprocessing amperometry data 109 Data collection rate Cyclic voltammetry 105 Electrochemical detector 110 Integrated amperometry 107 Data compression Cyclic voltammetry 105 DC amperometry 102 Entering the potential 102 DC Temperature Calibration Kit 64 Index 4 Doc 065342 06 12 11 Index Declaration of Conformity 19 Degassing eluents 25 Deionized water requirements 20 Detector See Conductivity Detector CD See Electrochemical Detector ED Detector output Low 224
175. c Refer to Section 4 9 for a list of valid concentration ranges for the cartridges and then edit the program as required DP SP flow rate is too low Increase the DP SP flow rate Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Technical Support for Dionex products for assistance 8 5 Peak Retention Times Are Too Late Eluent concentration setting is too low The correct eluent concentration setting depends on several factors the flow rate EGC type etc Refer to Section 4 9 for a list of valid concentration ranges for the cartridges and then edit the program as required DP SP flow rate is too high Decrease the DP SP flow rate Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Technical Support for Dionex products for assistance 8 6 No Peaks 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 220 Doc 065342 06 12 11 8 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 e Injection valve is not actuating or the sample loop is plugged 1 Testthe valve by manually switching the position from the DC ePanel in Chromeleon 7 or Control panel in
176. c Chromeleon commands for controlling sample injection with a Dionex AS DV Autosampler Time Command Yalue az E 1 Flow 0 000 18 19 20 21 Pump_1 B Value 0 0 22 Pump_1 C Value 0 0 23 Pump_1 D Value 0 0 7 Pump_1 Curve Figure 5 10 Commands for Loading and Injecting Sample with a Dionex AS DV Chromeleon 7 Script Editor Shown Doc 065342 06 12 11 181 Dionex ICS 5000 Operator s Manual Figure 5 11 shows the basic Chromeleon commands for controlling sample injection with a Dionex AS Autosampler Time Command Yes 53 Wait Sampler SampleReady Hi 55 Sampler Load 56 Wait Sampler CycleTimeState 57 Sampler Inject 58 Wait Sampler InjectState Hold ri dA anah as Me Mh ad li dd da Figure 5 11 Commands for Loading and Injecting a Sample with a Dionex AS Chromeleon 7 Script Editor Shown For details about controlling an autosampler refer to the operator s manual for your autosampler The manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 182 Doc 065342 06 12 11 6 Shutdown ee DP SP Shutdown If the Dionex ICS 5000 Dual Pump DP or Dionex ICS 5000 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
177. c office Before replacing any part refer to the troubleshooting information in Chapter 8 to correctly identify the cause of the problem Substituting non Dionex Thermo Fisher Scientific parts may impair a IMPORTANT module s performance thereby voiding the product warranty Refer to the warranty statement in the Dionex Terms and Conditions for more information Connecting Capillary Tubing When connecting precision cut 0 062 mm 0 0025 in ID blue PEEK tubing capillary tubing to a port make sure the ferrule and fitting bolt are at least 2 mm 0 1 in from the end of the tubing before you insert the tubing into the port Do not position the ferrule and fitting bolt flush with the end of the tubing Doc 065342 06 12 11 303 Dionex ICS 5000 Operator s Manual Figure 9 1 illustrates the correct and incorrect placement of the ferrule and fitting bolt on the tubing Correct Incorrect Figure 9 1 Correct and Incorrect Ferrule and Fitting Bolt Placement for Capillary Tubing Connections High Pressure Fitting and Ferrule Shown Follow the steps below to install capillary tube fittings 1 Install the fitting bolt and ferrule onto the tubing Position the ferrule at least 2 mm 0 1 in from the end of the tubing see Figure 9 1 2 Insert the tubing into the port until it stops 3 While maintaining pressure on the tubing to keep it in place in the port tighten the fitting bolt fingertight 4 If yo
178. cifications listed in Section 1 5 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 piston 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 Thermo Fisher Scientific the seal wash system is connected to pump 1 the bottom pump If 26 Doc 065342 06 12 11 2 Description Analytical 2 2 6 IC may 2 2 7 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 7 NOTE For users who need to operate a piston seal wash system for both pumps in the DP Thermo Fisher Scientific offers an External Seal Wash Kit P N 063518 or a second seal wash system P N 068661 Static Mixer Analytical IC only For an analytical pump 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
179. cing 333 Requirements 333 Fittings TC Replacing 407 Requirements 407 Flow restrictions 196 Front description DC Buttons and LEDs 51 Front description DP SP Buttons and LEDs 21 22 Front description EG Buttons and LEDs 37 Front description TC LEDs 115 Full scale analog output 86 Response range 85 Voltage output ranges 85 Fuses DC 81 Replacement procedure 371 Fuses DP SP 30 Replacement procedure 330 Index 8 Doc 065342 06 12 11 Index Fuses EG 46 Replacement procedure 357 Fuses TC 119 Replacement procedure 413 G Gas leak in TC 115 126 285 Gas sensor 126 285 Gas separator waste tube 72 Installation 142 Reordering 442 Gas vent line EG 46 Glassy carbon electrodes 75 GM 3 Gradient Mixer 27 219 436 GM 4 Gradient Mixer 27 219 436 Gold electrodes 75 Gradient proportioning valves 25 H Half cells 77 Heater Conductivity cell 69 Reaction coil 101 High pressure limit Limit is tripped 233 234 Selecting 158 High pressure fittings 305 High pressure inline filter 36 High pressure valve error 265 High pressure valves AM Controlling 98 Flow schematics 96 Installed in AM 94 Rebuilding 366 Reordering 441 Replacing 367 High pressure valves DC 65 10 port valve 68 4 port valve 66 6 port valve 67 For analytical IC system 65 For capillary IC system 65 High pressure valves TC 117 122 Reordering 445 Humidity leak in TC
180. click Execute Doc 065342 06 12 11 293 Dionex ICS 5000 Operator s Manual The injections limit for the column has been exceeded Or The injections limit will be exceeded for the column x Chromeleon monitors 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 A 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 A 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 A 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 runs a series of self diagnostics in which the status of the main components is checked This error occurs if a component is not ready for operation 294 Doc 065342 06 12 11 8 TC Troubleshooting To troubleshoot 1 Open the Chr
181. compartment of the DC see Figure 2 21 Two versions of CD are available e A capillary CD P N 072041 for use in systems running capillary flow rates e An analytical CD P N 061716 for use in systems running analytical standard bore or microbore flow rates The features and functions of the two CD versions are the same However because the cell volumes of the two are different the versions are not interchangeable The CD version must match the system type capillary IC or analytical IC If the CD version and system type are mismatched chromatograms will be affected for example broad peaks or lowered sensitivity Heated Conductivity Cell The flow through conductivity cell measures the electrical conductance of analyte ions as they pass through the cell Two passivated 316 stainless steel electrodes are permanently sealed into the PEEK cell body The cell design provides efficient sweep out low volume lt 1 uL and low dispersion Temperature control and compensation help ensure good peak reproducibility and baseline stability Temperature Control Temperature directly affects the conductivity of a solution For example laboratory heating and air conditioning systems can cause a regular slow Doc 065342 06 12 11 69 Dionex ICS 5000 Operator s Manual 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
182. connector and the power source Check that the wall outlet has power If the POWER LED still fails to light contact Technical Support for Dionex products for assistance 8 22 Liquid Leaks in the EG Analytical Ab IC Leaking fitting Locate the source of the leak Tighten or replace liquid line connections as needed see Section 9 12 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 EGC leaks Replace the EGC see Section 9 14 Analytical IC only RFIC Eluent Degasser leaks Replace the analytical IC system RFIC Eluent Degasser see Section 9 16 254 Doc 065342 06 12 11 8 EG Troubleshooting 8 23 No Flow Analytical IC 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 5 and resume operation DP SP pressure limit tripped Verify that the Current Pressure reading on the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset is between the high and low limits displayed on the panel For details see Section 4 8 NOTE The analytical EGC requires at least 14 MPa 2000 psi of backpressure for optimal removal of electrolysis gas from the
183. contact Technical Support for Dionex products for assistance Camshaft sensor always alight Or 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 Technical Support for Dionex products for assistance Degasser malfunction The vacuum degassing module monitors the vacuum system continuously If 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 Be careful not to overtighten fittings 2 Turn off the DP SP power for 30 seconds and then restart the pump 3 If the message appears again the vacuum degassing module should be replaced Contact Technical Support for Dionex products for assistance 228 Doc 065342 06 12 11 8 DP SP Troubleshooting 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 3 Be careful not to overtighten fittings Invalid flow value This error occurs if you enter an invalid value for the DP SP flow rate in Chromeleon To tro
184. corrugated drain hose P N 055075 is connected to this port during installation Place the free ends of the vent lines and drain hose into a waste container To maintain a positive siphon position the waste container below the level of the EG For correct drainage make sure the vent lines and drain hose are not bent pinched or elevated at any point Do not allow the ends of the lines to be submerged in waste liquid 2 9 EG Flow Schematics Liquid flows through the EG components in the following order e The pump delivers deionized water to the EGC Direct current is applied to the EGC to produce eluent e The electrolytically generated eluent flows to the CR TC which traps ionic contaminants and then into the degasser e After exiting the degasser the eluent flows through the backpressure coil if installed through the injection valve to the separator column and finally to the detector cell e The detector cell effluent is directed through the suppressor regenerant chamber to the degasser regenerant tubing through the CR TC regenerant chamber and finally to waste The flow paths for a capillary IC and an analytical IC system are the same However in a capillary IC system a degasser cartridge is located in the IC Cube inside the DC In an analytical IC system the degasser is located inside the EG Be Figure 2 13 illustrates the liquid flow path through an EG configured for a capillary IC system TIENI Figure 2 1
185. cted it is reported to Chromeleon 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 065342 06 12 11 203 Dionex ICS 5000 Operator s Manual 8 1 1 DP SP Error Messages Table 8 1 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 Level A program with this name already exists Abort page 227 Abnormal drive current for x x seconds Warning page 227 Camshaft index too early Abort page 228 Camshaft index too late Abort page 228 Camshaft sensor always alight Abort page 22
186. curacy lt 0 1 Analytical at 14 MPa 2000 psi Pressure Ripple lt 1 0 Analytical at 1 0 mL min typical lt 0 2 with damper at 10 uL min at 14 MPa 2000 psi Pressure None required Vacuum Degasser Integrated optional 1 channel for isocratic pump or 4 channel for quaternary pump Piston Seal Wash Standard automatic operation Gradient Formation Quaternary low pressure Analytical only or electrolytic eluent generation at high pressure Analytical and Capillary RFIC EG Gradients 0 1 100 mM Analytical 0 1 200 mM Capillary Doc 065342 06 12 11 415 Dionex ICS 5000 Operator s Manual ICS 5000 SP Single Pump and DP Dual Pump Specifications Continued Gradient Profiles Any combination of an unlimited number of linear convex and concave positive and negative gradient profiles Gradient Proportioning Accuracy and Precision Analytical only 0 5 at 2 mL min Gradient Mixing Analytical only Passive mixers for 2 mm and 4 mm ID columns optional Eluent Generation Optional eluent generation RFIC EG Eluent On Off Valve Electrically actuated standard Leak Sensor Optical standard System Software Software Chromeleon Chromatography Management Software supports Microsoft Windows XP or Vista Automated Procedure Wizards Yes standard feature System Smart Startup and Shutdown Yes stand
187. des 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 216 Doc 065342 06 12 11 8 Troubleshooting Analytical IC 3 seconds Repeat two or three 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 pH Ag AgCl reference electrode glass membrane NOTE To preventair from becoming trapped in the cell in the future increase the backpressure on the cell by connecting backpres sure 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 pH Ag AgcCI reference electrode diaphragm is plugged First try regenerating the pH Ag AgCl 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 30 DC
188. 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 all fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage bottle filled with saturated KCI solution See Section 4 1 2 for detailed instructions Contaminated pH Ag AgCl reference electrode Replace the pH Ag AgCl reference electrode see Section 9 28 5 Doc 065342 06 12 11 273 Dionex ICS 5000 Operator s Manual 8 28 5 Leak in pH Ag AgCl Reference Electrode Compartment Defective pH Ag AgCl reference electrode O ring Replace the pH Ag AgCl reference electrode O ring see Section 9 28 7 8 28 6 Shift in Ag AgCl Reference Potential Faulty pH Ag AgCl 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 pH Ag AgCl reference electrode with no shift Following the steps below measure the pH Ag AgCI reference electrode potential shift by comparing it to the potential shift of an unexposed electrode A spare pH Ag AgCl reference electrode P N 061879 stored in 3 M KCI can be kept on hand for this purpose Using a Digital Voltmeter to Determine Reference Potential
189. e Dionex SRS or Dionex MMS lt 0 28 MPa 40 psi Table 9 10 Suppressor Operating Pressure Ranges To verify that the required amount of backpressure is being generated follow the instructions in Backpressure Coil Pressure Test for Dionex Suppressors Document No 031759 the flier shipped with the suppressor The instructions are also in the suppressor manual on the Thermo Scientific Reference Library DVD P N 053891 If a 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 two or three times to create a pressure difference 384 Doc 065342 06 12 11 9 DC Service 9 28 ED Service Procedures 9 28 1 Disconnecting the ED Cell Before performing an ED cell service procedure follow these instructions to disconnect the cell 1 Turn off the cell voltage from the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset 2 Stop the pump flow 3 Disconnect the cell inlet and outlet lines from the ED cell and disconnect the two electrical cables see Figure 9 52 NOTE Fora capillary IC system disconnect the cell inlet line from the ELUENT OUT port of the IC Cube column cartridge Cables Outlet line Figure 9 52 Disconnecting the ED Cell Cell Configured for Analytical
190. e Pressure property available This error occurs if the device selected to monitor the system pressure is ineligible to do so To troubleshoot 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Under TC select the column name and select the SystemPressure command 4 Enter the name of the pump currently delivering flow for this column 5 For Chromeleon 6 8 click Execute 278 Doc 065342 06 12 11 8 TC Troubleshooting 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 30 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 simulation mode To troubleshoot If a TC is present and connected disable the demo mode 1 Start the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program 2 In the instrument or timebase right click the TC and select Properties 3 On the General tab page clear the Simulation Mode or Demo Mode check box 4 Ifthe TC does not appear in the Module address box click Browse and select the TC Click OK Communication error x This error occurs if there is a communication failure between the TC and the PC on which Chromeleon is installed To troubleshoo
191. e For details about the suppressors refer to the suppressor manuals The manuals are on the Thermo Scientific Reference Library DVD P N 053891 Installation of a suppressor is optional However if one is not used a suppressor bypass cartridge P N 072055 must be installed The suppressor bypass cartridge contains the plumbing connections necessary for eluent and waste flow through the system Doc 065342 06 12 11 57 Dionex ICS 5000 Operator s Manual my Column Heater and Column Cartridge The IC Cube column heater provides a temperature controlled compartment for the capillary guard and separator columns The heater temperature range is from 5 C above the temperature of the upper DC compartment to 80 C A column cartridge slides into the column heater and is secured with two thumbscrews The column cartridge contains the capillary guard column if included and the capillary separator column To access the columns disconnect the inlet and outlet tubing loosen the captive screws and slide the cartridge out of the oven The cartridge hinges open providing access to the columns and column plumbing The capillary columns are ordered separately For information about how to replace columns and column tubing see Section 9 26 2 be EG Degas Cartridge The EG degas capillary cartridge contains a tubing assembly that purges the electrolysis gas from eluent that has been generated by an EG After passing through the degas t
192. e Thermo Scientific Reference Library DVD P N 053891 9 Close the door 9 23 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 074699 4 port P N 061947 6 port P N 061948 10 port NOTE If the valve electronics require service contact Thermo Fisher Scientific Electronics related repair procedures must be performed by Thermo Fisher Sci entific personnel NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product warranty 1 Turn off the pump flow 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 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 3 Open the DC door Doc 065342 06 12 11 367 Dionex ICS 5000 Operator s Manual 4 Disconnect each liquid line connected to the valve 5 Unscrew the locking ring on the outside of the valve see Figure 9 35 and remove the ring Locking Ring Figure 9 35 Unscrew the Locking Ring Va
193. e Dionex ICS 5000 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 072058 2 5 2 Pressurizing Eluent Reservoirs All eluent reservoirs available for use with the DP SP can be pressurized Although the DP SP does not require pressurized reservoirs Thermo Fisher Scientific recommends pressurizing reservoirs with helium or nitrogen under the following circumstances e When using eluents that are sensitive to contamination 34 Doc 065342 06 12 11 2 Description CAUTION MISE EN GARDE VORSICHT When combining aqueous and nonaqueous components for example water 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 Ne mettez jamais les r servoirs d luants sous une pression sup rieure a 0 07 MPa 10 psi Setzen Sie den Eluentbehalter auf keinen Fall einem Druck ber 0 07 MPa aus If you plan to pressurize the eluent reservoirs an optional regulator kit is required The kit is available in two versions When the DC is installed as the topmost module in the system the EO Regulator
194. e Prime button 310 311 With the Prime button 310 Priming valve Leakage from knob 238 Seal knob replacement procedure 329 Problems See Troubleshooting Processing samples 172 Product warranty voiding 303 Program Wizard Waveforms 108 Programs Chromeleon Autosampler control 178 180 Creating programs 172 Proportioning valves 25 Leaks 237 Malfunction 218 220 Pulse damper for capillary pump 27 Pulsed amperometry 103 3D data 109 Chromatogram example 110 Data storage 109 Integration interval 103 Waveform example 103 See also Integrated amperometry Pump See Dual Pump DP Single Pump SP Q Quantification method 176 R Raw data 110 RCH 1 Reaction Coil Heater 101 Controlling 101 Installed in AM 94 Open circuit error 267 Over safe temperature 268 Reordering 444 Reagent Free IC RFIC 1 System configurations 129 140 Rear panel DC 82 AC sockets 81 Analog outputs 82 Description 80 Fuses 81 T O option 82 444 Power switch 81 TTL and relay connectors 82 USB connections 81 Rear panel DP SP Analog pressure output 32 Digital I O port 31 Fuses 31 Power receptacle 31 Doc 065342 06 12 11 Index 13 Dionex ICS 5000 Operator s Manual Power switch 30 USB connections 33 Waste lines 33 Rear panel EG 45 Exhaust fan 45 Fuse cartridge 46 Gas vent line 46 47 Power switch 46 USB connections 45 Waste lines 46 47 Rear panel TC
195. e To Waste Sample Per Carrier Eluent Figure 2 65 TC Injection Valve Flow Schematics 10 Port Valve Example Connections Large Loop to Concentrator e In the 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 Doc 065342 06 12 11 123 Dionex ICS 5000 Operator s Manual e Inthe 1_2 position carrier liquid flows through the sample loop and on 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 23 2 Injection Valve Plumbing Figure 2 66 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 Thermo Fisher Scientific 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 Green TO INJECT SAMPLE IN
196. e 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 Doc 065342 06 12 11 117 Dionex ICS 5000 Operator s Manual 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 analytical 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 24 for details about the column ID system 118 Doc 065342 06 12 11 2 TC Description 2 22 TC Rear Panel Figure 2 62 illustrates the rear panel of the TC 1 Main Power 2 Digital I O USB Receptacle o Drain Port Switch Fuse Connectors 2 B Connector Holder and Power Receptacle Fig
197. e safety limit on page 233 Electrical connections incorrectly installed The electrical cables may not be properly installed Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the user 236 Doc 065342 06 12 11 8 DP SP Troubleshooting 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 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 7 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 6 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 If the check valve continues to leak it is
198. eal 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 065342 06 12 11 321 Dionex ICS 5000 Operator s Manual 4 8 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 g If this is a capillary IC pump place the new backup ring P N 074371 on the seal wash body Rinse the new main piston seal P N 075493 for capillary pump P N 064946 for analytical pump with isopropyl alcohol IPA or dip it into a container of IPA The seal is easier to install when it is moist Insert the piston through the seal wash assembly and then through the new main piston seal 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 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
199. ecialized precision cutter If you need to replace the tubing or to install a different length tubing to accommodate a new column configu ration order an IC Cube Tubing Kit P N 072186 Before installing the new separator column tear off the column label and slide it into the holder on the front of the cartridge see Figure 9 48 If the new column configuration is the same as the previous connect the precision cut tubing that you removed in Step 8 to the new columns 376 Doc 065342 06 12 11 9 DC Service If you are changing the column configuration refer to the following figures for the precision cut tubing required for your configuration e O 250 mm Separator Column SON 65 mm 2 5 in 2 Precision Cut Tubing P N 072188 gt 50 mm Guard Sa Column N S415 mm 4 5 in o O Precision Cut Tubing P N 072189 Figure 9 45 Tubing Connections for 250 mm Separator Column and 50 mm Guard Column 150 mm Separator Column Sw 75 mm 3 in 0 4 2 Precision Cut Tubing P N 074603 x 35 mm Guard Column 115 mm 4 5 in Precision Cut Tubing P N 072189 Figure 9 46 Tubing Connections for 150 mm Separator Column and 35 mm Guard Column Separator Column a 2 210 mm 8 3 in 0 Precision Cut Tubing P N 072187 1 use with any p ag length separator column Figure 9 47 Tubing Connections for Separator Column Only Doc 065342 06 12 11 377 Dionex ICS 5000 Operator
200. ecord the backpressure d Disconnect all components after the injection valve e One at a time reconnect each component of the flow path If reconnecting a component causes an abnormal increase in backpressure replace the component Replace as many components 234 Doc 065342 06 12 11 8 DP SP Troubleshooting as necessary to resume operation at the standard operating backpressure 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 Thermo Scientific Reference Library DVD 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 Technical Support for Dionex products for assistance 8 13 DP SP Does Not Start 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 Flow rate is set to zero Select a Flow rate on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset While being primed pump starts briefly and an alarm sounds If the high pressure limit was tripped 1 Check that
201. ed in Section 1 5 4 Usea sharp tool for example the tip of a safety pin or a straight pin to remove the pH Ag AgCl reference electrode O ring see Figure 9 65 pH Ag AgCl Reference Electrode O Ring Figure 9 65 Removing the pH Ag AgC Reference Electrode O Ring 5 Slide the new O ring P N 014067 onto the electrode Doc 065342 06 12 11 399 Dionex ICS 5000 Operator s Manual 6 To avoid any hydraulic pressure buildup when inserting the pH Ag AgCl reference electrode make sure that fitting plugs are not installed on the cell inlet and outlet fittings 7 Screw the pH Ag AgCl reference electrode into the cell body and tighten fingertight 8 Orient the cell assembly with the yoke knob on the left and push the cell onto its mounting location in the DC compartment see Figure 9 52 9 Reconnect the two cables and the liquid lines 10 Start the pump flow 11 Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 9 28 8 Replacing a PdH Reference Electrode When to Replace a PdH Reference Electrode Replace the PdH reference electrode if its sensing surface is damaged or if the electrode no longer seals properly Replace the PdH electrode if performance has degraded for example lower response higher background or spikes The PdH reference electrode typically lasts several years depending on use Items Needed e PdH reference electrode P N 072075 e Tweeze
202. ed replacement parts NOTE NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product war ranty 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 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 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 Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT Open the TC door 4 Disconnect each liquid line connected to the injection valve Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 410 Doc 065342 06 12 11 9 TC Service 6 Reconnect all liquid lines to the injection valve see Figure 9 75 Green TO INJECT VALVE W 25 pL SAMPLE LOOP Orange TO INJECT VALVE P Figure 9 75 7 Turn on the power to the TC SAMPLE IN from door inject port or autosampler TO INJ VALVE C
203. ediately detect leakage from the membrane barrier because these leaks exit the EG through the vent line 8 9 High System Backpressure 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 EGC is the source of the high backpressure replace the outlet frit as instructed in the EGC manual The manual is on the Thermo Scientific Reference Library DVD P N 053891 3 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 Doc 065342 06 12 11 223 Dionex ICS 5000 Operator s Manual 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 Insufficient sample injected Increase the injection size or concentration ED Only Working electrode fouled 1 2 If a disposable working electrode is being used replace the electrode
204. eets the specifications listed in Section 1 5 7 Clean the polished surface of the cell with a clean damp lint free tissue 8 Install the new gasket 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 9 Verify that the gasket is flat against the cell body and is not wrinkled 388 Doc 065342 06 12 11 9 DC Service 10 11 12 13 14 15 Reinstall the working electrode block and the yoke knob and block Fingertighten the yoke knob by turning it a full 360 degrees NOTE Itis not possible to overtighten the yoke knob Once the knob clicks into place it does not tighten any fur ther The yoke knob ensures constant pressure is applied to the cell Orient the cell assembly with the 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 9 28 4 Polishing an ED Cell Conventional Working Electrode These instructions are for conventional nondisposable working electrodes only Do not polish disposable electrodes When to Polish the Working Electrode Do not polish new conventional working electrodes before installation After an electrode has been used for a pe
205. elect or define a feature that is not available for your TC To troubleshoot Select Help gt About Chromeleon to open the About Chromeleon screen e For Chromeleon 7 click Details to view all license features you purchased devices controlled number of timebases and other software options e For Chromeleon 6 8 the license features you purchased are listed on the About Chromeleon screen and labeled On If necessary upgrade your software by acquiring the corresponding licenses Contact your local Dionex products representative at Thermo Fisher Scientific for assistance 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 connect the TC to the Chromeleon server Check the Audit Trail for messages indicating whether the module was successfully connected 282 Doc 065342 06 12 11 8 TC Troubleshooting 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
206. electrode on a PTFE substrate or a conventional gold electrode 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 providing the solvent is compatible with PEEK tubing There is also no restriction on the use of organic solvents when disposable gold electrodes on PTFE substrate and PTFE gaskets are used Combination pH Ag AgCl Reference Electrode The pH Ag AgCl 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 reference potential of the combination 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 A
207. en However there are also some differences For example palladium is not as good a catalyst for the electrode half reaction as platinum As a consequence under identical conditions the reference potential of the palladium hydrogen electrode differs from that of the standard hydrogen electrode by a constant potential In addition because hydronium ions are involved in the reference half reaction the potential of the PdH electrode is pH dependent Waveforms for PdH Reference Electrodes in Chromeleon When you create or edit an instrument method in Chromeleon 7 or a program in Chromeleon 6 8 you can select a waveform created for use with the PdH reference electrode To use a waveform that was created for a pH Ag AgCl electrode select the waveform and then manually correct the potential values in the Waveform Editor The formula for correction is provided in the Waveform Editor No pH Readout with the PdH Reference Mode If the PdH electrode were connected to another reference electrode for example a Ag AgCl electrode the PdH electrode could serve as a pH indicator electrode However when the PdH electrode functions as a Doc 065342 06 12 11 79 Dionex ICS 5000 Operator s Manual reference electrode it cannot indicate pH In the same manner a glass electrode alone cannot measure pH it must be used with a suitable reference electrode The pH readout of the ED cell is disabled when the PdH reference mode is selected 2
208. en carefully remove the head and place it on a clean surface 9 If the piston was not removed with the pump head in Step 8 remove 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 pis ton to one side and then pull it out of the pump mecha nism 10 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 9 8 2 Reinstalling the New Piston Slide the new piston P N 068646 for capillary P N 062082 for analytical partway into the pump head approximately 6 mm 1 4 in of the sapphire part of the piston should extend from the head 9 8 3 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 Doc 065342 06 12 11 325 Dionex ICS 5000 Operator s Manual 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 POWE
209. en Out via the DC rear chase DC front view EG left side view RFIC EGC Eluent Degasser Cellin Cell Out Regen Regen Regen Out Eluent Out E ai o 1 Eluent In Regen In Li In Out Separator Concentrator Backpressure Device From AS To Waste e To AS Waste I Figure 3 9 Analytical IC Single RFIC EG System with Matrix Elimination Using an SP and a 10 Port Valve 138 Doc 065342 06 12 11 3 Configurations To pump 2 inlet via the pump rear chase To Regen In Pump front view via the DC A To pump 1 inlet A via the pump rear chase rear chase To 3 way valve 1 COM Port 4 via the DC rear chase A Pump 2 Valve To waste pump not to scale TN A 9 A A Piston pa B Seal i c Deionizod Wash jp gionize Deionized To the Pump 1 Water Reagent absorbance Water Regen or PDA detector 109 Y oO Oc gt From the suppressor Regen Out via the DC rear chasema ne ee i To waste DC front view EG plug 4 left side view Reagent in bod YS s fr 2 rom pump P ASS A lt f RCH 1 D 4 Aa A RFIC Eluent Degasser J EGC To waste Cell In Cell Out Rea Leon egen Out Eluent Out Eluent Eluent ry Ea Out y Y A A In luent In Regen In Y s Regen N I Out A In Out I PAN CI Separator L gt NU gt oem p Y W C A 6 3 y N Backpressure rara From AS
210. ent method 172 Panel tabset 11 151 171 Processing method 174 Programs 172 Programs Instrument methods 178 180 Quantification method 176 Sequence Wizard 174 175 Starting 149 151 Troubleshooting communication problems 256 USB connections DC 81 USB connections DP SP 33 USB connections EG 45 USB connections TC 121 User s guide 14 Virtual Column Separation Simulator 172 176 Chromeleon Instrument Configuration 84 408 Assigning TTL input functions 90 Chromeleon Server Configuration 84 408 Assigning TTL input functions 90 Cinch connector Pin assignments 32 Doc 065342 06 12 11 Index 3 Dionex ICS 5000 Operator s Manual CMMS 71 Column clips Reordering 445 Column ID chip card 118 125 Reordering 445 Slots for installation 118 Column ID system 125 Chip card readers 118 Installing a chip card 409 Selecting a column 408 Selecting column properties 409 Column open circuit 260 Column over safe temperature 260 266 Column properties Primary 125 290 295 Secondary 125 Selecting for column ID system 409 Columns Sizes available 62 Commands AS Autosampler control 182 AS AP Autosampler control 181 AS DV Autosampler control 181 Creating a program 172 Commands dialog box 26 126 156 Compartment open circuit 261 Compartment over safe temperature 261 Concentrator column 68 123 Condensation 199 Conductivity Detector CD 3 7 Air bub
211. entially 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 CAUTION injury gt Indicates that the function or process of the instrument may be impaired Operation does not constitute a hazard Messages d avertissement en frangais Signale une situation de danger imm diat qui si elle n est pas vit e entra nera des blessures graves mortelles gt DANGER Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures graves a mortelles gt AVERTISSEMENT Signale une situation de danger potentiel qui si elle n est pas vit e pourrait entrainer des blessures mineures mod r es galement utilis pour signaler une situation ou une pratique qui pourrait MISE EN GARDE gravement endommager l instrument mais qui n entra nera pas de blessures gt Warnhinweise in Deutsch Bedeutet unmittelbare Gefahr MiBachtung kann zum Tod oder schwerwiegenden Verletzungen f hren gt ACHTUNG Bedeutet eine m gliche Gef hrdung Mi achtung kann zum Tod oder schwerwiegenden Verletzungen f hren gt WARNUNG Bedeutet eine m gliche Gef hrdung Mifachtung 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 VORSICHT keine V
212. er sample is loaded into the sample loop and the injection valve is toggled to the Inject position eluent passes through the loop 74 Doc 065342 06 12 11 2 DC Description 2 15 2 15 1 e The eluent sample mixture is pumped through a temperature stabilizer analytical IC only through the guard and separator columns and then through the suppressor e From the suppressor the mixture flows through a CRD if installed to the cell where the analytes are detected A digital signal is sent to Chromeleon software e 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 Regenerant flow is routed through the CRD if installed through the EG degas tubing through the CR TC and then out to waste Q ED Electrochemical Detector One or two Dionex ICS 5000 Electrochemical Detectors EDs can be installed in the DC Each complete ED assembly consists of an amperometric detection 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 21 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 19 1 e Integrated amperometry includes pu
213. er to check the pH of the buffer Dry pH Ag AgCl reference electrode 1 2 Soak the pH Ag AgCl reference electrode in a solution containing 1 M KCl and 1 M HCI long enough to restore the electrode potential to within 30 mV when compared to an unexposed Ag AgCl reference electrode To test the pH Ag AgCl reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 274 Replace the pH Ag AgCl reference electrode see Section 9 28 5 To prevent a pH Ag AgCl 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 all fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage bottle filled with saturated KCI solution See Section 4 1 2 for detailed instructions Shift in ED 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 pH Ag AgCl reference electrode was new e Faulty pH Ag AgCl reference electrode 1 2 Check the electrode by following the instructions in Section 8 28 6 Regenerate the electrode by soaking in a solution containing 1 M KCl and 1 M HCI long enough to restore the electrode potential to within 30 mV when compared to an unexposed Ag AgCl reference electrode T
214. erature Stability lt 0 001 C Cell Temperature Compensation Default 1 7 per C programmable from 0 3 per C Flow Cell Maximum Pressure 10 MPa 1500 psi Flow Cell Volume 0 7 uL Analytical 0 02 uL Capillary Doc 065342 06 12 11 427 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Conductivity Detector Specifications Continued Cell Electrodes Passivated 316 stainless steel Compatible with MSA Cell Body Chemically inert polymeric material Heat Exchanger Inert tortuous path for low axial dispersion System Software Software Chromeleon Chromatography Data System requires Microsoft Windows XP or Vista Automated Procedure Wizards Yes standard feature System Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Application Templates Yes standard feature Automation Support of Third Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Customizable System Control Panels Yes standard feature Signal Channels Conductivity Total Conductivity Data Trending Yes all device numerical parameters plotted System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature System Trigger Commands and Co
215. erletzungsgefahr besteht gt Doc 065342 06 12 11 17 Dionex ICS 5000 Operator s Manual 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 Be Sections preceded with the Capillary IC flag indicate that the information in the section applies to capillary IC systems only Sections preceded with the Analytical IC flag indicate that the information in e the section applies to analytical IC systems only If a section is not flagged the information in the section applies to both capillary IC and analytical IC systems 1 4 2 Safety Symbols These symbols appear on the Dionex ICS 5000 modules or on labels affixed to the modules Alternating current Primary protective conductor terminal Secondary 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 PO 18 Doc 065342 06 12 11 1 Introduction 1 4 3 Declaration of Conformity The cETLus or cTUVus and CE marks on the model data labels on each Dionex ICS 5000 module indicate that the modules are in compliance with the following standards DIONEX MANUFACTURERS DECLARATION OF CONFORMITY Produc
216. erometry View window see Figure 2 57 To open the window 110 Doc 065342 06 12 11 2 DC Description double click the sample in the Browser to open the chromatogram On the View menu click 3D Amperometry elean JANDIKDISK _local 3DAmperometry Jan20_PittconWork 28 mix No6CWE_AcetWash 1 30mix JANDIKDESK2_local 3DAmperometr Ee Eck View Workspace Qualfication Window Help 2x OSU SHS BOK PF el a EEA A E N E EEEN ER ee jai Chromatogram Plot fine 5 Injection Data Mera lwaloht 100 l t Plot current vs waveform time Waveform Plot 10797410 na 125 138 7 727 men 210 00 me 74 na 0 330 v pres Figure 2 57 3D Amperometry View Window in Chromeleon 6 8 The chromatogram plot shown in Figure 2 57 was obtained by plotting integrated current charge nC vs retention time The window is divided into several display areas Sample injection data Displays information about the sample Chromatogram plot Displays a chromatogram of data selected from the selected integration interval in the 3D amperometry data plot 3D amperometry data plot Displays the raw 3D amperometry data Waveform I t plot Displays an I t plot current vs waveform time of selected data and optionally a waveform plot Doc 065342 06 12 11 111 Dionex ICS 5000 Operator s Manual In Chromeleon 6 8 the raw 3D amperometry data plot can be viewed as either an Iso or a 3D wireframe p
217. ers four channels Proportioning Valve Fittings Proportioning Valve Outlet to Primary Pump Head Static Mixer Pump Outlet to EG or Injection Valve Figure 2 4 Analytical Gradient Pump Components NOTE For easier access to pump components when performing ser vice procedures the pump panel can be pulled forward to the front of the pump compartment First make sure that the five red Phillips screws are removed from the component panel Then use the handles to pull the panel forward The upper and lower component panels slide forward together Pump Heads The DP SP is a low 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 24 Doc 065342 06 12 11 Analytical 2 Description 2 2 2 2 2 3 2 2 4 the pulsation increases as the operating pressure increases because part of the delivery stroke is
218. erty and select the Interval option f For Chromeleon 6 8 click the Execute button 4 8 Starting the Pump 1 2 Press the POWER button on the front of the DP SP If any of the following conditions applies prime the pump see Section 9 5 before proceeding e The eluent has been changed e The eluent line is new empty e The eluent line contains air On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab to display the Pump panel see Figure 4 7 ICS 5000 Home AS DC CD ED Pump Audit Queue Enter a new flow rate a sos or click the switch to pi A start the pump at the selected flow rate Rate 2 000 Duration 60s Eluent O0mmn 4000 4 psi 3000 ED2 ED_2_Total max 157 oops 21900 min O psi 0 000 100 Relay 1 Relay 3 Relay 2 Relay 4 Enter the maximum and minimum pressure limits Figure 4 7 Setting the Pump Flow Rate and Pressure Limits Chromeleon 7 Version Shown 4 Enter the Flow rate required for your application This starts the pump flow also Doc 065342 06 12 11 157 Dionex ICS 5000 Operator s Manual 5 If the preferred flow rate is already selected but the pump flow is off click the switch to start the pump at the selected flow rate NOTE After starting the pump or changing the flow rate wait at least 5 minutes longer for flow rates below 1 0 mL min
219. essors Capillary CD Dionex ACES 300 Capillary Dionex CCES 300 Capillary Analytical CD Dionex AAES Dionex CAES Dionex AMMS 300 Dionex CMMS Dionex ASRS 300 Dionex CSRS 300 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 Thermo Scientific Reference Library DVD P N 053891 Capillary IC Suppressor The suppressor for a capillary IC system is installed inside an IC Cube capillary suppressor cartridge For details about the IC Cube and the capillary suppressor cartridge see Section 2 11 2 Analytical IC Suppressor IC The analytical suppressor is installed on clips on the lower area of the analytical CD see Figure 2 27 The suppressor cable plugs into the connector next to the detector Conductivity Detector Suppressor Optional ASRS 300 model shown sn Suppressor Cable Lif si Figure 2 27 Analytical Conductivity Detector with Suppressor System 1 Doc 065342 06 12 11 71 Dionex ICS 5000 Operator s Manual Analytical IC 2 14 3 NOTE Itisalso possible to control an analytical suppressor with a Dionex ICS 5000 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 NOTE To prevent accumulation of oxygen or hydrogen gases c
220. et check valve Double hole assembly to verify that the double hole end of the cartridge see Inlet Check Valve Figure 9 4 is visible Assembly If the double hole end is not visible remove the cartridge from the housing and install it correctly Flow Figure 9 4 Inlet Check Valve Assembly The outlet check valve assembly DR housing has a smaller 10 32 port fi Outlet Check Valve 10 32 Port Inspect the new outlet check valve Single hole assembly to verify that the single rin hole end of the cartridge is visible Valve Assembly see Figure 9 5 If the single hole end is not visible remove the cartridge from the housing and install it correctly Flow Figure 9 5 Outlet Check Valve Assembly 314 Doc 065342 06 12 11 9 DP SP Service 6 NOTE The pump cannot operate properly unless the car tridges 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 Before installing the inlet and outlet check valves rinse the bottom of the check valve ports in the pump head with isopropyl alcohol and blow them clean using a 0 2 micron filtered canned air duster Inspect the bottom of each port for any particulate matter If necessary rinse and dry again until they are clean Install the inlet check valve assembly on the bottom of the primary pump head Install the outlet check v
221. f potential changes is repeated over time By repeatedly pulsing between optimized 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 19 4 for more information about waveforms Pulsed Amperometric Detection In pulsed amperometric detection PAD current is integrated at a single constant potential see Figure 2 50 0 7 Integration Potential Volts 0 1 0 1 E1 Detection Potential E2 Positive Cleaning 0 0 0 2 SERIO da 0 6 Potential Ime Seconds E3 Negative Cleaning l E1 LE2 E3 Potential Figure 2 50 Example Pulsed Amperometry Waveform The potentials labeled E1 E2 and E3 are applied for durations t1 t2 and t3 respectively At t1 the E1 potential is applied After a delay the signal is Doc 065342 06 12 11 103 Dionex ICS 5000 Operator s Manual 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 Integrated Pulsed Amperometric Detection With integrated pulsed amperometric detection IPAD current is integrated at two or more potentials see Figure 2 51 0 60
222. f the DC see Figure 2 16 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 zuganglich ist VORSICHT USB Connections The USB Universal Serial Bus receptacle B type connector allows connection to the PC on which Chromeleon software is installed The two USB ports A type connectors allows 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 072011 Doc 065342 06 12 11 81 Dionex ICS 5000 Operator s Manual 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 Two low pressure valve
223. f the humidity sensor detects an increased concentration of humidity inside the TC To troubleshoot 1 Find and eliminate the leak 2 Ifyou are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button Doc 065342 06 12 11 285 Dionex ICS 5000 Operator s Manual 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 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 Invalid date time format Either use DD MMM YYYY or 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 drop down list box available for this property Next qualification of this module is due in x day s due date is date Or 286 Doc 065342 06 12 11 8 TC Troub
224. feature System Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Doc 065342 06 12 11 419 Dionex ICS 5000 Operator s Manual ICS 5000 EG Eluent Generator Specifications Continued Application Templates Yes standard feature Automation Support of Third Party Instruments Yes fully controls over 300 different instruments including GC HPLC and MS from more than 30 manufacturers Customizable System Control Panels Yes standard feature Signal Channels Eluent concentration Data Trending Plots Device numerical parameters plotted System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature System Trigger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature Eluent Cartridge Information Storage Yes serial number and expiration date Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance Yes optional package provides security system modification history and electronic signatures Electrical Main Power Requirements 90 264 VAC 47 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Typical input power 18 W Maximum line draw 1 A at 110 VAC
225. ference electrode 274 Suppressor 270 Temperature stabilizer TC 300 LED descriptions DC 51 115 LED descriptions DP SP 21 22 Index 10 Doc 065342 06 12 11 Index LED descriptions EG 37 LED descriptions TC 115 Lithium hydroxide eluent 41 Loading samples 178 With a syringe 178 With a vacuum syringe 179 With an autosampler 178 Loading the autosampler tray 146 149 Low detector output 224 Low pressure limit Selecting 158 Lower compartment DC Description 62 Lower oven LED 51 Low pressure valves 82 Controlling 98 External valve outputs DC 82 Flow schematic 97 Installed in AM 94 Reordering 441 Luer adapter fitting Reordering 441 M Main power receptacle DC 81 DP SP 30 EG 46 TC 119 Main power switch DC 81 DP SP 30 EG 46 TC 119 Maintenance annual DC 200 DP 196 EG 197 SP 196 TC 202 Maintenance daily DC 199 201 DP SP 195 EG 197 TC 201 Maintenance periodic DP SP 196 TC 201 Maintenance weekly DC 199 DP SP 195 EG 197 TC 201 Manuals for ICS 5000 system 14 15 Mark analog output 86 Matrix elimination 61 94 System configuration 137 138 Methanesulfonic acid eluent 41 Methanol 76 Microbore IC applications 2 MicroMembrane Suppressor MMS 62 71 See also Suppressor Mixer static 27 Mobile phases See Eluents Moduleware 203 MSQ Plus Mass Spectrometer 3 10 N Needle seal assembly AS 359 362 Nitr
226. fications the Dionex ICS 5000 modules Appendix B Spare parts for the Dionex ICS 5000 modules Reordering Information Safety and Regulatory Information The Thermo Scientific Dionex ICS 5000 Ion Chromatography System was manufactured by Thermo Fisher Scientific Corporation at the following location 527 Lakeside Drive Sunnyvale CA 94088 3603 U S A The Dionex ICS 5000 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 a Dionex ICS 5000 module in a manner not specified by Thermo Fisher Scientific may result in personal injury If there is a question regarding appropriate usage contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientific office Safety Messages and Notes This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the Dionex ICS 5000 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 16 Doc 065342 06 12 11 1 Introduction Indicates a potentially hazardous situation which if not avoided could result in death or serious injury gt WARNING Indicates a pot
227. g 2 11 2 IC Cube for Capillary IC The IC Cube houses components for running capillary IC applications The IC Cube is installed in the upper compartment of the DC For a dual system two IC Cubes can be installed NOTE When an IC Cube is installed a Dionex ICS 5000 Automa tion Manager cannot be included in the DC Each IC Cube includes an injection valve a column heater and four component cartridges that slide into the housing Each cartridge holds a capillary IC component and includes the plumbing required to connect the component to other IC Cube and system components Doc 065342 06 12 11 55 Dionex ICS 5000 Operator s Manual Cartridges for the following components are available carbonate removal device CRD suppressor guard and separator columns and EG degasser NOTE Ifthe IC Cube does not include a CRD or suppressor bypass cartridges must be installed Bypass cartridges provide the internal plumbing connections required for eluent and regen erant flow between IC Cube components Figure 2 18 illustrates the features of the IC Cube CRD Cartridge or CRD Bypass Cartridge Suppressor Cartridge or Suppressor Bypass Cartridge Column Heater and Column Cartridge EG Degas Cartridge O O Injection Valve Figure 2 18 IC Cube Features Be CRD Cartridge or CRD Bypass Cartridge The CRD 200 Capillary cartridge P N 072054 contains a CRD 200 Carbonate Removal Device Capillary The CRD 200
228. g changes to operating parameters especially apparent when operating at high sensitivities Allow a longer system equilibration time up to 2 hours before starting operation Doc 065342 06 12 11 215 Dionex ICS 5000 Operator s Manual Noisy Baseline CD Only Analytical 9 IC PVE IC Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Cell above or below temperature Contact Technical Support for Dionex products for assistance Detector electronics not functioning correctly Run the detector dummy cell diagnostics from the Wellness panel see Section 9 27 Inappropriate suppressor operating conditions Refer to the suppressor manual for the correct operating conditions Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Temperature compensation setting not optimized Optimize the selected setting see Section 2 14 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 Inadequate system backpressure In an analytical IC system add backpressure tubing to the cell outlet see Section 9 27 4 Noisy Baseline ED Only DC Amperometry and Integrated Amperometry mo
229. g smooth flow minimizes noise The low volume lt 0 2 uL of the channel also allows operation with high efficiency narrow bore columns and capillary 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 tubing 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 ED Cell Solvent Compatibility The ED cell can be used with common reversed phase solvents such as methanol and acetonitrile If a disposable working electrode on polyester substrate is used the percentage of methanol should not exceed 30 and the percentage of acetonitrile should not exceed 10 In addition prolonged exposure more than 8 hours of disposable gold electrodes on polyester substrate to eluents containing hydroxide concentrations greater than 100 mM is not recommended Shorter rinse periods of 10 to 20 minutes for example 76 Doc 065342 06 12 11 2 DC Description 2 15 2 the carbonate removal step during monosaccharide and disaccharide chromatography at high hydroxide concentrations do not affect the electrode performance If sustained highly alkaline eluent conditions are required use a disposable gold
230. gCl Reference Electrode When to Replace a pH Ag AgCl Reference Electrode Replace the pH Ag AgcCI 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 pH Ag AgCl reference electrode typically lasts from 3 months to 1 year depending on use NOTE To regenerate a pH Ag AgCl reference electrode soak it in a solution of 1 M KCl and 1 M HCI Items Needed e pH Ag AgCl reference electrode P N 061879 pH Ag AgCl Reference Electrode Replacement Procedure 1 Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector 392 Doc 065342 06 12 11 9 DC Service 2 Unscrew the pH Ag AgCl reference electrode and remove it from the cell body see Figure 9 56 Unscrew the pH Ag AgCl reference electrode Figure 9 56 Removing the pH Ag AgCI Reference Electrode Cell Configured for Analytical IC Shown 3 Unscrew the storage cap from the new pH Ag AgCl reference electrode see Figure 9 57 Save the cap Always store the electrode in the storage cap filled with saturated KCI IMPORTANT solution when the cell is not in use This prevents the pH Ag AgCl reference electrode membrane from drying out and damag
231. ge serial number is not valid for the type of IC system To troubleshoot 1 Verify that an EGC of the correct type capillary or analytical is installed 2 Verify that the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 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 12 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 A pH modifier must be used with a different type of cartridge This error occurs if you attempt to configure an EPM III Electrolytic pH Modifier with an incompatible type of EGC To troubleshoot Verify that the EPM III is paired with an EGC II K CO3 The EPM III cannot be used with any other cartridge type 252 Doc 065342 06 12 11 8 EG Troubleshooting Pump is disconnected The EG mode and CR TC modes are turned off This error occurs if the pump linked to the EG is disconnected from Chromeleon To prevent damage to the EGC and CR TC the modes are automatically turned off to ensure that the EG does not operate when there
232. ge 7 2 Doc 065342 06 12 11 1 Introduction Product Type Product Name Page Detector inside DC Dionex ICS 5000 Conductivity page 7 Detector Dionex ICS 5000 Electrochemical page 7 Detector Accessory inside DC Dionex ICS 5000 Automation page 8 Manager Detector outside DC ICS Series Photodiode Array page 9 Detector ICS Series Variable Wavelength page 10 Detector Thermal Compartment Dionex ICS 5000 Thermal page 8 Compartment Autosampler Dionex AS Autosampler page 9 Dionex AS DV Autosampler page 9 Mass Spectrometer MSQ Plus page 10 Dionex ICS 5000 Dual Pump DP and Dionex ICS 5000 Single Pump SP Each Dionex ICS 5000 pump can be configured for either capillary IC applications or analytical standard bore and microbore IC applications Capillary IC pumps are always isocratic they deliver one eluent Analytical IC pumps can be either isocratic or low pressure proportioned gradient Gradient pumps deliver gradient mixtures of up to four eluent components The eluent composition selected for a gradient pump can be delivered as isocratic isocratic proportioned linear ramp step curved or any combination of these The SP contains one of the following pump types e Isocratic capillary IC pump e Isocratic analytical IC pump e Gradient analytical IC pump The DP contains two pumps in any combination of the three types listed above for example two isocratic capillary IC pumps or two
233. ge to the EGCs the DP SP automatically turns off electrical power to the cartridge when excessive current or voltage is detected Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the user EGC is expended Replace the cartridge see Section 9 14 No communication with Chromeleon 1 Check that the POWER button on the front of the EG is turned on 256 Doc 065342 06 12 11 8 EG Troubleshooting 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 Check the USB connections The EG should be connected to the DP SP or other Dionex ICS 5000 module via a USB cable P N 960777 In addition one module in the system must be connected to the PC on which Chromeleon is installed Check that the EG is configured in Chromeleon and is assigned to an instrument Chromeleon 7 or timebase Chromeleon 6 8 Doc 065342 06 12 11 257 Dionex ICS 5000 Operator s Manual 258 Doc 065342 06 12 11 ICS 5000 SDC Troubleshooting 8 25 Troubleshooting DC Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon Audit Trail CD cell option disconnected To troubleshoot 1 Checkthe
234. gen In Port CRD SUPPRESSOR LODP IN a EG BYPASS BYPASS From CREGENIN b l Autosampler n FIN LOOP OUT 1 SAMPLE ov To Waste ai 7 La Ld From CR TC Eluent Out Port Figure 2 20 IC Cube Eluent and Regenerant Flow Schematic for Electrochemical Detection PdH Electrode Shown 60 Doc 065342 06 12 11 2 DC Description 2 11 3 DC Interior Components for Analytical IC IC Figure 2 21 shows the interior compartments of a DC that is configured with the components for two analytical IC systems System 1 is used for electrochemical detection applications and system 2 is used for conductivity detection applications Upper Compartment Automation 1 Manager Components Electrochemical 2 Detector and Cell Conductivity Detector and Suppressor g Lower Compartment Columns and o injection Valves Figure 2 21 Example DC Interior View Dual Analytical IC System Shown Upper Compartment Features for Analytical IC The upper compartment consists of two sections e The top section houses an optional Dionex ICS 5000 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 18 for details about the AM e The lower section houses either one or two Dionex ICS 5000 Conductivity Detectors CDs one or two Dionex ICS 5000 Electrochemical Detectors EDs or one de
235. he IC Cube and verify that 5000 psi is printed on the label see the figure on the right If 5000 psi is not on the label you must change the high pressure limit to 21 MPa 3000 psi see page 158 or replace the cartridge with an EG degas capillary 5000 psi cartridge that is rated for 35 MPa 5000 psi F P N 074459 P N 074459 Doc 065342 06 12 11 5 Dionex ICS 5000 Operator s Manual Reagent Free IC with Eluent Regeneration RFIC ER IC RFIC ER is available as an option for Dionex ICS 5000 systems without an EG Eluent regeneration uses the suppressor to reconstitute the starting eluent allowing use of a single 4 liter bottle of eluent for up to four weeks Because the system is a closed loop it can run continuously eliminating the need for recalibration or re equilibration during the 28 days of non stop operation RFIC ER uses carbonate carbonate bicarbonate or MSA eluents for isocratic separations on standard bore columns Dionex ICS 5000 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 072058 All eluent reservoirs available for use with the DP SP can be pressurized If you plan to pressurize the eluent reservoirs the optional EO Regul
236. he following configurations are possible e Single system one capillary IC or one analytical IC system e Dual system two capillary IC systems or two analytical IC systems or one system of each type a hybrid Doc 065342 06 12 11 53 Dionex ICS 5000 Operator s Manual ay 2 11 1 DC Interior Components for Capillary IC In capillary ion chromatography systems the upper compartment of the DC houses the required components If the DC is used for capillary IC only the lower compartment is unused The DC upper compartment consists of two sections e The top section houses one or two Dionex IC Cubes IC Cube For details about the IC Cube see Section 2 11 2 The tray slides forward for easy access to components e The lower section houses either one or two Dionex ICS 5000 Conductivity Detectors CDs one or two Dionex ICS 5000 Electrochemical Detectors EDs or one detector of each type For details about the CD see Section 2 14 For details about the ED see Section 2 15 54 Doc 065342 06 12 11 2 DC Description Figure 2 17 shows the upper compartments of a DC that is configured for two capillary IC systems Both systems are configured for conductivity detection 1 IC Cube System 1 3 IC Cube System 2 Conductivity Detector Conductivity Detector 2 Capillary System 1 4 Capillary System 2 Figure 2 17 Example DC Interior View Upper Compartment of a Dual IC System Shown E
237. hen specify the methods and report template later You can also edit other details of the sequence for example add or remove samples after you finish the wizard After you finish the wizard the new sequence is displayed in the Console Data view see Figure 5 3 Creating a New Sequence in Chromeleon 6 8 In Chromeleon 6 8 two wizards are available to help you create a new sequence the Sequence Wizard and the Application Wizard If the program and quantification method have already been created use the Sequence Wizard If you want to create a new program and quantification method in addition to the sequence use the Application Wizard 174 Doc 065342 06 12 11 5 Operation Using the Sequence Wizard 1 On the Sequence Control panel in the Chromeleon 6 8 panel tabset click Create Sequence see Figure 5 4 ICS 5000 22 l Home Sequence Control Status Autosampler Gradient Pumps Eluent Generator Detector Compartment Cond Detector System Log Audit Trail 400 20 0 pl from Pos 1 10 53 23 AM Manually acquired samples will be stored temporarily in a psi CD 1 Total sequence SEQ AMARQUARDT2_localiCS 5000 manual 0 a 1 10 53 23 AM Chromeleon server version 6 80 SR8 Build 2598 Beta CD_1 154575 started serial nurnber 39 Pump_1_Pressure 10 53 37 AM User AMarquardt from AMARQUARDT2 has acquired control Pump 2 Pressure over timebase ICS 5000 ie 202 0 00 0
238. hen inserting the reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings Verify that the pH Ag AgCl reference electrode O ring is present see Figure 9 63 and then screw the pH Ag AgCl reference electrode into the reference electrode well and tighten it fingertight see Figure 9 62 pH Ag AgCl Reference Electrode O Ring Figure 9 63 pH Ag AgCl reference electrode O Ring Orient the cell assembly with the yoke knob on the left see Figure 9 52 and push the cell onto its mounting location in the DC compartment Reconnect the cell inlet and outlet 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 398 Doc 065342 06 12 11 9 DC Service 9 28 7 Replacing the pH Ag AgCl Reference Electrode O Ring 1 Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector 2 Unscrew the pH Ag AgCl reference electrode and remove it from the cell body see Figure 9 64 Unscrew the pH Ag AgCl reference electrode Figure 9 64 Removing the pH Ag AgCI Reference Electrode Cell Configured for Analytical IC Shown 3 To remove any precipitated salt rinse the pH Ag AgCI reference electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications list
239. hoot 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 262 Doc 065342 06 12 11 8 DC Troubleshooting connector on the back of the detector is securely connected to the receptacle on the detector compartment Push here to ensure the detector s electrical connection is secure ED Cell Cable Figure 8 4 Electrochemical Detector Connection Analytical Cell Shown 2 Ifthe error appears again contact Technical Support for Dionex products for assistance The detector electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the user ED cell working electrode 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 ED pH offset calibration failed This error occurs when the pH reading differs by more than 1 0 pH unit from 7 0 which is the value specified for offset calibration This can be caused by too large a change in the Ag AgCl reference potential or by a damaged glass membrane in the pH sensing part of the reference electrode T
240. ibility Liquid leaks 1 Check for leaks from the piston seals Replace the piston seal on any head with a leak see Section 9 7 2 Check for leaks throughout the remainder of the system including the check valves injection valve and columns Tighten or replace fittings as needed DP SP not primed Prime the pump see Section 9 5 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 Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Technical Support for Dionex products for assistance 218 Doc 065342 06 12 11 8 Troubleshooting e Inoperative check valves Replace the check valve cartridges see Section 9 6 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 e Fluent is contaminated 1 Clean all eluent reservoirs thoroughly inside and out with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Dry with clean particulate free air If a reservoir still appears dirty or if
241. ics components cannot be serviced by the user Suppressor over power This error appears when in order to maintain the selected current the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is required to apply a higher voltage than the suppressor can support To troubleshoot 1 Reduce the flow rate 268 Doc 065342 06 12 11 8 DC Troubleshooting 2 Rehydrate the suppressor Refer to the suppressor manual for instructions Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 3 If the error persists replace the suppressor see Section 9 27 2 Suppressor 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 27 2 Suppressor stopped for flow rate This message occurs if the pump flow stops while the suppressor is on The suppressor is automatically turned off to prevent damage to the suppressor To troubleshoot If the pump stopped unexpectedly see Section 8 14 for pump troubleshooting information 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 If the door is fully closed and the error pers
242. idge and pull the cartridge out of the IC Cube 374 Doc 065342 06 12 11 9 DC Service 5 Lift the lid of the column cartridge to open it Figure 9 42 shows the column cartridge when a capillary guard column and a capillary separator column are installed Separator Column Outlet Separator Column Separator Column Inlet Precision Cut Tubing Guard Column e Outlet QO Guard Column Guard Column Inlet Precision Cut Tubing Figure 9 42 Separator and Guard Columns Installed in Column Cartridge Figure 9 43 shows the column cartridge when only a capillary separator column is installed Separator Column Outlet Separator Column Separator Column Inlet Precision Cut Tubing oo o Figure 9 43 Separator Column Only Installed in Column Cartridge Doc 065342 06 12 11 375 Dionex ICS 5000 Operator s Manual 10 Remove the guard column if present and separator column from the column clips Lift up the separator column outlet fitting see Figure 9 44 slightly to free it from the clips and then slide it out of the cartridge Remove the columns from the cartridge Disconnect the tubing from the 4 columns Save the tubing i j Figure 9 44 Separator Column Outlet Fitting NOTE Do not cut the tubing that you removed from the col umns and do not substitute different tubing To ensure good chromatographic results capillary tubing is cut at the factory using a sp
243. il Error Message Default Severity Level Concentration out of range The maximum value Error page 241 at time 1 is 2 Concentration out of range The maximum value Error page 241 is 1 CR TC1 open circuit Abort page 241 CR TC2 open circuit CR TC1 over current Abort page 242 CR TC2 over current CR TC1 stopped because EGC1 OFF Abort page 242 CR TC2 stopped because EGC2 OFF CR TC1 stopped due to zero flow Abort page 243 CR TC2 stopped due to zero flow The CR TC mode is off for a virtual pump Abort page 243 CR TC mode will be turned off for invalid flow Abort page 243 Flow range for analytical EGC 0 100 3 000 mL min capillary EGC 0 001 0 100 mL min Current linked pump is capillary Please installa Abort page 244 capillary EGC Table 8 2 EG Error Messages Doc 065342 06 12 11 205 Dionex ICS 5000 Operator s Manual EG Related Audit Trail Error Message Default Severity Level Current linked pump is analytical Please install Abort page 244 an analytical EGC EG1 cartridge disconnected Abort page 244 EG2 cartridge disconnected EG1 invalid activation date Abort page 245 EG2 invalid activation date EG1 invalid concentration Abort page 245 EG2 invalid concentration EG1 invalid flow Abort page 245 EG2 invalid flow EG1 invalid flow rate concentration Abort page 246 EG2 invalid flow rate concentration EG1 in
244. in power cord from its 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 Doc 065342 06 12 11 371 Dionex ICS 5000 Operator s Manual 9 26 9 26 1 CAUTION 4 The fuse drawer is located above the main power switch see Figure 9 39 Suo A small tab locks the fuse drawer in place Using a small screwdriver Tab press the 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 fuses P N 954772 Thermo Fisher Scientific recommends always replacing both fuses Figure 9 39 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 IC Cube Service Procedures Replacing an IC Cube Cartridge 1 Turn off the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC power To avoid injury wait for the DC to cool down before opening the door or performing any maintenance or service procedures Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance
245. ing connections e O Check eluent reservoir levels and refill as needed O Check waste containers and empty as needed For detailed weekly maintenance instructions for each module see DP SP page 195 EG page 197 DC page 199 TC page 201 7 1 3 Periodic Maintenance O Clean eluent reservoirs when making fresh eluent or as needed see Section 9 4 O Optional Have Thermo Fisher Scientific perform the performance qualification PQ procedure for IC systems For detailed periodic maintenance instructions for each module see DP SP page 196 DC page 199 TC page 201 NOTE There are no periodic maintenance instructions for the EG 7 1 4 Annual Maintenance O Thermo Fisher Scientific recommends performing preventive maintenance on each module annually Preventive Maintenance Kits contain all the required parts for these procedures The following kits are available DP SP Preventive Maintenance Kits e ICS 5000 Analytical Pump Preventive Maintenance Kit P N 075038 192 Doc 065342 06 12 11 7 Maintenance ICS 5000 Capillary Pump Preventive Maintenance Kit P N 075039 DC TC Preventive Maintenance Kits NOTE 0 4 uL Internal Loop High Pressure Valve Preventive Maintenance Kit P N 075040 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 10 Port High Pressure Valve Preventive Maintenance Kit P N 075042 There is no Preventive Maintenance Kit for the EG Doc 065342 06 12 11
246. ing the electrode See Section 6 4 for storage instructions Save the storage cap a A Figure 9 57 pH Ag AgCI Reference Electrode in Storage Cap 4 Rinse the new electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 to remove any precipitated salt 5 Calibrate the pH Ag AgCl reference electrode see Section 9 28 6 Doc 065342 06 12 11 393 Dionex ICS 5000 Operator s Manual 9 28 6 Calibrating the pH Ag AgCl Reference Electrode When to Calibrate Calibrate after installing a new pH Ag AgCl 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 in most cases this is either pH 10 or pH 4 pH Ag AgCl Reference Electrode Calibration Procedure 1 Complete the following if you are calibrating an electrode that is currently in use a Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector b Unscrew the pH Ag AgCl reference electrode and remove it from the cell body see Figure 9 56 c To remove any precipitated salt rinse the pH Ag AgCl reference electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 2 With the pH Ag AgCl reference e
247. ing 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 Thermo Fisher Scientific 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 For users who need to operate a piston seal wash system for both pumps in the DP Thermo Fisher Scientific offers an External Seal Wash Kit P N 063518 or a second seal wash system P N 068661 154 Doc 065342 06 12 11 4 DP SP Startup 1 Note the tubing connected from the peristaltic pump to the seal wash tube on the secondary pump head on pump 1 see Figure 4 5 item Disconnect this tubing from the pump head and connect it to the seal wash tube on the secondary pump head on pump 2 Connection from peristaltic pump to secondary pump head Connection between pump heads Seal Wash Reservoir Inlet Line Seal Wash Reservoir Outlet Line Figure 4 5 Piston Seal Wash Connections to Pump 1 2 Disconnect the short piece of tubing between the primary and secondary pump heads on pump 1 see Figure 4 5 item Connect this tubing to the pump heads on pump 2 3 Disconnect the seal wash reservoir inlet line from the primary pump head on pump 1 see Figure 4 5 item Connect the inlet line to the primary pump head on pump 2 4 Whe
248. inimize downtime The modular system design lets you quickly configure and customize hardware The single channel Dionex ICS 5000 can be configured to run either capillary IC applications or microbore or standard bore IC applications e Capillary IC applications use 0 4 mm diameter columns with flow rates typically from 0 005 to 0 02 mL min e Microbore IC applications use 2 mm diameter columns and with flow rates typically from 0 2 to 0 5 mL min e Standard bore IC applications use 4 mm diameter columns with flow rates typically from 1 0 to 2 0 mL min A dual Dionex ICS 5000 system can be configured with any combination of the above application types for example one capillary IC channel and one microbore IC channel or two capillary IC channels or one microbore IC channel and one standard bore IC channel 1 1 1 Dionex ICS 5000 System Components The table below identifies modules in the Dionex ICS 5000 product line as well as additional products that can be added to a Dionex ICS 5000 system Refer to the page number indicated here for a brief product overview Product Type Product Name Page Pump Dionex ICS 5000 Dual Pump page 3 Dionex ICS 5000 Single Pump page 3 Eluent Generator Dionex ICS 5000 Eluent Generator page 5 Eluent Organizer Dionex ICS 5000 Eluent Organizer page 6 Detector Chromatography Dionex ICS 5000 page 7 Compartment Detector Chromatography Module IC Cube inside DC Dionex IC Cube pa
249. ion 214 Doc 065342 06 12 11 8 Troubleshooting MEIN IC 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 that meets the specifications listed in Section 1 5 DP SP not properly primed Prime the pump see Section 9 5 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 7 Inadequate system or cell backpressure Add backpressure tubing to the cell outlet see Section 9 27 4 or to the pump if no column is installed Analytical EG only System backpressure is below 14 MPa 2000 psi The optimal system backpressure is 16 MPa 2300 psi in an analytical IC system with an EG installed 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 17 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 19 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 followin
250. ion 8 31 Rinse off any dried eluent with ASTM filtered Type I 18 megohm cm deionized water that meets the specifications listed in Section 1 5 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 reglements locaux MISE EN GARDE Neutralisieren Sie saurehaltige und atzende Abf lle vor ihrer Entsorgung Entsorgen Sie alle Abfalle 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 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 Doc 065342 06 12 11 201 Dionex ICS 5000 Operator s Manual e Check for excess condensation 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
251. is no flow 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 12 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 EGC leaks Replace the EGC see Section 9 14 RFIC Eluent Degasser leaks Replace the RFIC Eluent Degasser see Section 9 16 EGC electrical connection is open 1 Tug gently on the EGC electrical cable the locking connector should hold the cable in place see Figure 2 10 2 Ifthe electrical cable is fully seated but the problem persists the cartridge is defective and must be replaced see Section 9 14 EGC input electrical connection has shorted out Replace the EGC see Section 9 14 Doc 065342 06 12 11 253 Dionex ICS 5000 Operator s Manual Electrical error The EG current and or voltage may have become unstable Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography 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
252. is formed and the point where it enters the column This includes the mixer transfer tubing and swept volume in the injector or autosampler Pulse Damper Capillary IC only For a capillary pump flow output from the pressure transducer continues to the pulse damper which smooths minor pressure variations From there flow is directed to the injection valve and then to the remainder of the chromatography system Doc 065342 06 12 11 27 Dionex ICS 5000 Operator s Manual 2 3 DP SP Flow Schematics 2 3 1 Isocratic Pump Flow Schematic Figure 2 5 illustrates the liquid flow path through an isocratic pump CHECK VALVE DI WATER OR ELUENT SECONDARY PRIMARY PUMP PUMP HEAD HEAD INLET CHECK VALVE A d TO ELUENT GENERATOR ELUENT SUPPLY OR INJECTION VALVE ON OFF VALVE Capillary IC pumps only Figure 2 5 Isocratic Pump Flow Schematic e Eluent flows from the reservoir through the vacuum degas chamber 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 eluent generator if installed or injection valve and
253. is message appears if the selected eluent concentration is out of range for the flow rate The time indicated in the message refers to the time specified in the Chromeleon 7 instrument method or Chromeleon 6 8 program To troubleshoot Check the information in Section 4 10 to verify that the selected concentration is within the accepted range for the cartridge type and flow rate Adjust the flow rate or concentration as needed CR TC1 open circuit Or CR TC2 open circuit To troubleshoot 1 Check that the CR TC is correctly plugged into the EG Push the CR TC electrical cable firmly into the CR TC 1 or CR TC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 2 Ifthe error persists the CR TC may be faulty Replace the CR TC see Section 9 15 Doc 065342 06 12 11 241 Dionex ICS 5000 Operator s Manual 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 10 2 Refer to Section 8 23 to determine why liquid flow stopped 3 If the error message appears again contact Technical Support for Dionex products for assistance The CR TC co
254. isco cea agis Boa Keene cite age nes ae wa ene S 222 8 8 Low System Backpressure 0 00 e eee eee eee ee 223 8 9 High System Backpressure LL 223 8 10 Low Detector Output 224 8 11 High Background 225 viii Doc 065342 06 12 11 Contents DP SP Troubleshooting 227 8 12 Troubleshooting DP SP Error Messages 04 227 8 13 DP SP Does Not Start 235 8 14 DP SPStOpS criar 236 8 15 DP SP Liquid Leaks Leak Alarm LL 237 8 16 Vacuum Degassing Module Low Vacuum 238 8 17 Vacuum Degassing Module Does Not Run 238 8 18 DP SP Digital I O Port Inoperative 00 0 0008 239 EG Troubleshooting 0 cece eee ee eens 241 8 19 Troubleshooting EG Error Messages LL 241 8 20 EG ALARM LED Is Lighted 2 0 00 00 e eee eee 253 8 21 EG POWER LED Fails to Light 254 8 22 Liquid Leaks inthe EG 254 8 237 NO BIOW soise eme nyn e EEEE hier 255 8 24 EG Stops Operation s eee re erer tan E E CEEE EEROR 256 DC Troubleshooting 259 8 25 Troubleshooting DC Error Messages 0 00 005 259 8 26 Liquid Leaks from DC Components 270 8 27 VALVE Button Not Working 271 8 28 ED Cell Troubleshooting 0 0 0 0 eee ee eee 271 8 28 1 ED Cell pH Readout Always 7 0 0 271 8 28 2 Cannot Set ED Cell pH Readout to 7 0
255. isocratic analytical IC pumps or one isocratic capillary IC pump and one gradient analytical IC pump Doc 065342 06 12 11 3 Dionex ICS 5000 Operator s Manual The second pump in the DP can be operated as a second channel chromatography pump an auxiliary dependent pump or an auxiliary independent pump Capillary IC pumps operate at flow rates ranging from 0 001 to 3 0 mL min and operating pressures up to 41 MPa 6000 psi without RFIC and up to 35 MPa 5000 psi with RFIC IMPORTANT Capillary IC pumps shipped before February 17 2011 were rated for lower operating pressures than the pumps currently being shipped The older pumps can be operated at pressures up to 35 MPa 5000 psi without RFIC and up to 21 MPa 3000 psi with RFIC Before operating at pressures above these limits verify that you have the appropriate pump e HPC is stamped on the secondary pump heads of the older lower pressure rated capillary IC pumps e HPC 2 is stamped on the secondary pump heads of the newer higher pressure rated capillary IC pumps A Capillary Pump High Pressure Upgrade Kit P N 075994 is available for converting a lower pressure rated capillary IC pump to a higher pressure rated pump The kit includes the HPC 2 secondary pump head and high pressure pump seals NOTE A high pressure EG degas capillary cartridge P N 074459 is also required when operating a capillary RFIC system at pressures up to 35 MPa 500
256. ists contact Technical Support for Dionex products for assistance Doc 065342 06 12 11 269 Dionex ICS 5000 Operator s Manual 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 19 Broken liquid line Replace the line and fittings with the same length and internal diameter tubing see Section 9 19 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 19 Leaking injection valve 1 Make sure the liquid line connections to the transducer are tight Replace any damaged fittings see Section 9 19 2 If the leak is from behind the valve stator the rotor seal may be scratched Rebuild the injection valve see Section 9 22 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 Technical Support for Dionex products for assistance Leaking suppressor Refer to the suppressor manual for troubleshooting procedures
257. ite in samples 147 Noisy baseline 215 Normal edge TTL input control DC 93 Normal pulse TTL input control DC 93 O Offset percentage analog out 86 Offsetting background conductivity 167 Open circuit 267 Operating temperature DP SP 417 Doc 065342 06 12 11 Index 11 Dionex ICS 5000 Operator s Manual Operation Analyzing samples 172 Creating a sequence 173 174 Direct control of modules 171 Filling vials 146 149 Loading samples 178 Overview 172 Sample preparation 147 Starting a sequence 176 177 Organic solvent 77 Oven TC 116 See also Temperature control TC Oven LED TC LED is flashing 116 300 LED is lighted 116 Oven LEDs DC LED is flashing 51 LED is lighted 51 P PAD See Pulsed amperometry Palladium hydrogen PdH reference electrode 79 Replacement procedure 400 Panel tabset 11 Home panel 11 149 151 How to display 157 165 169 255 256 Parameters Chromeleon commands 172 Peak height Reproducibility 69 Peaks Fronting 118 Reversed 86 Tailing 118 222 Periodic maintenance DC 199 DP SP 196 TC 201 pH gradient 77 pH half cell 77 pH limits 145 pH modifier 43 pH reading Adjusting potentials for 77 Always 7 0 271 Cannot be set to 7 0 272 Effect on potentials 77 Monitoring 78 Nonexistent 273 pH Ag AgCl reference electrode 75 77 Long term storage 187 O ring replacement procedure 399 Replacement procedure 392
258. ivity Follow these steps to change the sensitivity setting of the gas or humidity sensor or to turn off a sensor 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Select the TC 4 If you are using Chromeleon 7 Click the Parameters tab page for the TC click the GasLeakSensor or HumidityLeakSensor parameter Select the new sensitivity setting or select Off to disable the sensor 5 If you are using Chromeleon 6 8 click the plus sign beside TC to display the items underneath Under TC_Temp select the GasLeakSensor or 126 Doc 065342 06 12 11 2 TC Description HumidityLeakSensor parameter Select the new sensitivity setting or select Off to disable the sensor and click Execute 2 26 TC 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 the ambient temperature changes during the analysis increased heating or cooling ensures that the column temperature remains constant O
259. k gas separator waste tube P N 045460 in an uncapped waste container Connect the Waste Gas Separator line to the waste tube NE FERMEZ PAS LE CONTENEUR DE GAZ RESIDUEL Le Dionex ICS 5000 Eluent Generator EG le Atlas Electrolytic Suppressor et le Self Marma 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 a gaz r siduel diam tre int rieur 1 3 cm n de commande 045460 a 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 Dionex ICS 5000 Eluent Generator EG Atlas Electrolytic Suppressor und Self Regenerating Suppressor SRS verwenden einen Elektrolyseprozess VORSICHT 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 conti
260. k ieee ela teak 382 9 27 4 Removing Trapped Air from the Conductivity Cell 383 9 28 ED Service Procedures LL 385 xii Doc 065342 06 12 11 Contents 9 28 1 Disconnecting the ED Cell 00 00 04 385 9 28 2 Replacing an ED Cell Disposable Working Electrode Gasket ese arta ied sea ele la ER Wiehe So A eRe Lo 386 9 28 3 Replacing an ED Cell Conventional Working Electrode Gasket eusta e i seh Dee RE Lp Ee antes 386 9 28 4 Polishing an ED Cell Conventional Working Electrode 389 9 28 5 Replacing a pH Ag AgCl Reference Electrode 392 9 28 6 Calibrating the pH Ag AgCI Reference Electrode 394 9 28 7 Replacing the pH Ag AgCl Reference Electrode O Ring 399 9 28 8 Replacing a PdH Reference Electrode 400 9 28 9 Replacing an ED Detector 404 TO SOMViICE a 320 tae Fo LIA A DL 407 9 29 Replacing Tubing and Fittings LL 407 9 30 Setting Up the Column ID System 408 9 31 Rebuilding an Injection Valve 0 0 0 0 eee eee 410 9 32 Replacing an Injection Valve Pod 2 00 0 411 9 33 Changing the Main Power Fuses 00000 e eee 413 A Specifications DP SP Specifications 415 EG Specifications raea 419 DG Specifications piscia iaia 423 TC Specifications i 433 Doc 065342 06 12 11 xiii Dionex ICS 5000 Operator s Manual B Reordering Information
261. kflow Wizard opens Complete the steps in the wizard For details about an eWorkflow Wizard page click the Help icon Doc 065342 06 12 11 173 Dionex ICS 5000 Operator s Manual 5 2 2 4 After you finish the eWorkflow Wizard the sequence is displayed in the Console Data view see Figure 5 3 Anions New gt stat f Siics so00 gt ate H i al Save Studio Print gt e Insert Row ni Fill Down 2 Filtering On Grouping On E Up 4 Pump_1_Pressur gt Name Type Positio Volume InstrumentMeth Processi Stat 1 None 3 Injection 1 Unknown 1 20 0 AS124 Product AS124 Idle 2 None if Injection 2 Unknown 2 20 0 AS12A Product AS124 Idle None ia Injection 3 Unknown 3 20 0 AS124 Product AS124 Idle 4 None 3 Injection 4 Unknown 4 20 0 AS124 Product AS124 Idle 5 None a Injection Unknown 5 20 0 AS12A Product AS12A Idle go CALA Per if Injection Ga a Unknown 6 rs ere RR ASIZA Product ASTZA Idle Figure 5 3 New Sequence in Chromeleon 7 Using the Sequence Wizard 1 2 On the Console menu bar click the Create button The Sequence Wizard opens Complete the steps in the wizard specifying the number of samples and standards that you want and the instrument method processing method and report template to use For details about a wizard page click the Help icon NOTE If preferred you can create the sequence first and t
262. l sample loop volumes Excess sample will exit through the injection valve waste line Leave the syringe in the port This prevents the sample from exiting the loop before injection Switch the injection valve to the Inject position 5 3 3 Loading Samples with a Vacuum Syringe Pull Method 1 Verify that a luer adapter fitting is installed on the sample loading port on the front of the DC and that tubing is connecting the sample loading port and the injection valve If this is not the case refer to Section 9 20 for connection instructions Disconnect the waste line from the injection valve and replace it with a 25 to 30 cm 10 to 12 in piece of PEEK or PTFE tubing see Figure 5 8 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 Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset or by 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 see Figure 5 8 and pull out the plunger to draw the sample into the injection valve Doc 065342 06 12 11 179 Dionex ICS 5000 Operator s Manual 5 4 6 Switch the injection valve to the Inject position Figure 5 8 Loading Sample with a Vacuum Syringe Pull Method Autosampler Commands for Loading and Injecting Samples Commands for loading and injecting a sample
263. lace Close the EG door 354 Doc 065342 06 12 11 Analytical Analytical 9 EG Service 9 16 9 17 Replacing the RFIC Eluent Degasser 1 Turnoff the pump flow 2 Open the front door of the EG 3 Push down on the slide release latch and pull the tray forward until it reaches the stop 4 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 5 Disconnect the four lines connected to the RFIC Eluent Degasser fittings ELUENT OUT REGEN OUT REGEN IN and ELUENT IN 6 Connect the four lines that were disconnected in Step 5 to the new RFIC Eluent Degasser P N 062137 7 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 8 Push the tray into the module until it locks into place Close the EG door Installing a Backpressure Coil In an analytical IC system the EGC 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 backpre
264. lace the outlet frit as instructed in the EGC manual The manual is included on the Thermo Scientific Reference Library DVD P N 053891 3 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 14 Replacing the EGC Replace the EGC when the cartridge is expended or when it leaks Refer to Table 2 2 for a list of the EGC models that can be used with the Dionex ICS 5000 Eluent Generator Analytical IC systems require EGC III cartridges Previous versions of EGC lc are not compatible with the Dionex ICS 5000 Eluent Generator The EGC replacement procedure consists of e Removing the old EGC see Section 9 14 1 e Disposing of the old EGC see Section 9 14 2 e Installing and conditioning a new capillary EGC see Section 9 14 4 or e Installing and conditioning a new analytical EGC see Section 9 14 5 The EGC contains one of the following a corrosive base KOH LiOH or NaOH a corrosive acid MSA or a concentrated K2CO3 solution Wear protective eyewear and gloves when handling the cartridge CAUTION 336 Doc 065342 06 12 11 9 EG Service MISE EN GARDE VORSICHT La cartouche d EGC contient un de ce qui suit une base corrosive KOH LiOH ou NaOH un acide corrosif MSA ou une solution concentr e de K2CO3 Porter des lunettes e
265. lary or Analytical 063342 Waste and Drain Lines e One waste line is connected to the secondary pump head on each pump and is routed through the tubing chace to the rear of the DP SP e The drain port removes any liquid that collects in the drip tray in the bottom of the DP SP A clear corrugated drain hose P N 055075 is connected to this port during installation Place the free ends of the waste lines and drain hose into a waste container To maintain a positive siphon position the waste container below the level of the pump For correct drainage make sure the waste lines and drain hose are not bent pinched or elevated at any point Do not allow the ends of the lines to be submerged in waste liquid Doc 065342 06 12 11 33 Dionex ICS 5000 Operator s Manual 2 5 Eluent Reservoirs The following reservoirs are available for use with the DP SP e 1 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 plastic reservoirs for offline vacuum degassing of eluents The reservoirs were not designed for this purpose CAUTION N utilisez pas le r servoir en plastique pour le d gazage a vide hors ligne d luants Le r servoir n a pas t congu a cette fin MISE EN GARDE Verwenden Sie keine Plastikbehalter zum Offline Vakkum Entgasen von Eluenten Die Behalter sind dafir nicht ausgelegt VORSICHT 2 5 1 EO Optional Th
266. lectrode 442 Doc 065342 06 12 11 B DC Reordering Information Part Number Item 063722 ED AAA gold working electrode with gasket and polishing kit 060082 Gold AAA Direct disposable working electrodes 6 electrodes with 2 gaskets 060139 Gold carbohydrate disposable working electrodes polyester substrate 6 electrodes with 2 gaskets 066480 Gold carbohydrate disposable working electrodes PTFE substrate 6 electrodes with 2 gaskets 064440 Platinum disposable working electrodes 6 electrodes with 2 gaskets 063003 Silver disposable working electrodes 6 electrodes with 2 gaskets 069336 Carbon disposable working electrodes 6 electrodes with 2 gaskets 060141 Gaskets for disposable working electrodes PTFE 0 002 in 4 gaskets for analytical systems 069339 Gasket for carbon disposable working electrodes ULTEM 0 001 in for analytical systems 072117 Gasket for disposable working electrodes PTFE 0 001 in 2 gaskets for capillary systems 062158 ED cell polypropylene support block for use with disposable electrodes 036313 Polishing kit 036319 Coarse polishing compound 036318 Fine polishing compound 036321 Polishing pads Automation Manager 061738 Dionex ICS 5000 Automation Manager two 10 port high pressure valves two low pressure 3 way valves 061736 Dionex ICS 5000 Automation Manager one 10 port high pressure valve one l
267. lectrode by soaking it in a solution containing 1 M KCl and 1 M HCI 6 4 2 Long term Storage of the pH Ag AgCI Reference Electrode If the cell will not be used for 2 days or more remove the pH Ag AgCl reference electrode and store it in a solution of saturated KCl as instructed in the procedure below 1 Prepare a saturated solution of KCl in ASTM filtered Type I 18 megohm cm deionized water that meets the specifications listed in Section 1 5 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 Ag AgCl reference electrode from the cell 4 Insert the electrode into the cap and screw on the cap see Figure 6 2 Doc 065342 06 12 11 187 Dionex ICS 5000 Operator s Manual 5 Make sure there is no air bubble in the cap Add more KCI solution if needed Storage Call Figure 6 2 pH Ag AgCI Reference Electrode in Storage Cap 188 Doc 065342 06 12 11 fa TC Shutdown 6 5 Consumables Storage The columns and other consumable items used with a Dionex ICS 5000 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 Thermo Scientific Reference Library DVD P N 053891 6 6 Short term Shutdown Before a TC shutdown of less than one week no special procedure is required 6 7 Long term Shutdown Before interrupting TC o
268. lectrode removed from the cell connect the cell and electrode electrical cables to the detector 3 On the Chromeleon 7 ePanel Set click the ED tab on the Chromeleon 6 8 panel tabset click the EC Detector tab 394 Doc 065342 06 12 11 9 DC Service 4 Click the Calibration button The Wellness panel opens see Figure 9 58 EE Electrochemical Detector Wellness pH Electrode Calibration Instructions Place the pH electrode in a pH 7 buffer solution Press the pH 7 Offset Calibration button to calibrate the pH offset Wait until the calibration has finished Place the pH electrode in a pH buffer solution Enter the pH of the buffer in the pH Slope Buffer Value field Press the pH Slope Calibration button to calibration the pH slope Current pH Reading 10 00 Offset Calibration PH Slope Buffer Value 10 00 pH Offset Calibration Slope Calibration pH Slope Calibration Update Wellness Database Instructions In case of a loss of syncronization between the module and the software the calibration values may need to be downloaded to a module You can choose to download the factory previous or current version to the device Settings to Download Current v Current and Previous Values Current pH Electrode Offset Current pH Electrode Slope Current Calibration Date Previous pH Electrode Offset Previous pH Electrode Slope Previous Calibration Date Service Wellness DOOR 0 00
269. leon 7 Instrument Controller Service 149 4 4 2 Starting the Chromeleon 7 Client 149 4 5 Starting Chromeleon 6 8 150 4 5 1 Starting the Chromeleon 6 8 Server 150 4 5 2 Starting the Chromeleon 6 8 Client 151 DP SP Startup i 153 4 6 Setting Up the Eluent Reservoirs 0 0 0 0 ee eee 153 4 7 Setting Up the Piston Seal Wash System 154 4 8 Starting the Pump 157 EG Start p cerr het epics eevee nes a E a A AEN 161 4 9 Entering the Eluent Concentration nanana 161 4 10 Selecting an Eluent Concentration 0 0 0 0 000 162 DG Start P i643 oh seeds eee bP EO as 165 4 11 Starting the DC sui nia Vialli a MAM ee taal 165 4 12 Equilibrating the System and Verifying Operational Readiness 166 TO StartUb c oicrsiazilaa di ae esi eee ee 169 4 13 Starting the TO a ina alii ia ciali ci iii 169 4 14 Equilibrating the System and Verifying Operational Readiness 170 Doc 065342 06 12 11 Vv Dionex ICS 5000 Operator s Manual 5 Operation 5 1 5 2 5 3 5 4 Controlling Modules Directly 0 0 0 0 ee eee 171 Analyzing Samples LL 172 5 2 1 Creating a New Sequence in Chromeleon 7 173 5 2 2 Creating a New Sequence in Chromeleon 6 8 174 5 2 3 Starting a Sequence 176 Loading Samples Into the Sample Loop or Concentrator 178 5 3 1 Loading Samples with a
270. leshooting 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 A Next qualification of this module is overdue due date was date Module may no longer be used Chromeleon monitors the date on which qualification was last performed and displays 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 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 Technical Support for Dionex products 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 monitors the date on which service was last performed and 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 nu
271. lot 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 58 The x axis is the retention time min and the y axis is the waveform period ms The z axis which is represented by different colors in the plot is the response nA om 1025 10 50 1075 1100 1125 Figure 2 58 3D Amperometry Data in Chromeleon 6 8 Iso View NOTE The 3D data shown in Figures 2 58 and 2 59 were collected using an analytical waveform see Analytical vs Scanning Waveforms on page 108 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 of responses as well as the colors representing different magnitudes of detection signal along the z axis 112 Doc 065342 06 12 11 2 DC Description see Figure 2 59 For this view imagine you are standing in front and slightly to the left of the plot lt q c A c e 2 a as os 1038 10 50 O75 1100 1128 1150 1138 1200 1225 1220 1276 1200 19 28 na 12 76 Figure 2 59 3D Amperometry Data in Chromeleon 6 8 3D View Baseline Correction Based on the peak recognition algorithm or by peaks obtained with a user drawn base
272. lp for details Click Next gt and select the in a new sequence via Sequence Wizard option Click Next gt to go to the Sequence Wizard Complete the steps in the Sequence Wizard specifying the number of samples and standards that you want 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 displayed in the Chromeleon 6 8 Browser A program and quantification method appropriate for the selected application are copied to the sequence 5 2 3 Starting a Sequence Starting a Sequence in Chromeleon 7 1 Click Start on the sequence control bar see Figure 5 5 Anions New 5 icss000 Idle E ld Save Studio Gj Print Insert Row 8 Fil Down NZ Filtering On Grouping On B Up gt Pump_1_Pressurb Name Type Positio Volume Instrument Meth Processi Stat 1 None if Injection 1 Unknown 1 20 0 AS12A Product AS12A Idle 2 None Ha Injection 2 Unknown 2 20 0 ASIZA Product AS124 Idle 3 None in Injection 3 Unknown 3 20 0 ASIZA Product AS124 Idle 4 None if Iniection 4 Unknown 4 20 0 AS124 Product AS124 Idle 5 None if Iniection5 Unknown 5 20 0 ASIZA Product AS12A Idle ERNIS auaa lad ESE S a a LAM atta andre 20 0 ASIZA Product ATA i Figure 5 5 Starting a New Sequence in Chromeleon 7 176 Doc 065342 06 12 11 5 Operation 2 The sequence is appended to
273. lsed amperometric detection PAD and integrated pulsed amperometric detection IPAD see Section 2 19 2 e Cyclic voltammetry see Section 2 19 3 Electrochemical Detector Cell The ED cell includes three different electrodes It is a miniature flow through amperometric detection cell with a titanium cell body the counter electrode a working electrode and a combination pH Ag AgCl reference electrode see Figure 2 30 or a PdH reference electrode 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 Five disposable working electrode types are available gold on two different substrates polyester or PTFE silver platinum and carbon Doc 065342 06 12 11 75 Dionex ICS 5000 Operator s Manual The ED cell can be used in either capillary IC or analytical IC systems When used in a capillary IC system the inlet tubing is made of PEEK When used in an analytical IC system the inlet tubing is made of titanium see Figure 2 30 Working Electrode Cell Body counter electrode pH Ag AgCl Reference Electrode Titanium Inlet Tubing for analytical IC Figure 2 30 ED Cell with pH Ag AgCI Reference Electrode Cell Configured for Analytical IC Shown Cell Design The ED cell is a thin layer design Eluent flows in a thin channel parallel to the surface of a flat disk electrode The resultin
274. lso access the Audit Trail from here Home CD Left Sampler Pump EluentGenerator DC Audit Startup Queue Instrument_3 Injection Number Fina Sequence Method 10005 2 cl 750 HS CD_1_Total Q sagh Pump Top mor Srl ooo od 0 000 ml min MA j O psi 2504 Pump Bottom s004 Bor Fme 4 ooo 7504 J min 0 000 ml min MA 1000 0 00 1 25 2 50 3 75 5 00 6 25 7 50 8 75 10 00 O psi 4 DP o it si t _ Yy EGC Left EGC Right SO Si Injection State Of Or ezans SOIA i Cel emer 35 0000 AT EGCKOH EGCKOH Vial Position RAT Suppressor Left on ns Injection Type PushFull x Left Valve Reaction Coil Heater Right Valve 0 00 mM 0 00mM PS L 35 00 r 35 0 3 Sam A Injection Volume 100 0 le anne fer hm 3 Column 4 Si Pa 30 00 Cer 20 00 Ca W Of J oi AS AP LoadPosition LoadPosition EG _ _ Figure 4 3 Example Chromeleon 7 ePanel Set 4 5 Starting Chromeleon 6 8 4 5 1 Starting the Chromeleon 6 8 Server To start the Chromeleon 6 8 Server right click the Chromeleon Server Monitor icon which is crossed out in red on the Windows taskbar and click Start Server The icon changes to gold to indicate that the Chromeleon Server is starting When the Chromeleon Server is running idle the icon changes to gray Sa If the Server Monitor icon i
275. lve see Figure 9 76 and remove the ring 5 Grasp the front of the valve pod and pull out firmly to remove it from the TC Figure 9 76 Unscrewing the Locking Ring 6 Check that the new pod 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 77 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 412 Doc 065342 06 12 11 9 TC Service 8 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 9 77 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Figure 9 77 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 29 12 Close the TC door 9 33 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 Doc 065342 06 12 11 413 Dionex I
276. lve in IC Cube Shown 6 Grasp the front of the valve pod and pull out firmly to remove it from the DC or AM 7 Align the slots in the new pod with the runner in the valve holder on the DC or AM see Figure 9 36 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 368 Doc 065342 06 12 11 9 DC Service 8 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 9 36 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder _ Figure 9 36 High Pressure 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 For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 12 Close the door 9 24 Installing or Replacing an I O Option Board 1 Press the POWER button on the front of the DC for 2 seconds to turn off the power 2 Turnoff the main power switch on the DC rear panel see Figure 2 31 Doc 065342 06 12 11 369 Dionex ICS 5000 Operator s Manual 3 Disconnect the main power cord from both its
277. lyethylene tubing 1 8 in fitting bolt Tan 052267 The suppressor REGEN OUT 1 8 in ferrule Yellow 048949 port and the eluent reservoirs 10 32 fitting bolt Black 043275 All other tubing connections 10 32 ferrule double Tan 043276 cone Table 9 4 Tubing and Fittings for an Analytical IC EG Channel WN Notes for analytical IC channels IC For ferrule fitting tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 For an analytical IC channel 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 072011 Refer to the instructions provided with the cutter Doc 065342 06 12 11 335 Dionex ICS 5000 Operator s Manual 9 13 Isolating a Restriction in the Liquid Lines A restriction in the liquid plumbing will cause excessive system backpressure 1 Begin pumping eluent through the system including the columns 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 EGC is the source of the high backpressure rep
278. m 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 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 a aucune des pi ces m talliques a 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 hlt 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 Help for details e Monitoring of the total cooling and heating workload performed by the compartment and the total operating hours since initial operation e Monitoring of the injection valve usage e Reminders for service and qualification periods including display of warning messages when limits are approaching or overdue Predictive Perf
279. m the EGC vent opening during installation Install the plug into the vent opening 6 Lift the EGC straight up and off the cartridge holder 7 Turn the EGC upside down and place it on the EG drip tray see Figure 9 17 This is the service position for the cartridge Drip Tray Figure 9 17 EGC in the Service Position Analytical Version Shown 8 Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the EGC 338 Doc 065342 06 12 11 9 EG Service 9 14 2 Disposing of the Old EGC If the EGC is expended follow these steps to dispose of it 1 Hold the cartridge with the eluent generation chamber on top 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 EGC for the chemical description 2 Rinse the electrolyte reservoir and membranes three times with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Rinsing should render the reservoir and membranes nonhazardous however check your local state and federal regulatory agency regulations for proper disposal 9 14 3 Storing an Old EGC If the EGC is not expended follow these steps to prepare the cartridge for storage 1 Plug all fittings Tighten the vent fitting capillary EGC or cap the vent
280. mand during data Warning page 276 acquisition Can t find download image TC3000 HEX Abort page 276 Can t start acquisition at negative retention Error page 277 times Can t start acquisition The server configuration Abort page 277 does not fulfill the license conditions Can t start TC firmware A firmware download Abort page 277 may be necessary Can t use device x as a source of the column Error page 278 pressure Please check the property SystemPressure for a valid device name The device must have the Pressure property available Table 8 4 TC Error Messages Doc 065342 06 12 11 209 Dionex ICS 5000 Operator s Manual TC Related Audit Trail Error Message Default Severity Level Can t use device x as a source of the column Error page 278 pressure Please check the property y for a valid device name The device must have the Pressure property available Card data checksum error Error page 279 Command is not available in demo mode Abort page 279 Communication error x Abort page 279 Communication time out Abort page 280 Configuration doesn t match X not installed Warning page 280 Configuration mismatch x CM uses y Abort page 280 Column Compartment uses z Please use the Server Configuration program to check the installation Current flow is out of limits defined for the Warning page 280 column C
281. manual is on the Thermo Scientific Reference Library DVD 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 Doc 065342 06 12 11 407 Dionex ICS 5000 Operator s Manual 9 30 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 includes five chip cards These are the main steps required to implement the column ID system e Specify the column you want to monitor e Installa 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 Start the Chromeleon 7 Instrument Configuration program or the Chromeleon 6 8 Server Configuration program 2 Under the instrument or 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 72 Dionex TC Thermal Compartment General Components Configuration Relays Inputs Error Levels Installed components Left Valve I controlled by AS Right Valve fopots x controlled by AS M Column A Column _A N ICS 3000 v I Column B on 5 300 gt I Column C r on I Column D olu on x Figure 9 72 TC Properties Dialog Box Components
282. mber of days before the due date that the warning is first displayed To troubleshoot Contact Technical Support for Dionex products for information about performing annual preventive maintenance Doc 065342 06 12 11 287 Dionex ICS 5000 Operator s Manual 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 30 Or if you do not want to store information about this column follow the steps below to disable this option 1 In the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 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 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 Technical Support for Dionex products for assistance 288 Doc 065342 06 12 11 8 TC Troubleshooting Operating columns above 70 C could affect column performance
283. med into memory To troubleshoot Flash memory cannot be serviced by the user Contact Technical Support for Dionex products 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 requests confirmation before executing the command To troubleshoot If you want to execute this command click Execute otherwise click Cancel 284 Doc 065342 06 12 11 8 TC Troubleshooting A Firmware download in progress Please wait This error occurs if you attempt to issue a command while firmware 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 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 Ifyou are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation A Humidity leak detected This error occurs i
284. method or Chromeleon 6 8 program is running 2 17 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 Doc 065342 06 12 11 89 Dionex ICS 5000 Operator s Manual e ED detectors 1 and 2 on off e CD ED detectors 1 and 2 auto offset e CD ED detectors 1 and 2 mark e Suppressors 1 and 2 on off e Reaction coil heater on off e A C relays 1 and 2 open closed Assigning TTL Input Functions TTL input control functions are assigned in the Chromeleon 7 Instrument Configuration program or the Chromeleon 6 8 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 1 is assigned 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 Open the Chromeleon 7 Instrument Configuration program or Chromeleon 6 8 Server Configuration program 2 Double click the DC icon under the instrument or timebase 90 Doc 065342 06 12 11 2 DC Description 3 Select the TTL In
285. mixer P N 061686 4 mm P N 063443 2 mm EGC III KOH 074532 Generates potassium hydroxide eluent for anion exchange separations EGC III LiOH 074534 Generates lithium hydroxide eluent for anion exchange separations EGC III MSA 074535 Generates methanesulfonic acid eluent for cation exchange separations EGC III NaOH 074533 Generates sodium hydroxide eluent for anion exchange separations Table 2 2 Capillary and Analytical EGCs Doc 065342 06 12 11 41 Dionex ICS 5000 Operator s Manual For more information refer to the EGC manual The manual is included on the Thermo Scientific Reference Library DVD P N 053891 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 The following versions of the CR TC can be used with the EG CR TC Version IC System Part Type Number Continuously Regenerated Anion Trap Column Capillary 072078 Capillary CR ATC Capillary Continuously Regenerated Cation Trap Column Capillary 072079 Capillary CR CTC Capillary Continuously Regenerated Anion Trap Column Analytical 060477 CR ATC Continuously Regenerated Cation Trap Column Analytical 060478 CR CTC Il Figure 2 11 Capillary and Analytical CR TCs
286. mment KyCO3 EPM 0 1 to 15 mM at 0 1 to 1 0 ml min The total of the eluent Electrolytic pH flow concentrations from Modifier 0 1 to X mM at 1 0 to 2 0 ml min both cartridges flow KyCO3 and EPM where X 15 flow 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 The eluent KOH MSA flow concentration range KOH NaOH 0 1 to X mM at 1 0 to 3 0 mL min for each cartridge is MSA MSA flow 50 of the range for MSA NaOH where X 50 flow an independent NaOH NaOH cartridge LiOH LIOH 0 1 to 40 mM at 0 1 to 1 0 mL min The eluent flow 0 1 to X mM at 1 0 to 3 0 mL min flow where X 40 flow concentration range for each cartridge is 50 of the range for an single independent cartridge KOH Capillary MSA Capillary 0 1 to 100 mM at 0 001 to 0 01 mL min 0 1 to X mM at 0 01 to 0 1mL min where X 1 flow The eluent concentration range for each cartridge is 50 of the range for an independent cartridge Table 4 3 Eluent Concentration Ranges for Linked Dual Cartridge Configurations Doc 065342 06 12 11 163 Dionex ICS 5000 Operator s Manual Notes for Generating Carbonate Bicarbonate Eluent If an EGC II KCO and an EPM III Electrolytic pH Modifier are installed EGC_1 and EGC_2 respectively 1 Set EGC_1 Target Concentration to the concentration of KCO required for yo
287. mperature Zone Model Independent Temperature Control of Each Zone Upper Zone Temperature Range 10 40 C minimum temperature ambient 20 C maximum temperature ambient 20 C Lower Zone Temperature Range 10 70 C minimum temperature ambient 15 C maximum temperature ambient 50 C Temperature Accuracy 0 5 C Temperature Stability 0 2 C Temperature Precision 0 2 C Lower Zone Analytical Injection Valves Up to two 6 or 10 port valves upgradeable field installable Up to two column sets 1 9 mm diameter Maximum Column Length 250 mm plus 50 mm guard column Precolumn Heat Exchangers two 2 mm or 4 mm column ID version Automation Manager Optional Analytical Only Injection Valves Up to two high pressure valves either 6 or 10 port 2 position Low Pressure Valves Up to two inert 2 or 3 way Reaction Coil Heater RCH Holds two reaction coils RCH Temperature Range 5 C above upper zone 80 C maximum AutoPrep Kit Dual loop with sample pre concentration All valves and heater upgradeable and field installable Capillary IC Cube Optional but required for capillary chemistries One or two IC Cube modules hold the following Injection Valves Up to two one per cube high pressure valves 4 port 2 position EG Degasser Column and Guard Carbonate Removal Device Capillary Suppressor See Suppressor section IC Cubes and cartridges are customer
288. mple mixture is pumped first through a temperature stabilizer analytical IC only through the guard and separator columns and then through the suppressor e From the suppressor the mixture flows through a CRD if installed to the cell where the analytes are detected A digital signal is sent to Chromeleon 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 Doc 065342 06 12 11 73 Dionex ICS 5000 Operator s Manual chamber Flow is again routed through the CRD if installed and then to waste Figure 2 29 illustrates the flow path through an EG and a DC for a conductivity detection application using suppression in recycle mode DI WATER IN FROM PUMP COND CELL For anion suppression only CRD MA 13 CR TC WASTE REGEN IN EG pecas 7 SEPARATOR COLUMN GUARD 6 10 SUPPRESSOR SAMPLE TEMP Eluent Flow IE STABILIZER Regenerant Flow For analytical IC only ELUENT IN tes Position WASTE Figure 2 29 EG and DC Flow Schematic for Conductivity Detection Suppression in Recycle Mode e Deionized water from the pump enters the EGC which generates the eluent Eluent exits the EGC and passes through the CR TC which traps ionic contaminants through the EG degas tubing and then into the injection valve e Aft
289. n 2 6 EG Front Features The status bar on the front of the Dionex ICS 5000 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 8 CONNECTED ALARM e Figure 2 8 EG Status Bar Button LED If the LED Is On Comment Label CONNECTED The EG is connected toa Chromeleon 7 instrument or a Chromeleon 6 8 timebase ALARM An EG related problem has Check the Chromeleon Audit occurred for example the Trail for the cause eluent generator cartridge EGC was disconnected EGC 1 The EGC 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 compartment Doc 065342 06 12 11 37 Dionex ICS 5000 Operator s Manual 2 7 Button LED If the LED Is On Comment Label POWER Use this POWER button for The main power switch is on routine on off control of the the EG rear panel EG When the power is on this LED is lighted To turn off the EG press and hold this POWER button for 2 seconds NOTE The EG status bar LEDs do not flash EG Interio
290. n 043276 cone Table 9 8 Tubing and Fittings for an Analytical IC DC System Notes for analytical IC systems IC e 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 362 Doc 065342 06 12 11 9 DC Service on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 072011 Refer to the instructions provided with the cutter e For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 9 20 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 072011 e One 1 4 28 fitting P N 052230 and ferrule P N 052231 e One 10 32 fitting P N 062980 and ferrule P N 062978 e 0 75 mm 0 030 in ID green PEEK tubing P N 052304 e One luer adapter fitting P N 024305 2 Locate the metal release tab under the sample loading port on the front of the DC see Figure 9 31 Press up on the tab to release the port and pull the port out the front of the DC asr Sa je Rea e a Sample Loadin i SD Ani ei So pai Tre PANI Release Tabs Figure 9 31 DC Sample Loading Ports and Release Tabs 3 Remove the fitting plug from the rear of the port Doc 065342 06 1
291. n Autosampler 178 5 3 2 Loading Samples with a Syringe 178 5 3 3 Loading Samples with a Vacuum Syringe Pull Method 179 Autosampler Commands for Loading and Injecting Samples 180 6 Shutdown DP SP SNULAOWIN ice dba 183 EG SNUtdOwi 5565 50 a ara 185 6 1 Short term Shutdown 0 0 0 cee eee eee eee 185 6 2 Long term Shutdown 0 0 2c ee eee eee 185 DG SHULAOWN 655 1 lai 187 6 3 Consumables Storage 0 cee eee eee 187 64 ED Cell Storage senon odro eee eee 187 6 4 1 Short term Storage of the ED Cell 187 6 4 2 Long term Storage of the pH Ag AgCl Reference Blectrode nr anian shee SEA See ce wee 187 vi Doc 065342 06 12 11 Contents TC SNULAOWN irta 189 6 5 Consumables Storage 0 0 0 0 189 6 6 Short term Shutdown 0 0 cece eee eee eee 189 6 7 Long term Shutdown 0 0 cece eee eee 189 7 Maintenance 7 1 System Maintenance Checklists 0 000000 0 eae 191 7 1 1 Daily Maintenance 0 0 0 eee eee ee 191 7 1 2 Weekly Maintenance 0 0 0 eee eee eee 191 7 1 3 Periodic Maintenance 0 0 0 eee eee eee 192 7 1 4 Annual Maintenance 0 0 0 eee eee 192 DP SP Routine Maintenance 195 7 2 DP SP Daily Maintenance 0 0 eee eee ee 195 7 3 DP SP Weekly Maintenance 0 0 0 0 2 ce eee eee 195 7 4 DP SP
292. n cut degas ELUENT IN 0 062 mm 0 0025 in ID PEEK 61 cm 24 in Tubing assembly Blue 072204 CR TC ELUENT IN to EGC precision cut OUT 0 062 mm 0 0025 in ID PEEK 18 cm 7 in Tubing assembly Black 072224 EG degas REGEN OUT to 0 25 m 0 010 in ID CR TC REGEN IN PEEK 64 cm 25 in Tubing assembly Clear 072225 CR TC REGEN OUT to waste 1 58 mm 0 062 in ID ETFE 2 1 m 7 ft 10 mm 0 39 in ID Colorless 055075 Drip tray drain hose polyethylene High pressure 10 32 Blue 074449 Use high pressure fittings for fitting bolt e Pump outlet to EGC IN e EGC OUT to CR TC ELUENT IN e CR TC ELUENT OUT to EG degas ELUENT IN High pressure 10 32 Blue 074372 Use with high pressure fitting ferrule double cone bolts Table 9 3 Tubing and Fittings for a Capillary IC EG Channel Doc 065342 06 12 11 333 Dionex ICS 5000 Operator s Manual Tubing Fitting Size Color P N Use to connect and Type 10 32 fitting bolt Black 043275 All other tubing connections 10 32 ferrule double 043276 cone Table 9 3 Tubing and Fittings for a Capillary IC EG Channel Eey Notes for capillary IC channels Do not cut the 0 062 mm 0 0025 in ID blue PEEK tubing used for capillary IC connections This tubing must be cut at the factory using a specialized precision cutter This ensures good chromatographic results If you need to replace any tubing of this type order the appropriate
293. n 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 The DC TTL inputs respond to four types of signals ioni sd to accommodate different controlling devices The inverted edge default control type Normal Edge is compatible Normal pulse with the output signals provided by Dionex Inverted pulse modules Normal edge v 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 92 Doc 065342 06 12 11 2 DC Description controlling device and the information below to determine the correct type Select the input control type in the Device Configuration dialog box for each TTL input see Figure 2 38 e Normal Edge In normal edge operation the negative falling Action Off or No Effect A edge of a signal turns on the SENTE function The action of the positive rising Action On 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 the valve to Load and the rising edge switches the valve to Inject Similarly for the detector start stop the falling edge starts the de
294. n 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 8 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 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 pres du module et facilement accessible Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist Tubing Chase The tubing chase routes tubing from the front of the EG through the interior of the module and to the rear panel Suppressor Vent and Drain Lines e The lines exiting the tubing chase white tubing are for connecting the REGEN IN port on the RFIC Eluent Degasser or EPM III Electrolytic pH Modifier to the REGEN OUT port on the suppressor e The gas vent line clear tubing discharges the electrolysis gas H or 0 that is vented from the electrolyte reservoir of the EGC 46 Doc 065342 06 12 11 2 EG Description e The drain port removes any liquid that collects in the drip tray in the bottom of the EG A clear
295. n you finish these connections go to the next section to continue setting up the seal wash system Doc 065342 06 12 11 155 Dionex ICS 5000 Operator s Manual Setting Up the Seal Wash System All pumps 1 Add ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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 Place the cap on the reservoir and tighten fingertight Insert the reservoir into the holder on the component panel Check that the tubing is engaged in the peristaltic pump see Figure 4 6 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 Tubing to Secondary Pump Head Lever Outlet Tubing from Seal Wash Reservoir Figure 4 6 Peristaltic Pump Follow these steps to activate the piston seal wash function a Open the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset b Press the F8 key to open the Commands dialog box c Select the pump name d For Chromeleon 7 click the Properties tab on the right pane of the dialog box For Chromeleon 6 8 scroll through the list of commands and properties under the pump name 156 Doc 065342 06 12 11 4 DP SP Startup e Select the RearSealWashSystem prop
296. ncentration 161 Shutdown procedures 185 Spare parts 439 Specifications 419 Status bar buttons and LEDs 37 System configuration 129 USB connections 45 Waste lines 46 47 Eluent generator cartridges 41 Backpressure requirement 43 141 142 255 256 Conditioning procedure 186 Electrical connections 44 Frit outlet 223 336 Leaks 223 253 254 Replacement procedure 336 349 Selecting the eluent concentration 161 Start up procedures 186 Storage long term 186 Storage short term 185 Eluent Organizer EO 2 6 34 Eluent proportioning valves 25 Eluent reservoirs See Reservoirs eluent Eluent filtering 36 Eluents Aqueous 196 Degassing 25 Filtering 153 Flushing lines after eluent change 218 Monitoring pH 77 Outgassing 383 End line filter See Filter end line EO Regulator Kit 35 ePanel Set 11 149 171 EPM III Electrolytic pH Modifier 41 43 44 252 Equilibration 166 170 Error messages Audit Trail description 203 DC summary 207 DP SP summary 204 EG summary 205 TC summary 209 Error messages DC 259 269 CD cell disconnected 259 CD cell over safe temperature 260 Column open circuit 260 Column over safe temperature 260 266 Index 6 Doc 065342 06 12 11 Index Compartment open circuit 261 Compartment over safe temperature 261 ED cell disconnected 261 264 High pressure valve error 265 Lower leak sensor wet 267 Reaction coil open circuit
297. nd download image TC3000 HEX TC3000 HEX is the version of the TC instrument control firmware file that should be available in the Bin directory of your Chromeleon installation This error occurs if the file is missing To troubleshoot Select Tools gt Instrument Qualification Chromeleon 7 or Qualification gt Chromeleon 6 8 IQ Chromeleon 6 8 to run the Chromeleon IQ and diagnose the problem When you eliminate the source of the error rerun the Setup program 276 Doc 065342 06 12 11 8 TC Troubleshooting 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 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 your local Dionex products representative at Thermo Fisher Scientific to obtain the appropriate software version and license Can t start TC firmware A firmware download may be necessary Or Error finishing download Oor TC Firmware download failed If the TC firmware cannot be started after a firmware download or if Chromeleon is unable to successfully dow
298. nditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory present and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks Doc 065342 06 12 11 A DC Specifications Dionex ICS 5000 Conductivity Detector Specifications Continued GLP Compliance Yes optional Physical Dimensions 6 9 x 16 7 x 9 9 cm 2 7 x 6 5 x 3 9 in h x w x d Weight 400 g 1 6 Ib ICS 5000 ED Electrochemical Detector Specifications Electronics Type Microprocessor controlled digital signal processing Electronic Noise Wet Noise Capillary and Analytical IPAD Au electrode lt 50 pC 10 mM KOH DC Amperometry GC lt 10 pA catecholamine eluent Potential Range 2 0 to 2 0 V in 0 001 V increments Signal Range Digital and Analog Integrated amperometry 50 pC to 200 uC DC amperometry 5 pA to 74 pA Filter 0 10 s response time user settable Control Mode Local or remote control using relay closures or TTL or control using Chromeleon via DC module Cell Body Titanium body with narrow bore PEEK inlet tubing for capillary format titanium inlet tubing for analytical format Compatible with 0 2 0 6 mm ID columns PEEK inlet 2 7 mm ID columns titanium inlet Working Elect
299. nel tabset click the tab for the module 2 Use the controls buttons sliders etc on the panel to issue commands 3 If the function that you want to perform is not available from the panel press the F8 key to open the Commands dialog box You can access all commands available for the system from this dialog box Doc 065342 06 12 11 171 Dionex ICS 5000 Operator s Manual 5 2 Analyzing Samples Figure 5 1 shows the basic steps used to analyze a sample in a chromatography system To analyze a sample with a Dionex ICS 5000 system you add sample injections to a Chromeleon sequence The sequence determines how the group of injections will be analyzed and the order in which they will be run A sequence typically includes the following elements e A predefined list of commands and parameters for controlling Dionex ICS 5000 modules and acquiring sample data called an instrument method in Chromeleon 7 or a program in Chromeleon 6 8 e The chromatographic data acquired for each injection Load the sample 4 Autozero 4 Inject the sample J Start data acquisition 4 Stop data acquisition Evaluate sample data Figure 5 1 Sample Analysis Overview e A predefined set of instructions for evaluating the acquired data called a processing method in Chromeleon 7 or a quantification method in Chromeleon 6 8 e Templates for displaying chromatographic data on the screen and for printing repor
300. ng 0 15 cm 0 060 in ID Note Order 12 in of tubing for replacement of piston seal wash tubing 063518 External Seal Wash Kit Eluent Storage and Delivery 072059 EO without reservoirs 072057 Dionex ICS 5000 Eluent Organizer with 2 2 liter reservoirs 072058 Dionex ICS 5000 Eluent Organizer with 4 2 liter reservoirs 063291 Eluent reservoir plastic 1 liter 062510 Eluent reservoir plastic 2 liter 063292 Eluent reservoir plastic 4 liter 074423 EO Regulator Accessory and Stand 064792 TC VWD PDA Regulator Bracket Kit 074422 Regulator 045987 Filter end line 044105 Filter high pressure inline Miscellaneous 042126 GM 3 Gradient Mixer 049135 GM 4 Gradient Mixer 043276 Ferrule fitting 10 32 double cone 0643275 Fitting bolt 10 32 for double cone ferrule fitting 062511 Ferrule fitting 1 16 in 052230 Fitting bolt 1 16 in 042772 Plug 436 Doc 065342 06 12 11 B Reordering Information Part Number Item 054578 Syringe 10 cc 954773 Fuse IEC 60127 2 slow blow rated at 2 A 250 V 063246 USB cable 1 m 3 ft long 005 9001A Cinch connector 2 pin Maintenance Kits 075038 ICS 5000 Analytical Pump Preventive Maintenance Kit 075039 ICS 5000 Capillary Pump Preventive Maintenance Kit Doc 065342 06 12 11 437 Dionex ICS 5000 Operator s Manual 438 Doc 065342 06 12 11 fa EG Reo
301. ng tabs on the detector Then pull the suppressor toward you 7 Orient the new suppressor with the ELUENT IN and REGEN OUT ports on the bottom see Figure 9 50 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 8 Reconnectthe four liquid lines to the new suppressor 9 Plugin the suppressor cable 10 Close the DC door 11 Turnon the DC power and restart the pump flow 9 27 3 Replacing a CD 1 Stop the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 382 Doc 065342 06 12 11 9 DC Service 3 Open the DC upper door and disconnect the tubing from the CD CELL IN and CELL OUT ports see Figure 9 51 Disconnect tubing Release Lever Figure 9 51 Disconnecting the CD Liquid Lines Capillary CD shown 4 For an analytical CD remove the suppressor from the detector For E instructions refer to Section 9 27 2 5 Press the release lever located below the detector see Figure 9 51 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 6 Note the electrical plug on the back of the detector and the receptacle on the inside of the DC 7 Push the new detector in
302. nged Properties cannot be changed A chip card has Error page 290 not been inserted properly Check the CardState property for all cards and reinsert those indicating BusBlocked Properties cannot be changed if the Error page 290 compartment door is open Properties cannot be changed there is no card Error page 291 in the card reader Raw data file x cannot be created Warning page 291 Raw data file x cannot be created Continuing Warning page 291 with network failure protection Raw data file x cannot be written Warning page 291 Raw data file x cannot be written Continuing Warning page 291 with network failure protection Starting data acquisition manually will overwrite Warning page 292 any data which has been acquired so far TC Firmware download failed Abort page 277 TC is not remote Abort page 282 The command can format only chip cards with Error page 292 an invalid data structure The communication interface is closed Error page 292 Reconnect the instrument The compartment door is open a batch or a Warning page 293 program may need to wait until the door has been closed Please close the door Table 8 4 TC Error Messages Continued 212 Doc 065342 06 12 11 8 Troubleshooting TC Related Audit Trail Error Message Default Severity Level The counter name value x has exceeded its Warning page 293 limit y Module should no longer be used Replace the name
303. nload 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 power 2 Download new firmware to the TC as follows a Insert the CD containing the new firmware version into the CD drive Doc 065342 06 12 11 277 Dionex ICS 5000 Operator s Manual b Start the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program c In the instrument or 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 If the error occurs again contact Technical Support for Dionex products for assistance The firmware cannot be serviced by the user Can t use device x as a source of the column pressure Please check the property SystemPressure for a valid device name The device must have the Pressure property available Or A 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 th
304. not be created Or A Raw data file x cannot be created Continuing with network failure protection or A Raw data file x cannot be written Or A 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 Doc 065342 06 12 11 291 Dionex ICS 5000 Operator s Manual 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 error occurs if there is a communication failure between the TC and the PC on which Chromeleon is installed To troubleshoot 1 Check the USB connections 2 Check the connection from the TC
305. ns fingertight and then tighten an additional one quarter turn only 5 Push the component mounting panel back into the enclosure Close the DP SP door 6 Press the POWER button on the front of the DP SP to turn on the pump 7 Reconnect the pump to the software by clicking Connected on the Pump panel 8 Turn on the pump flow 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 8 1 e Reinstalling a new piston see Section 9 8 2 e Reinstalling the pump head see Section 9 8 3 NOTE Capillary IC pumps and analytical IC pumps use different pistons Before continuing verify that you have the correct piston for your pump type P N 068646 for capillary P N 062082 for analytical Doc 065342 06 12 11 323 Dionex ICS 5000 Operator s Manual 9 8 1 Before beginning locate the 3 0 mm hex key P N 062338 in your pump ship kit Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 063342 Additional items e Cleanroom gloves lint free particle free and oil free e ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications
306. ntilation 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 TC Temperature Stabilizer Not Operating Properly Temperature stabilizer installed incorrectly Remove the temperature stabilizer and install it correctly Make sure there is good thermal contact between the temperature stabilizer and the thermal element For detailed instructions refer to Thermo Scientific Dionex ICS 5000 Ion Chromatography System Installation Instructions Document No 065343 TC calibration is incorrect The TC cannot be calibrated by the user Contact Technical Support for Dionex products for assistance Defective temperature stabilizer Replace the temperature stabilizer standard bore P N 064548 microbore P N 064650 Doc 065342 06 12 11 301 Dionex ICS 5000 Operator s Manual 302 Doc 065342 06 12 11 9 e Service This chapter describes Thermo Scientific Dionex ICS 5000 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 Thermo Fisher Scientific personnel For assistance contact Technical Support for Dionex products In the U S and Canada call 1 800 346 6390 Outside the U S and Canada call the nearest Thermo Fisher Scientifi
307. ntrol electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components cannot be serviced by the user CR TC1 stopped because EGC1 OFF or CR TC2 stopped because EGC1 OFF This error occurs if you attempt to turn on the CR TC when the EGC is turned off The CR TC current is automatically turned off to prevent damage to the CR TC To troubleshoot Verify that the pump flow and the EGC are on before turning on the CR TC 242 Doc 065342 06 12 11 8 EG Troubleshooting CR TC1 stopped due to zero flow Or CR TC2 stopped due to zero flow This error occurs if you turn off the pump flow while the EGC current and CR TC are on The CR TC current is automatically turned off to prevent damage to the CR TC To troubleshoot If the pump stopped unexpectedly follow the troubleshooting steps in Section 8 23 The CR TC mode is off for a virtual pump This error occurs when a live EG is linked to a virtual pump and you try to turn on the CR TC The mode is automatically turned off to ensure that the EG does not operate when there is no flow CR TC mode will be turned off for invalid flow Flow range for analytical EGC 0 100 3 000 mL min capillary EGC 0 001 0 100 mL min This error occurs when the flow to the CR TC is out of range or there is no pumped linked to the EGC To troubleshoot 1 Set the flow rate to a v
308. nts of sample to an injection valve In addition to the normal mode the autosampler can operate in several other modes including concentrate simultaneous and sequential injections Dionex 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 Doc 065342 06 12 11 9 Dionex ICS 5000 Operator s Manual chromatograms at individual wavelengths instead of from spectra offers two advantages it eliminates the need to perform extractions for chromatograms that do not require spectral data and it conserves disk space Dionex 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
309. nue to generate eluent at the concentration set for the last step of the last Chromeleon 7 instrument method or Chromeleon 6 8 program If this occurs the eluent concentration will increase in proportion to the decrease in the flow rate In extreme cases excessive heat buildup can occur and damage the EGC For a complete list of operating precautions for EGCs and CR TC trap columns refer to the product manuals The manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 142 Doc 065342 06 12 11 4 Startup 4 1 2 ED Cell Operating Precautions To maintain good reproducibility of detection results Prepare all eluents with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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 a pH Ag AgcCI 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 all fitting plugs For longer shutdowns see Section 6 4 Be careful to keep the polished surface of the ED 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
310. ny special startup procedures required for the columns suppressors etc Startup procedures are described in the quick start guides and manuals provided on the Thermo Scientific Reference Library DVD P N 053891 4 1 Operating Precautions 4 1 1 EG Operating Precautions In an analytical IC system the EGC requires at least 14 MPa 2000 psi of ls 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 panel in Chromeleon 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 EGC For instructions refer to Section 9 17 IMPORTANT The recommended maximum operating pressure for the EG in an analytical IC system is 21 MPa 3000 psi Excessive backpressure may rupture the tubing inside the RFIC Eluent Degasser Doc 065342 06 12 11 141 Dionex ICS 5000 Operator s Manual DO NOT CAP THE WASTE CONTAINER The Dionex ICS 5000 Eluent Generator EG Atlas Electrolytic Suppressor and Self Regenerating Suppressor SRS use an electrolytic process that results in the CAUTION 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 blac
311. o pull the panel forward until it reaches the stop Doc 065342 06 12 11 317 Dionex ICS 5000 Operator s Manual 6 To prevent contamination of pump parts wear cleanroom gloves while disassembling and reassembling 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 7 Disconnect all tubing connections to the pump head with the defective piston seal 8 The primary and secondary pump heads have different components When disassembling a pump head refer to Figure 9 6 for a primary pump head or Figure 9 7 for a secondary pump head Note Each check valve assembly includes a valve body B anda cartridge C Seal Wash Body P N 074446 Capillary P N 062064 Analytical Piston O Ring Primary Pump Head P N 068646 Capillary P N 040695 P N 074447 Capillary P N 062082 Analytical Capillary and Analytical P N 062083 Analytical Seal Retainer Backup Ring Outlet Check Valve Assembly P N 068627 Capillary P N 074371 P N 044540 Capillary P N 062092 Analytical Capillary only P N 045721 Analytical Piston Seal Wash Seal Main Piston Seal D Inlet Check Valve Assembly P N 068628 Capillary P N 075493 Capillary P N 044541 Capillary P N 063382 Analytical P N 064946 Analytical P N 045722 Analytical Figure 9 6 DP SP Pump Primary Pum
312. o test the pH Ag AgCl reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 274 272 Doc 065342 06 12 11 8 DC Troubleshooting 3 If soaking does not fix the problem replace the electrode see Section 9 28 5 8 28 4 No ED Cell pH Readout or Intermittent Readout The pH reading is displayed on the ED ePanel in Chromeleon 7 or the EC Detector Control panel in Chromeleon 6 8 PdH reference electrode selected Select the AgCl reference electrode mode on the ED ePanel in Chromeleon 7 or the EC Detector Control panel in Chromeleon 6 8 or in the Chromeleon 7 instrument method or the Chromeleon 6 8 program Disconnected reference electrode Verify that the reference electrode cable is securely connected see Figure 8 8 Uncalibrated pH Ag AgCl reference electrode Calibrate the pH Ag AgCl reference electrode see Section 9 28 6 Dry pH Ag AgcCI reference electrode 1 Soak the pH Ag AgCl reference electrode in a solution containing 1 M KCl 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 on page 274 2 If soaking the pH Ag AgCl reference electrode does not fix the problem replace the electrode see Section 9 28 5 To prevent a pH Ag AgCl reference electrode from
313. o troubleshoot Doc 065342 06 12 11 263 Dionex ICS 5000 Operator s Manual Check the buffer selection Verify that the electrode is properly immersed in the calibration buffer Repeat the calibration procedure see Section 9 28 6 If the error recurs repeat the calibration at least one more time If the error recurs after repeating the calibration at least two times replace the Ag AgCl reference electrode see Section 9 28 5 ED pH slope calibration failed This error occurs when the pH sensing glass membrane of the Ag AgCl reference electrode is broken or otherwise affected causing the calibration slope to deviate by more than 10 from the theoretical slope of 59 mV pH unit at 25 C To troubleshoot 1 2 Make sure the calibration temperature is as close as possible to 25 C Verify that the correct buffer is being used and that the electrode is properly immersed in the calibration buffer Repeat the calibration procedure see Section 9 28 6 If the error recurs repeat the calibration at least one more time If the error recurs after repeating the calibration at least two times replace the Ag AgCl reference electrode see Section 9 28 5 ED reference electrode disconnected To troubleshoot Check the cable connection Verify that the signal cable from the working electrode is connected to the detector block see Figure 8 4 264 Doc 065342 06 12 11 8 DC Troubleshooting
314. ocations Refer to Figure 2 32 or the label on the DC rear panel for the connector pin assignments To attach a wire to the plug strip the end of the wire insert it into the plug and use a screwdriver to tighten the locking screw If necessary multiple ground wires can be attached to a single ground pin When attaching wires to the connector plug be careful not to allow stray strands of wire to short to an adjoining position on the connector Plug the connector into the appropriate 12 pin connector on the DC rear panel 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 If you connected a TTL input verify that the correct function is assigned to the input and that the correct input control type is selected Select different settings if necessary Input functions and control types are assigned from the Chromeleon 7 Instrument Configuration program or the Chromeleon 6 8 Server Configuration program see Section 2 17 4 84 Doc 065342 06 12 11 2 DC Description 2 17 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 31 The analog outputs supply a voltage signal proportional to the current me
315. 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 dis abled in Chromeleon When disabled you can control the valve only from the software To enable or disable a button open the Commands dialog box press the F8 key select the Advanced or Expert user level and select the Valve1 Button or Valve2Button property in the list of properties for the DC The front of the DC has two sample loading ports see Figure 2 16 that can be connected to injection valves installed inside the DC A syringe can then be used to manually load sample through the ports For automated sample 52 Doc 065342 06 12 11 2 DC Description injection the DC can be connected to an autosampler For more information about sample injection see Section 5 2 Figure 2 16 DC Sample Loading Ports 2 11 DC Interior Components The interior of the DC consists of two temperature controlled compartments upper and lower To access the upper compartment lift up the top door To access the lower compartment pull down the lower door The upper and lower compartments are isolated from each other in separate temperature zones There is no common air flow between the two compartments For details about DC temperature control see Section 2 12 The compartments can accommodate the components necessary for up to two IC systems T
316. ogram 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 AII samples scheduled for run on timebases x need to specify the same value for property nominal Temperature Or All samples scheduled for run on timebases x need to specify the same value for property TempCtrl Or Doc 065342 06 12 11 275 Dionex ICS 5000 Operator s Manual 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 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 Can t fi
317. olumn e Guard column to separator column e Separator column to suppressor High pressure 10 32 7 074373 Use with high pressure ferrule double cone fitting bolts blue Table 9 7 Contents of the IC Cube Tubing Kit P N 072186 360 Doc 065342 06 12 11 9 DC Service my Notes for Capillary IC systems e The 0 062 mm 0 0025 in ID blue PEEK tubing capillary tubing used for IC Cube connections is cut at the factory using a specialized precision cutter If you need to replace any of this type of tubing order an IC Cube Tubing Kit P N 072186 or the individual tubing listed in Table 9 7 e When replacing capillary tubing make sure the ferrule and fitting bolt are at least 2 mm 0 1 in from the end of the tubing before you insert the tubing into the port Do not position the ferrule and fitting bolt flush with the end of the tubing For detailed connection instructions see Section 9 1 e Except for capillary tubing you can 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 072011 Refer to the instructions provided with the cutter e For tightening requirements for the high pressure fitting bolt P N 074449 and ferrule P N 074373 see Section 9 2 e For tightening requirements for the 10 32 fitting bolt P N 0432
318. omeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Check the status of each property listed in the error message The table below indicates the status required for operation Command Status CardState OK Door Closed Ready Ready Standby NoStandby 4 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 requests confirmation before saving the new property To troubleshoot If you are sure that the proposed change is correct go ahead and save it 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 Doc 065342 06 12 11 295 Dionex ICS 5000 Operator s Manual A The Warning threshold must be higher than the Limit threshold This error occurs if the Warning value selected for a Predictive Performance command for example LeftRotorSealSwitches is lower than the Limit value Chromeleon issues a warning
319. on nect a gas separator waste tube P N 045460 to the suppres sor waste line during installation For details refer to Thermo Scientific Dionex ICS 5000 Ion Chromatography System Installation Instructions Document No 065343 System Flow Schematics for Conductivity Detection Figure 2 28 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 Thermo Scientific Reference Library DVD P N 053891 NOTE The basic flow path is the same for both capillary IC and ana lytical IC systems However in capillary IC systems connec tions to components installed inside IC Cube cartridges columns suppressor and CRD are not visible 72 Doc 065342 06 12 11 2 DC Description COND CELL For anion suppression only optional SUPPRESSOR C SEPARATOR COLUMN TEMP Eluent Flow STABILIZER Regenerant Flow For analytical IC only PUMP or WASTE _ VALVE ELUENT Inject Position ELUENT GENERATOR Figure 2 28 DC Flow Schematic for Conductivity Detection Suppression in Recycle Mode e Eluent from the pump 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 sa
320. on the Thermo Scientific Reference Library DVD P N 053891 EGC Eluent Concentration Range KOH Capillary 0 1 to 200 mM at 0 001 to 0 010 mL min flow 0 1 to X mM at 0 010 to 0 030 mL min where X 2 flow MSA Capillary 0 1 to 200 mM at 0 001 to 0 010 mL min flow 0 1 to X mM at 0 010 to 0 030 mL min where X 2 flow KyCO3 0 1 to 15 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 2 0 mL min flow 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 flow 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 2 Eluent Concentration Ranges for Single Cartridge and Independent Dual Cartridge Configurations 162 Doc 065342 06 12 11 4 EG Startup Linked Dual Cartridge Configuration In the linked dual cartridge configuration the EG contains two EGCs linked to a single pump 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 EGC manual EGC manuals are included on the Thermo Scientific Reference Library DVD P N 053891 EGCs Eluent Concentration Range Co
321. operties 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 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 Help Doc 065342 06 12 11 125 Dionex ICS 5000 Operator s Manual 2 25 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 e The corresponding sensor is activated e The ALARM LED on the front of the TC lights red and remains red as long as the sensor is exposed to gases or humidity e The error is logged in the Chromeleon Audit Trail e A beep sounds What to do when an alarm occurs 1 Find and eliminate the leak 2 Ifyou are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation Adjusting the Sensor Sensit
322. or IC Cube 1 heater over safe temperature Error page 266 IC Cube 2 heater over safe temperature Lower door opened Warning page 267 Lower leak sensor wet Warning page 267 Reaction coil open circuit Abort page 267 Reaction coil over safe temperature Abort page 268 Suppressor over current Abort page 268 Suppressor over power Abort page 268 Suppressor over voltage Abort page 269 Suppressor stopped for flow rate Warning page 269 Upper door opened Warning page 269 Table 8 3 DC Error Messages Continued 208 Doc 065342 06 12 11 8 Troubleshooting 8 1 4 TC Error Messages Table 8 4 lists the TC related error messages and their default severity levels For troubleshooting assistance refer to the page indicated in the table TC Related Audit Trail Error Message Default Severity Level AcqOff without previous AcqOn Error page 275 Acquisition is still on at program end Error page 275 All samples scheduled for run on timebases x Error page 275 need to specify the same value for property nominal Temperature All samples scheduled for run on timebases x Error page 275 need to specify the same value for property TempCtrl All samples scheduled for run on timebases x Error page 276 need to specify the same value for property y Can t execute Disconnect command during Warning page 276 data acquisition Can t execute Standby com
323. ormance commands and parameters are available in the Chromeleon Commands dialog box 128 Doc 065342 06 12 11 3 1 3 Configurations Overview This chapter provides example component and plumbing drawings for the following Dionex ICS 5000 system configurations Dionex ICS 5000 IC System Configuration See Capillary IC Dual RFIC EG System CD CD page 130 Capillary IC Dual RFIC EG System CD ED page 131 Hybrid System Dual RFIC EG System CD Analytical CD page 132 Capillary Analytical IC Single System without EG CD page 133 Analytical IC Single RFIC EG System CD page 134 Analytical IC Dual RFIC EG System CD CD page 135 Analytical IC Dual RFIC EG System CD ED page 136 Analytical IC Single RFIC EG System with Matrix Elimination page 137 Using a DP and a 6 Port Valve Analytical IC Single RFIC EG System with Matrix Elimination page 138 Using an SP and a 10 Port Valve Analytical IC Single RFIC EG System with Post Column page 139 Reagent Addition Bromate Analytical IC Single RFIC EG System with ED and VP for page 140 Carbohydrate Analysis Doc 065342 06 12 11 129 Dionex ICS 5000 Operator s Manual To pui Deionized Water DC front view Pump front view DP Seal a mp 2 inlet via the pump rear chase To pump 1 inlet via the pump rear chase System 2 pump not to scale To waste To EGC D 2 In
324. ow also b EG panel Enter 100 mM in the Target Concentration field This turns on the power to the EGC also c Verify that eluent is exiting the cell d ED panel Set the reference electrode mode to PdH e Select DC amperometry mode set the cell voltage to 0 000 V and turn on the cell voltage Switch to integrated amperometry mode and select the PdH referenced carbohydrate waveform Condition the electrode for 1 hour at these settings Turn off the pump flow This turns off the EGC power and the cell voltage 9 28 9 Replacing an ED Detector 1 Di Turn off the pump flow Press the POWER button on the front of the DC for 2 seconds to turn off the DC Open the DC upper door and disconnect the cell inlet and outlet lines Disconnect the reference electrode cable and the cell cable Grasp the cell body and pull straight out to remove the cell from the detector 404 Doc 065342 06 12 11 9 DC Service 6 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 7 Note the electrical plug on the back of the detector and the receptacle on the inside of the DC 8 Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure 9 Reinstall the cell and reconnect the cell inlet and outlet lines and the cables NOTE If you
325. ow pressure 3 way valve 061740 Dionex ICS 5000 Automation Manager one 6 port high pressure valve one low pressure 3 way valve Doc 065342 06 12 11 443 Dionex ICS 5000 Operator s Manual Part Number Item 061734 Dionex ICS 5000 Automation Manager tray with no valves 061746 RCH 1 Reaction Coil Heater 062561 Temperature stabilizer standard bore 0 25 mm 0 010 in ID 062562 Temperature stabilizer microbore 0 125 mm 0 005 in ID Analog Output Relay TTL 062201 YO option 923686 Connector plug 12 position 043598 Twisted pair of wires Miscellaneous 954772 Fuse IEC 60127 2 slow blow rated at 10 A 250 V 960777 USB cable 1 8 m 6 ft long 062437 Leak sensor 043276 Ferrule fitting 10 32 double cone 043275 Fitting bolt 10 32 for double cone ferrule fitting 044105 Filter high pressure inline Maintenance Kits 075040 0 4 uL Internal Loop High Pressure Valve Preventive Maintenance Kit 075041 6 Port High Pressure Valve Preventive Maintenance Kit 075042 10 Port High Pressure Valve Preventive Maintenance Kit 444 Doc 065342 06 12 11 TC Reordering Information Part Number Item Valves and Accessories 057896 Injection Valve Rebuild Kit for 6 port valve includes valve seal hexagon wrench and instructions 061759 Injection Valve Rebuild Kit for 10 port valve includes valve seal hexagon wrench and instructions
326. own for more than 3 le to 4 days hydrate the suppressor as instructed in the product manual Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 3 Let the system equilibrate 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 Doc 065342 06 12 11 185 Dionex ICS 5000 Operator s Manual 2 Verify that the current to the EGC and the suppressor is off IMPORTANT Supplying power to the EGC when there is no eluent flow can severely damage the cartridge 3 If you plan to store the EGC 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 14 1 to remove the EGC from the EG and the instructions in Section 9 14 3 to store the EGC To restart the EG 1 Select the parameters for the analysis on the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset For EG startup information see Section 4 9 2 Condition the EGC For instructions see Conditioning the Capillary EGC on page 343 or Conditioning the Analytical EGC on page 348 3 Hydrate the CR TC see Installing and Flushing the New CR TC on page 350 4 Hydrate the suppres
327. p Head Assembly 318 Doc 065342 06 12 11 9 DP SP Service Piston PIN 068646 Capillary P N 062082 Analytical Seal Retainer P N 068627 Capillary P N 062092 Analytical Piston Seal Wash Seal P N 068628 Capillary P N 063382 Analytical Seal Wash Body P N 074446 Capillary P N 063968 P N 062064 Analytical Capillary and Analytical Capillary only Main Piston Seal P N 075493 Capillary Assembly P N 062057 P N 064946 Analytical Capillary and Analytical Secondary Pump Head P N 074240 Capillary P N 062079 Analytical Priming Valve Priming Valve Seal P N 063382 Capillary and Analytical Capillary and Analytical Membrane P N 062081 Capillary and Analytical Pressure Transducer Figure 9 7 DP SP Secondary Pump Head Assembly 9 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 10 Remove the seal wash body from the pump head Or if the seal wash body was not removed with the pump head in Step 9 pull it straight out of the pump mechanism now 11 Pull the piston 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 pis ton to one side and then pull it out of the pump mecha nism Doc 065342 06 12 11 319 Dionex ICS 5000
328. p card in reader 288 No response from x 288 Nominal temperature must be set 294 Nominal temperature value out of range 294 Operating columns above 289 Oven not fully operable 294 Parameter x value exceeded 289 Primary column ID property 295 Primary property x already assigned 290 Properties cannot be changed 290 291 Raw data file x cannot be created 291 Raw data file x cannot be written 291 Starting data acquisition manually 292 TC firmware download failed 277 TC is not remote 282 The command can format 292 There was already an AcqOff 296 There was already an AcqOn 296 This function cannot be adjusted 297 This operation may affect 297 Two AcqOn commands for channel 296 Unknown error code 297 Unknown format of card data 297 Upper limit must be higher 295 USB LAN communication error 283 Value for parameter is not within 289 Value x replaced by 289 Warning threshold must be higher 296 Warning threshold must be lower 296 X position error 298 You do not have the privilege 298 eWorkflows 173 External low pressure valves DC 82 External Seal Wash Kit 27 154 436 F Filter end line Bacterial contamination 196 Installation Maintenance 195 Filter inline 36 Fittings DC Replacing 359 Requirements 359 Fittings DP SP Replacing 306 Requirements 306 Fittings EG Repla
329. p only Enter 100 for the channel A B C or D to be primed Set the priming flow rate to the desired rate The default rate for a capillary IC pump is 3 0 mL min The default rate for an analytical IC pump is 6 0 mL min Click the Prime button on the Pump panel A warning message asks you to verify that the purge priming valve is open Click Execute despite warnings Chromeleon 7 or OK Chromeleon 6 8 Priming starts 310 Doc 065342 06 12 11 9 DP SP Service 10 11 Prime the pump until all air is purged and no air bubbles can be seen exiting the waste line Click the Prime button to stop priming NOTE Priming will stop automatically after the number of seconds specified in the Duration box have elapsed You can set the duration to a preferred value Gradient pump only To prime additional eluent lines select another eluent channel and repeat the priming procedure 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 destroy the cap seal Open or close the priming valve only when the system pressure is down Enter the flow rate required for your application Gradient pump only Enter the required proportions of eluents A B C and D on the Pump panel Turn on the pump flow NOTE After starting the pump wait at least 5 minutes longer for flow rates below 1 0 mL min before beginning an analy
330. ped potentials is being applied see the example waveform in Figure 2 51 108 Doc 065342 06 12 11 2 DC Description With scanning waveforms integration occurs while the potential is being increased linearly over time see the example scanning waveform in Figure 2 55 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 19 5 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 E4 1 0 0 0 4 Potential Volts gt E1 1 0 Integration E3 2 5 i I I 0 0 0 5 1 0 1 5 2 0 Time Seconds E1 Pre adsorption potential E2 Scanning period E3 Negative cleaning potential E4 Positive cleaning potential Figure 2 55 Example Scanning Waveform 2 19 5 Storing and Reprocessing Amperometry Data Chromeleon provides storage of 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 56 The retention Doc 065342 06 12 11 109 Dionex ICS 5000 Operator s
331. perating 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 Thermo Scientific Reference Library DVD 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 selected 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 Doc 065342 06 12 11 127 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT 2 26 1 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 ambient Maximu
332. peration for more than one week or before shipping the TC rinse the fluid connections with deionized water Doc 065342 06 12 11 189 Dionex ICS 5000 Operator s Manual 190 Doc 065342 06 12 11 7 Maintenance This section describes routine maintenance procedures for the Dionex ICS 5000 system that users may perform All other maintenance procedures must be performed by Thermo Fisher Scientific personnel For information about maintenance procedures for the EGC CR TC trap column or suppressor refer to the appropriate product manual These manuals are included on the Thermo Scientific Reference Library DVD 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 reservoirs for microbial growth clean reservoirs and replace eluent as needed Mie O Check eluent reservoir levels and refill as needed ema O Check waste containers and empty as needed For detailed daily maintenance instructions for each module see DP SP page 195 EG page 197 DC page 199 TC page 201 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 Doc 065342 06 12 11 191 Dionex ICS 5000 Operator s Manual buildup is evident or if eluent flow is blocked See Section 4 6 for instructions O Check for plugged or blocked tub
333. precision cut tubing assembly listed in Table 9 3 e When replacing capillary tubing make sure the ferrule and fitting bolt are at least 2 mm 0 1 in from the end of the tubing before you insert the tubing into the port Do not position the ferrule and fitting bolt flush with the end of the tubing For detailed connection instructions see Section 9 1 e For tightening requirements for the high pressure fitting bolt P N 074449 and ferrule P N 074373 see Section 9 2 e For tightening requirements for the 10 32 fitting bolt P N 043275 and ferrule P N 043276 refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 334 Doc 065342 06 12 11 9 EG Service 9 12 2 Tubing and Fittings for Analytical IC EG Channels IC Table 9 4 lists the tubing and fittings used to plumb an EG channel for analytical IC Tubing Fitting Size Color P N Used to connect and Type 0 25 mm 0 010 in ID Black 042690 EGC to pump PEEK tubing 1 in e EGC to CR TC RFIC Eluent Degasser to injection valve e RFIC Eluent Degasser to eluent reservoir 1 6 mm 0 062 in ID Colorless 014157 RFIC Eluent Degasser PTFE tubing 1 in REGEN IN to CR TC e RFIC Eluent Degasser REGEN OUT to waste 1 58 mm 0 062 in ID Colorless 047203 EGC gas vent line polyurethane tubing 10 mm 0 39 in ID Colorless 055075 Drip tray drain hose po
334. ptional IC Cube 2 mm and 4mm anion and cation Membrane and MonoDisc suppression bed types available Membrane for capillary 0 4 mm suppressor Electrolytic Suppression Self Regenerating External Water Mode 0 4 mm with optional IC Cube 2 mm and 4mm anion and cation Membrane and MonoDisc suppression bed types available for 2 mm and 4 mm Membrane for capillary 0 4 mm suppressor Salt Converter Available in 2 mm and 4 mm versions AMMS ICE Available in 2 mm and 4 mm versions 424 Doc 065342 06 12 11 A DC Specifications Dionex ICS 5000 DC Detector Chromatography Compartment Specifications Carbonic Acid Removal for Anions ASRS and AMMS plus CRD 300 for 2 mm and 4 mm versions CRD 0 4 mm for capillary suppressors Suppression Capacities Anion SRS 300 4 mm 200 peg min Cation SRS 300 4 mm 110 peg min Anion SRS 300 2 mm 50 ueg min Cation SRS 300 2 mm 37 5 peg min Anion MMS 300 4 mm 150 peg min Cation MMS 300 4 mm 150 peg min Anion MMS 300 2 mm 37 5 peg min Cation MMS 300 2 mm 37 5 peg min Anion AES 25 ueg min Cation AES 25 peg min AMMS ICE N A Anion CES 0 4 mm 2 peg min Cation CES 0 4 mm 1 5 peg min Suppressor Void Volumes SRS 300 4 mm lt 50 uL SRS 300 2 mm lt 15 uL MMS 300 4 mm lt 50 uL MMS 300 2 mm lt 15 uL AMMS ICE 300 4 mm lt 50 uL AMMS ICE 300 2 mm lt 15 uL AES Anion or Cation lt 35
335. puts tab see Figure 2 37 Dionex DC Detector Chromatography General Detectors High Pressure Valves Low Pressure Valves TTLs Relays AC Thermal Controls Suppressors TTL Inputs Error Levels Name Description TTL_Input_1 TTL Input 1 TTL_Input_2 TTL Input 2 TTL_Input_3 TTL Input 3 TTL_Input_4 TTL Input 4 TTL_Input_5 TTL Input 5 TTL_Input_6 TTL Input 6 TTL_Input_ TTL Input 7 Deactivate check boxes to remove unused devices Hit F2 to edit selection or double click it Cancel Appl Help Figure 2 37 DC Server Configuration Properties TTL Inputs 4 Select the name of the input and press the F2 key or double click the name Doc 065342 06 12 11 91 Dionex ICS 5000 Operator s Manual The Device Configuration dialog box for the selected input appears Device Configuration Device Name TTL_Input_1 Mode Normal edge X Control Functions Injiectalve_Left position 4 B MI Injectvalve_Right position A B AM_HP_A position A B AM_HP_B position A B AM_LP_A position open closed AM_LP_B position open closed C DC_LP_A position open closed Deactivate check boxes for unused functions Cancel Figure 2 38 Assign TTL Input Control Functions 5 In the Control Functions list select the check box of one or more functions to be controlled by this input When connected to a controlling device the device ca
336. r 27 Status bar buttons and LEDs 21 System configurations 129 138 USB connections 33 Waste lines 33 Sodium hydroxide eluent 41 Solvent compatibility ED 76 Spare parts DC 441 DP SP 435 EG 439 TC 445 Specifications Conductivity Detector CD 427 DC 423 DP SP 415 EG 419 Electrochemical Detector ED 429 TC 433 Standard bore IC applications 2 Start up procedures DC 165 DP SP 153 EG 161 Equilibrate the system 166 170 Offsetting the background 167 TC 169 Static mixer 219 See also GM 3 Gradient Mixer Status bar DC 51 LEDs described 51 115 Status bar DP SP LEDs described 22 Status bar EG LEDs described 38 Status bar TC LEDs described 115 Sulfite in samples 147 Suppressor Description 71 For analytical IC system 71 For capillary IC system 71 Leaking 270 Reordering 442 Replacement procedure 381 Types supported 62 Suppressor alarms Suppressor over current 268 Suppressor over power 268 Suppressor over voltage 269 Suppressor bypass cartridge for IC Cube 57 Suppressor cartridge for IC Cube 57 Suppressor LEDs DC LED is lighted 51 Switched AC sockets DC 81 Syringe Reordering 441 Syringe injection 178 Vacuum 179 System configuration drawings 129 139 Analytical IC RFIC EG dual CD and ED system 136 Analytical IC RFIC EG dual CD system 135 Analytical IC RFIC EG single system 134 Analytical IC system non RFIC 133 Analytical RFIC EG with post column
337. r Chromeleon 6 8 panel tabset 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 3 Verify that the detector baseline is at the expected reading for your application and is stable The system is now ready for operation 170 Doc 065342 06 12 11 5 1 5 Operation Controlling Modules Directly When the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is not running automated analyses you can directly control the system modules by issuing commands from the ePanel Set in Chromeleon 7 or the panel tabset in Chromeleon 6 8 For example you can turn on the pump flow set the eluent concentration or set the compartment temperature To display the Chromeleon 7 ePanel Set 1 On the Console click the Instruments category bar 2 In the Navigation Pane click the instrument that you want to control Chromeleon 7 connects to the instrument and displays the ePanel Set To display the Chromeleon 6 8 panel tabset 1 Click View gt Default Panel Tabset or click the toolbar button E 2 Select the Chromeleon server and click OK 3 If more than one timebase is configured on the server Chromeleon 6 8 displays a panel tabset for each timebase Click the Expand Timebase View button for the timebase that you want to control To issue direct control commands to a module 1 On the ePanel Set or pa
338. r Components The EG component compartment which is located directly behind the front door accommodates the components required for generating eluent in a single system or in both channels of a dual system A component mounting panel divides the compartment into two sections e The left section is for a single channel EG or for system 1 of a dual channel EG e The right section is for system 2 of a dual channel EG Each section holds the components for either a capillary IC or an analytical IC system A dual channel EG can hold components for two capillary IC systems two analytical IC systems or one system of each type Figure 2 9 shows the component panel for a capillary IC system Figure 2 10 shows the component panel for an analytical IC system 38 Doc 065342 06 12 11 2 EG Description 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 1 EGC Capillary Chase for Electrical Cables CR TC Capillary Leak Sensor Drip Tray Slide Release Latch 0 0 Note For a capillary IC system the eluent degasser is installed in the IC Cube Figure 2 9 Example EG Interior Components for a Capillary IC System System 1 Shown Doc 065342 06 12 11 39 Dionex ICS 5000 Operator s Manual EGC III Analytical RFIC Eluent Degasser for Analytical IC only Electrical Cables CR TC Anal
339. r Hydrating a Capillary CR TC 3 If you are installing a CR TC in an analytical IC system IC a Locate the CR TC Hydration Tubing Kit P N 063487 provided in the EG Ship Kit Doc 065342 06 12 11 351 Dionex ICS 5000 Operator s Manual b Refer to Figure 9 27 to plumb the four ports on the CR TC To RFIC Fluent Degasser Analytical CR TC Flushing From EGC Out Port 9 Pump at application flow rate for 10 min A CR TC Hydration Kit Tubing Assembly P N 063487 Temporary connection Figure 9 27 Plumbing for Hydrating an Analytical CR TC 4 On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset select the following settings a DC panel Verify that the suppressor Mode is off To avoid damaging the suppressor always turn off the suppressor IMPORTANT before hydrating the CR TC The pump flow is on during conditioning however no flow reaches the suppressor b Pump panel e Gradient pump only Select the correct eluent channel A B C or D e Analytical pumps Set the flow rate recommended for your application This turns on the pump flow also Allow the pump to run for at least 10 minutes e Capillary pumps Set the flow rate to 0 02 mL min This turns on the pump flow also Allow the pump to run for 15 minutes 352 Doc 065342 06 12 11 9 EG Service 5 Turn off the pump flow 6 Disconnect the temporary tubing from the ELUENT OUT and REGEN IN ports on the CR TC
340. rdering Information Part Number Item Consumables for Capillary EG 072076 EGC KOH Capillary 072077 EGC MSA Capillary 072078 CR ATC Capillary 072079 CR CTC Capillary Consumables for Analytical EG 074536 EGC III KpgCO3 074532 EGC III KOH 074534 EGC III LiOH 074535 EGC III MSA 074533 EGC III NaOH 060477 CR ATC 060478 CR CTC 080135 EPM III Electrolytic pH Modifier 061686 EGC CO3 Mixer 4 mm 063443 EGC CO Mixer 2 mm Precision Cut Tubing for Capillary EG 072203 0 062 mm 0 0025 in ID PEEK 61 cm 24 in CR TC ELUENT OUT to EG Degas ELUENT IN 072204 0 062 mm 0 0025 in ID PEEK 18 cm 7 in CR TC ELUENT IN to EGC OUT Backpressure Coils 053762 Backpressure coil 2 0 mL min 500 psi 4 mm 053763 Backpressure coil 2 0 mL min 1000 psi 4 mm 053764 Backpressure coil 0 5 mL min 500 psi 2 mm 053765 Backpressure coil 0 5 mL min 1000 psi 2 mm Doc 065342 06 12 11 439 Dionex ICS 5000 Operator s Manual Part Number Item Miscellaneous 074459 EG degas cartridge for capillary IC systems Can be used with system pressures up to 35 MPa 5000 psi 074218 RFIC Eluent Degasser f5or analytical IC systems 954773 Fuse IEC 60127 2 slow blow rated at 2 A 250 V 063246 USB cable 1 m 3 ft long 043276 Ferrule fitting 10 32 double cone 043275 Fitting bolt 10 32 for double cone ferrule fit
341. re the waste line is not elevated at any point after it exits the TC If a line is blocked replace it see Section 9 29 Leaking injection valve 1 Make sure the liquid line connections to the valve are tight Replace any damaged fittings see Section 9 29 2 Liquid leaks from behind the valve stator may indicate a scratched rotor seal Rebuild the injection valve see Section 9 31 Leaking temperature stabilizer 1 Tighten the fittings on the temperature stabilizer inlet and outlet 2 Iftightening 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 300 Doc 065342 06 12 11 8 TC Troubleshooting 8 32 8 33 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 Technical Support for Dionex products 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 ve
342. re valves installed in a Dionex ICS 5000 Automation Manager NOTE NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product war ranty 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 2 Press the POWER button on the front of the DC for 2 seconds 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 hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT Open the DC door 4 Disconnect each liquid line connected to the valve Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 6 Reconnect all liquid lines to the injection valve 366 Doc 065342 06 12 11 9 DC Service 7 Turn on the power to the DC 8 Turn on the pump flow Check for leaks from the valve Tighten fittings as required For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on th
343. ressure reaches zero do the following e Disconnect the pump from the software by clicking Connected on the Pump 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 4 Five red Phillips screws are installed on the component mounting panel before shipment from the factory Remove these screws if present 5 Use the handles on the component mounting panel to pull the panel forward until it reaches the stop 6 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 7 The check valves are installed in the primary pump head see Figure 9 3 Outlet Check Valve Primary Pump Head Inlet Check Valve Figure 9 3 DP SP Check Valves Doc 065342 06 12 11 313 Dionex ICS 5000 Operator s Manual 9 6 2 10 Disconnect the tubing connections from the inlet and outlet check valves Loosen both check valve assemblies using the 1 2 inch wrench P N 062336 Remove both check valve assemblies from the pump head Installing the New Check Valves 1 The inlet check valve assembly housing has a 1 4 28 port Inlet Check Valve 1 4 28 Port Inspect the new inl
344. revent the leak sensor from triggering additional error messages 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 Iftheerror persists the heater may be faulty Replace the heater P N 061746 Doc 065342 06 12 11 267 Dionex ICS 5000 Operator s Manual 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 Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Appendix A for environmental specifications Suppressor 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 Thermo Scientific Reference Library DVD P N 053891 2 Follow the instructions in the suppressor manual to clean the suppressor 3 If you suspect a malfunction in the suppressor controller contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electron
345. riod of time a layer of contamination may build up When this occurs the electrode must be polished 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 Doc 065342 06 12 11 389 Dionex ICS 5000 Operator s Manual e Gloves e Tweezers Working Electrode Polishing Procedure NOTE To avoid electrode fouling always wear gloves when han dling electrodes 1 Follow the instructions in Section 9 28 3 Step 1 through Step 4 to remove the working electrode from the cell 2 Prepare the polishing pads a Designate a pad for use with the coarse polishing compound b Designate another pad for fine polishing compound also designate the working electrode type with which it will be used NOTE Do not use the same fine polishing pad to polish more than one type of working electrode this can contami nate the electrode surface with microparticles from the other working electrodes Designate a pad that will not be used with polishing compound This pad is for removal of particles after polishing see Step 5
346. rodes Conventional gold glassy carbon platinum and silver Disposable gold platinum carbon and silver Reference Electrode pH Ag AgCl combination one piece design Analytical and Capillary PdH combination one piece design Capillary only Autoranging Yes Analog Output User selectable full scale of 10 100 or 1000 mV Cell Volume Working Electrode lt 0 2 uL Doc 065342 06 12 11 429 Dionex ICS 5000 Operator s Manual ICS 5000 ED Electrochemical Detector Specifications Continued Maximum Cell Operating Pressure 0 7 MPa 100 psi System Software Software Chromeleon Chromatography Data System requires Microsoft Windows XP or Vista Detection Modes DC amperometry pulsed amperometry and integrated amperometry Detection modes include use of multiple waveforms and multiple integration times to optimize detection conditions for individual analytes Integrated amperometry mode unlimited changes to the waveform profile s number of segments duration of each segment and voltage applied at each segment 3 D Amperometry Three dimensional display of the raw integrated amperometry data set with crosshairs on an isoamperometric plot used to select slices of the plot along the applied voltage axis to render a chromatogram and along the time axis to render a voltammogram Automated Procedure Wizards Yes standard feature Sys
347. rol over timebase ICS 5000 Pump_1_Pressure Pump_2_Pressure Run Time Elapsed 20 0 00 0 50 1 00 1 Create Application 2 Prepare System Create Program Application Wizard 3 Execute Application System Maintenance Hold Daily Audit Trail Continue Consumable Change Edit Program Eluent Change Sequence Standard 1 Sample 1 Sample 2 Sample 3 Samnle 4 Single Single Single Single Sinale Standard Unknow Unknow Unknow I Inkenmae AS18 Tra AS18 Tra AS18 Tra AS18 Tra ASIR Tra ASMA Aninn Figure 5 7 Starting a Sequence in Chromeleon 6 8 Doc 065342 06 12 11 177 Dionex ICS 5000 Operator s Manual 5 3 5 3 1 5 3 2 Loading Samples Into the Sample Loop or Concentrator Two methods are available for loading samples e Loading samples with an autosampler see Section 5 3 1 e Loading samples with a syringe through the sample loading ports on the DC front door see Section 5 3 2 Loading Samples with an Autosampler 1 Verify that the autosampler output line is connected to the sample port on the DC or TC injection valve Direct the waste line as required for this autosampler model 2 Prepare and fill the sample vials and place them in the autosampler tray or carousel Refer to the autosampler manual for detailed instructions Autosampler manuals are provided on the Thermo Scientific Reference Library DVD
348. rrent applied to the EGC exceeds the maximum current allowed The EGC 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 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Refer to Section 8 23 to determine why there is no flow 3 If the error message appears again contact Technical Support for Dionex products for assistance The cartridge control electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components cannot be serviced by the user Doc 065342 06 12 11 247 Dionex ICS 5000 Operator s Manual 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 EGC can support To troubleshoot Replace the EGC see Section 9 14 EG1 over voltage Or EG2 over voltage This error occurs when the current applied to the EGC exceeds the maximum current allowed The EGC 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 Refer to Section 8 23 to determine why there is no flow 2 Ifthe error message appears again contact Technical S
349. rs e Wrench PdH Reference Electrode Replacement Procedure 1 Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector 400 Doc 065342 06 12 11 9 DC Service 2 Use a wrench to unscrew the PdH reference electrode nut and then remove the nut from the reference electrode well see Figure 9 66 Figure 9 66 Unscrewing the PdH Reference Electrode Nut 3 Pull the reference electrode out of the well see Figure 9 67 PdH Reference Electrode Figure 9 67 Removing the PdH Reference Electrode from the Reference Electrode Well Doc 065342 06 12 11 401 Dionex ICS 5000 Operator s Manual 4 Using tweezers remove the PdH reference electrode gasket from the well see Figure 9 68 PdH Reference Electrode Gasket Figure 9 68 Removing the PdH Reference Electrode Gasket 5 Using tweezers grasp the new PdH reference electrode gasket P N 072214 on its edge see Figure 9 69 To avoid deforming the gasket cutout do not place the tweezer tips on the cutout Cutout PA PdH Reference Electrode Gasket Figure 9 69 Installing the PdH Reference Electrode Gasket 6 Align the gasket so that the notched edge of the gasket aligns with the corresponding notch in the reference electrode well and press the gasket into the well 402 Doc 065342 06 12 11 9 DC Service 7 To avoid any hydraulic pressure build
350. rt 2500 e eee Not used Table 2 1 25 Pin D Sub I O Port Female Continued Analog Pressure Output 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 Function Inner ring Signal pressure Outer ring Ground 32 Doc 065342 06 12 11 2 Description 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 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Select the pump name 4 Select the AnalogOut property and select PumpTop For Chromeleon 6 8 click Execute USB Connections e One USB receptacle B type connector allows a connection from the PC on which Chromeleon is installed e Three USB Universal Serial Bus ports A type connectors are provided for connections to other Dionex ICS 5000 modules One 1 8 m 6 ft USB cable P N 960777 is provided in the pump ship kit Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capil
351. s 31 Dec 1999 current 1year 6months Invalid enumerated value Warning page 286 Next qualification of this module is due in x Warning page 286 day s due date is date Next qualification of this module is overdue due Warning page 287 date was date Next qualification of this module is overdue due Error page 287 date was date Module may no longer be used Next qualification of this module was due on Warning page 287 date Allowing x more grace day s Next service of this module is due in x day s Warning page 287 due date is date Next service of this module is overdue due date Warning page 287 was date No chip card in the reader for the column x Error page 288 No response from x for x seconds Warning page 288 No response from x for x seconds Device Abort page 288 disconnected Table 8 4 TC Error Messages Continued Doc 065342 06 12 11 211 Dionex ICS 5000 Operator s Manual TC Related Audit Trail Error Message Default Severity Level Operating columns above 70 C could affect Warning page 289 column performance Verify recommended column operating conditions before setting temperature above 70 C Parameter x value exceeded its allowed range Warning page 289 Set to closest valid value y Primary property x is already assigned and Error page 290 cannot be cha
352. s P N 045972 e Gloves e Blunt end tweezers 386 Doc 065342 06 12 11 9 DC Service ED Cell Gasket Replacement Procedure NOTE Always wear gloves when handling the ED cell Never touch the electrode surface 1 Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector 2 Loosen the yoke knob on the yoke block by unscrewing it two to three turns see Figure 9 53 First loosen the yoke knob Then squeeze the tabs on the yoke block and pull to remove it Figure 9 53 Disassembling the ED Cell Cell Configured for Analytical IC Shown 3 Squeeze the tabs on the sides of the yoke block and pull the block and knob off the working electrode see Figure 9 53 NOTE Handle the cell gasket and the inside surfaces of the cell carefully to prevent scratches which may subse quently cause leaks Doc 065342 06 12 11 387 Dionex ICS 5000 Operator s Manual 4 Carefully separate the parts see Figure 9 54 Conventional Working Electrode Block Cell Body Cell Gasket Figure 9 54 ED Cell Components 5 Use tweezers to remove the old cell gasket from the cell body see Figure 9 55 Alignment E nventional Pins Co G Working Electrode Gasket Figure 9 55 ED Cell Gasket for Conventional Working Electrodes 6 Rinse the surface of the cell with ASTM Type I 18 megohm cm filtered and deionized water that m
353. s 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 17 for details about the I O option Drain Port The drain port removes any liquid that collects in the drip tray in the bottom of the DC A clear corrugated drain hose P N 055075 is connected to this port during installation Place the drain hose into a waste container To maintain a positive siphon position the waste container below the level of the DC For correct drainage make sure the drain hose is not bent pinched or elevated at any point Do not allow the end of the hose to be submerged in waste liquid 82 Doc 065342 06 12 11 2 DC Description 2 17 IO Option When the I O option P N 062201 is installed two 12 pin connector strips are on the DC rear panel Figure 2 32 describes the functions assigned to each connector pin Description 16 bit analog output from detector 1 16 bit analog output from detector 2 5 V 200 mA Ground Solid state relay contacts output Connect for either normally open N O or normally closed N C Solid state relay contacts outp
354. s not on the Windows taskbar click Start gt All Programs gt Chromeleon gt Server Monitor to open the Server Monitor and click Start 150 Doc 065342 06 12 11 4 Startup 4 5 2 Starting the Chromeleon 6 8 Client 1 To start the Chromeleon 6 8 client click Start gt All Programs gt Chromeleon gt Chromeleon 2 To display the Chromeleon 6 8 panel tabset click View gt Default Panel Tabset or click the toolbar button EE The panel tabset opens to the Home panel by default see Figure 4 4 This panel displays basic status information for each instrument in the system In addition a limited number of device functions can be controlled directly from this panel You can also access the Audit Trail from here isson 10 Home Sequence Conto Stata Autoramgier Gradient Pumpr Evert Geneeator Detects Compartment Cond Detectar EC Detector 30 Amp Pt System a Aman tian Snp Stats beet a io E Elapsed Tere Figure 4 4 Example Chromeleon 6 8 Panel Tabset Doc 065342 06 12 11 151 Dionex ICS 5000 Operator s Manual 152 Doc 065342 06 12 11 ICS 5000 DP SP 4 6 DP SP Startup Setting Up the Eluent Reservoirs 1 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 that meets the specifications listed in Section 1 5 to prepare eluent and regenerant or to rinse el
355. s used for sample injection Optionally the 6 port valve can be installed instead of the 4 port valve In addition to the injection valve one or two high pressure valves can be installed in the lower compartment These valves can be used for applications requiring auxiliary valves In an analytical IC system one 6 port high pressure valve is installed in the Lo lower compartment for each system configured in the DC This valve is used for sample injection Optionally one or two high pressure valves can be installed on an AM see Section 2 18 These valves can be used for applications requiring auxiliary valves Each valve has two operating positions When configured as an injection valve liquid flows through either the Load or Inject path depending on the valve position In the Load position sample is loaded into the sample loop In the Inject position sample is swept to the column for analysis When configured as an auxiliary valve the flow path through system components in each valve position depends on the component configuration Doc 065342 06 12 11 65 Dionex ICS 5000 Operator s Manual 2 13 1 4 Port Valve The 4 port valve P N 074525 is the standard injection valve for capillary IC systems It is installed in the IC Cube see Figure 2 18 The valve has a 0 4 uL internal sample loop Figure 2 24 shows flow schematics for the 4 port valve LOAD POSITION INJECT POSITION Internal Internal Sample In Loop as In Loop
356. se und der Netzbuchse auf der R ckseite des EG The fuse drawer is located above the main power switch see Figure 9 30 A small 7 Fuse tab locks the fuse drawer in place Using a Drawer small screwdriver press the tab in and then Tab up to release the fuse drawer Pull the fuse drawer out of the rear panel and remove the old fuses Replace the two fuses with new 2 A IEC 60127 2 slow blow fuses P N 954773 Thermo Fisher Scientific recommends always replacing both fuses Figure 9 30 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 Doc 065342 06 12 11 357 Dionex ICS 5000 Operator s Manual 358 Doc 065342 06 12 11 b DC Service 9 19 Replacing Tubing and Fittings E 9 19 1 Tubing and Fittings for Capillary IC Systems Table 9 6 lists tubing and fittings used to plumb a DC system for capillary IC Tubing Size and Type Color P N Used to connect IC Cube Tubing Kit N A 072186 See Table 9 7 AS needle seal White 057301 AS normal and assembly 46 cm 18 in concentrate modes only with 10 32 ferrule fitting Injection valve to the AS inject port 0 25 mm 0 010 in ID Black 042690 AS sequential modes only PEEK tubing 50 cm 1 in Injection valve to AS 20 in diverter valve ED Cell Inlet Tubing Kit N A 074221 ED cell inlet to column outlet 10 32 fitting bolt Black 0432
357. sis This allows the DP SP to stabilize the flow rate Doc 065342 06 12 11 311 Dionex ICS 5000 Operator s Manual 9 6 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 Capillary IC pumps and analytical IC pumps use different check valves Verify that you have the correct check valve assembly for your pump type see Table 9 2 Pump Type Check Valve Assembly Part Number Capillary IC Inlet 044541 Outlet 044540 Analytical IC Inlet 045722 Outlet 045721 Table 9 2 DP SP Check Valve Assemblies Before beginning locate the 1 2 inch wrench P N 062336 in your pump ship kit DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 063342 Additional items e Cleanroom gloves lint free particle free and oil free e 0 2 micron filtered Class 10 isopropyl alcohol IPA e 0 2 micron filtered canned air duster ITW Chemtronics Ultrajet or equivalent 312 Doc 065342 06 12 11 9 DP SP Service 9 6 1 Removing the Check Valves 1 Turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system p
358. sor as instructed in the product manual Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 5 Let the system equilibrate before collecting data Before shipping the EG 1 Follow the instructions in Section 9 14 1 to remove the EGC from the EG 2 Plugall fittings Tighten the vent fitting capillary EGC or cap the vent port analytical EGC This will prevent the evaporation of water in the electrolyte reservoir IMPORTANT Make sure the EGC packaging conforms to hazardous material shipping requirements Refer to the Material Safety Data Sheet MSDS shipped with the EGC for the chemical description 186 Doc 065342 06 12 11 4 DC Shutdown 6 3 Consumables Storage The columns suppressors and other consumable items used with a Dionex ICS 5000 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 Thermo Scientific Reference Library DVD P N 053891 6 4 ED Cell Storage 6 4 1 Short term Storage of the ED 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 all fitting plugs NOTE Ifthe pH Ag AgCl reference electrode remains in the cell but eluent is not being pumped through the cell the pH Ag AgCI reference electrode frit may partially dry out If this occurs regenerate the e
359. ssing 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 Doc 065342 06 12 11 25 Dionex ICS 5000 Operator s Manual 2 2 5 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 vac uum degassing module delivers the optimal degassing perfor mance 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 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset Press the F8 key to open the Commands dialog box Select the pump name Select the Degasser property and select Off For Chromeleon 6 8 click Execute Si Pi o Di To turn on the degasser again select On Piston Seal Wash System The piston seal wash system 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 that meets the spe
360. ssure coil see Table 9 5 between the injection valve and the OUTLET port on the EGC Connect one end of the backpressure coil to Port P 2 on the injection valve connect the other end to the TO INJ VALVE IN P line Doc 065342 06 12 11 355 Dionex ICS 5000 Operator s Manual The EG Ship Kit P N 072047 includes four backpressure coils see Table 9 5 Part Backpressure Flow Rate Approximate Number Coil Description Backpressure Added 053762 4mm ID 2 0 mL min 3 5 MPa 500 psi 1 0 mL min 1 75 MPa 250 psi 053763 4mm ID 2 0 mL min 7 MPa 1000 psi 1 0 mL min 3 5 MPa 500 psi 053764 2mm ID 0 50 mL min 3 5 MPa 500 psi 0 25 mL min 1 75 MPa 250 psi 053765 2mm ID 0 50 mL min 7 MPa 1000 psi 0 25 mL min 3 5 MPa 500 psi Table 9 5 EG Backpressure Coils 356 Doc 065342 06 12 11 9 EG Service 9 18 DANGER DANGER ACHTUNG Changing the EG Main Power Fuses 1 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 12 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 Steckdo
361. stop 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 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 15 2 Installing and Flushing the New CR TC 1 Remove the plugs from the ports on the new CR TC If you are installing a CR TC in a capillary IC system a Connect a piece of 0 25 mm 0 010 in ID PEEK tubing between the ELUENT OUT and REGEN IN ports of the CR TC see Figure 9 26 This is a temporary connection b Locate the 38 cm 15 in piece of 0 025 mm 0 001 in ID tan PEEK tubing P N 074582 in the EG Ship Kit P N 072047 c Connect this line to the EGC INLET port and connect the other end to the EGC IN line from the pump pulse damper see Figure 9 19 This is a temporary connection to provide backpressure 350 Doc 065342 06 12 11 9 EG Service d Connect the EGC OUT line to the CR TC ELUENT IN port and connect the waste line to the CR TC REGEN OUT port Capillary CR TC Flushing Pump at 0 02 mL min for 15 min 0 062 mm 0 0025 in ID n PEEK Tubing Assembly P N 072204 TO PUMP DAMPER To Waste gt 1 58 mm 0 062 in ID Tefzel Tubing Assembly P N 072225 0 25 mm 0 010 in ID PEEK Tubing Temporary connection Figure 9 26 Plumbing fo
362. t 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 Technical Support for Dionex products for assistance Doc 065342 06 12 11 279 Dionex ICS 5000 Operator s Manual Communication time out This error occurs if a TC firmware 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 If you cannot identify the cause of the error contact Technical Support for Dionex products for assistance 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 Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program 2 In the instrument or timebase right click the TC and select Properties 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 280 Doc 065342 06 12 11 8 TC
363. t Identification Product Ion Chromatography System Brand Dionex Model ICS 5000 DC SP DP EG TC Manufacturer Dionex Corporation 1228 Titan Way Sunnyvale California 94088 USA Representative Larry McNary Dionex Corporation 1228 Titan Way Sunnyvale CA USA 94085 Function Director Engineering Means of conformity The product s listed above are in conformity to the following listed directives and standards All products were tested and evaluated to the corresponding current standard based on the date this document was signed Low Voltage Safety Directive 2006 95 EC EMC Directive 2004 108 EC Safety Standards EN 61010 1 UL 61010 1 CAN CSA C22 2 No 61010 1 EMC Standards EN 61326 1 Signature of Representative Tu Name Larry McNary Place Sunnyvale CA USA Date 28 MAY 2010 Doc 065342 06 12 11 19 Dionex ICS 5000 Operator s Manual 1 5 Deionized Water Requirements for IC For eluent generation or when manually preparing eluent and regenerant use ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Table 1 1 Contaminant Specification lons Resistivity gt 18 0 megohm cm Organics TOC lt 10 ppb lron Transition Metals lt 1 ppb Pyrogens lt 0 03 Eu mL Particulates gt 0 2 um lt 1 units mL Colloids Silica lt 10 ppb Bacteria lt 1 cfu mL Type Water Iron transition metal content no
364. t 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 Doc 065342 06 12 11 77 Dionex ICS 5000 Operator s Manual 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 pH Ag AgcCI reference electrode to dry out Make sure that eluent is being pumped continuously through the cell at a low flow rate for example 0 05 mL min 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 elec trode from the cell and store it in its storage cap filled with saturated KCI solution See Section 6 4 for detailed storage instructions Monitoring the ED Cell pH Readout Monitoring the pH readout of a solution with a known composition lets you detec
365. t any reference potential shift that may occur over time This allows you to determine when the pH Ag AgCl reference electrode needs regenerating or replacing thus improving the reproducibility of your analyses For instructions on how to monitor the pH readout see Section 4 1 2 NOTE Monitor the pH when the pH Ag AgCl reference electrode is used in the Ag mode as well as in the pH mode 78 Doc 065342 06 12 11 2 DC Description 2 15 3 Palladium Hydrogen PdH Reference Electrode The PdH reference electrode consists of palladium and platinum electrodes immersed in an aqueous solution With a potential applied between the two electrodes palladium is connected as a cathode and platinum as an anode As a consequence of the applied potential hydrogen gas is generated at the palladium electrode and oxygen gas at the platinum electrode Whereas the oxygen gas is swept out of the cell in the liquid stream a portion of the hydrogen gas is taken up by palladium metal An equilibrium develops between molecular hydrogen in the liquid phase and the adsorbed hydrogen in palladium The palladium hydrogen electrode becomes a reference electrode with a half reaction of Ht e H3 Where the hydrogen is supplied by the following process Pd H gt Pd H ds gt Pd H py The PdH reference electrode is thus similar to the standard hydrogen electrode which is based on the same half reaction between the hydronium ions and molecular hydrog
366. t des gants protectives en manipulant la cartouche Die EGC Kartusche enthalt eine korrodierende Base KOH LiOH oder NaOH eine korrodierende S ure MSA oder eine konzentrierte K2C03 L sung Tragen Sie daher beim Umgang mit Kartusche eine Schutzbrille und Handschuhe 9 14 1 Removing the Old EGC 1 Turn off the pump flow This turns off the power to the EGC and the suppressor also Open the front door of the EG Pull the tray forward until it reaches the stop Twist the ring on the EGC electrical cable counter clockwise to loosen it and then pull the cable straight out of the EGC 1 or EGC 2 hermo bulkhead connector see Figure 9 14 EGC Cables Figure 9 14 EGC Gables Close or cap the EGC vent opening to prevent leakage when you turn over the cartridge in Step 7 If you are removing a capillary EGC tighten the Vent Fitting vent fitting on the top of the EGC see Figure 9 15 7 N AN wARNI Mi tig Net are highly we Figure 9 15 Capillary EGC Vent Fitting Doc 065342 06 12 11 337 Dionex ICS 5000 Operator s Manual If you are removing an analytical EGC IC a Remove the VENT line from the EGC by unscrewing the 10 32 luer adapter see Figure 9 16 pre NOTE If necessary use a i pocne artridge vide wrench to hold the pannel rh luer adapter in place mt while unscrewing the wat vent line ENA ie b Locate the 10 32 plug P N 053981 removed fro
367. t is held until injection Excess sample flows out to waste Eluent flows from the pump through the valve and to the column bypassing the sample loop e In the Inject position 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 1 describes how to inject samples with an autosampler and Section 5 3 2 describes how to inject samples manually A 10 uL PEEK sample loop P N 042949 is installed between ports L 1 and L 4 Thermo Fisher Scientific 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 Doc 065342 06 12 11 67 Dionex ICS 5000 Operator s Manual 2 13 3 10 Port Valve The 10 port valve P N 061962 is an optional valve available for various applications Figure 2 26 shows example flow schematics for the 10 port valve when it is connected for an application that uses a concentrator column NOTE Other plumbing configurations for the 10 port valve are pos sible depending on the components to be connected to the valve and the application to be run Refer to the appropriate Application Note for more information LOAD POSITION Loop Loading Concentrator To Column Eluent INJECT POSITION Concentrator Loading Concentrator To Column Eluent e Pump In seers Pump In Large Large Loop Loop NA OCF
368. t specified for ASTM Table 1 1 ASTM Filtered Type Deionized Water Specifications for lon Chromatography 20 Doc 065342 06 12 11 ICS 5000 DP SP 2 1 2 Description DP SP Description DP SP Front Features A status bar on the front of the Dionex ICS 5000 Dual Pump DP and Dionex ICS 5000 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 eee Se MII E CONNECTED ALARM YV PUMP 1 A PUMP 2 Figure 2 1 DP Status Bar FLOW PRIME So sta OF CONNECTED ALARM V PUMP 1 Figure 2 2 SP Status Bar Doc 065342 06 12 11 21 Dionex ICS 5000 Operator s Manual Button LED If the LED Is On If the LED Is Flashing Label CONNECTED The DP SP is connected to Does not flash a Chromeleon 7 instrument or Chromeleon 6 8 timebase ALARM A DP SP related problem Does not flash has occurred for example a pressure limit was activated Check the Chromeleon Audit Trail for the cause PUMP 1 FLOW PUMP 2 FLOW Use the FLOW button to start and stop the pump flow The LED indicates when the flow is on Does not flash PUMP 1 PRIME PUMP 2 PRIME Use the PRIME button to prime the pump see Section 9 5 The LED indicates whether the pump is being primed The pump is being primed POWER
369. te specifications EG1 invalid flow rate concentration or EG2 invalid flow rate concentration This error occurs if the selected concentration is too high for the current flow rate To troubleshoot Set the flow 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 EGC type and cartridge configuration For details refer to Section 4 9 EGI1 invalid ion count or EG2 invalid ion count This error occurs if the ion count reported by the EGC is invalid This may indicate a problem with the memory chip in the EGC To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance 246 Doc 065342 06 12 11 8 EG Troubleshooting EG1 invalid serial number or EG2 invalid serial number This error occurs if the serial number reported by the EGC is invalid This may indicate a problem with the memory chip in the EGC To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance EG1 over current Or EG2 over current This error occurs when the cu
370. tector 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 edge FRE mode works identically to the TTL 5V normal edge mode except that the INVERTED positive and negative edges are EDGE gii reversed in function Action Off Di No Effect e Normal Pulse In normal pulse operation the negative falling TIL t5V edge of the TTL signal is the active Mn i edge and the positive rising edge is ignored Action On A R 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 to the normal pulse mode except that the positive and negative edges are reversed in function Action On Action Off Doc 065342 06 12 11 93 Analytical Dionex ICS 5000 Operator s Manual 2 18 Automation Manager The Dionex ICS 5000 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 39 The tray is installed in the upper compartment of the DC see Figure 2
371. tector of each type For details about the CD see Section 2 14 For details about the ED see Section 2 15 Doc 065342 06 12 11 61 Dionex ICS 5000 Operator s Manual Suppressors for conductivity detection are also installed in the upper compartment The following types of suppressors can be used e Thermo Scientific Dionex SRS 300 Self Regenerating Suppressor 2 and 4 mm e Thermo Scientific Dionex AES Atlas Electrolytic Suppressor e MMS 300 MicroMembrane Suppressor Lower Compartment Features for Analytical IC IC 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 13 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 22 Handle for pulling tray forward Figure 2 22 DC Lower Compartment Tray Handle 62 Doc 065342 06 12 11 2 DC Description 2 12 DC Temperature Control Zones The following temperature control zones are possible with the DC depending on the options installed e e e no E Ic DC upper compartment DC lower compar
372. tectors e Injection valves e Switching valves e Guard and separator columns e Suppressors e Dionex IC Cubes or Dionex ICS 5000 Automation Manager Dionex ICS 5000 Conductivity Detector CD The CD is a modular detector with an integrated cell 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 For a dual system two CDs can be installed Dionex ICS 5000 Electrochemical Detector ED The ED is a modular detector and a modular cell The ED supports multiple waveforms multiple integration times and post analysis data manipulation With Chromeleon 6 8 the ED is also capable of providing 3D amperometry data The ED cell can be configured with gold silver platinum carbon or glassy carbon working electrodes The ED is installed in the upper compartment of the DC For a dual system two EDs can be installed Ber Dionex IC Cube IC Cube The IC Cube houses components for running capillary IC applications Each IC Cube includes an injection valve a column heater and removable cartridges containing capillary IC components Cartridges for the following components are available carbonate removal device CRD suppressor guard and separator columns and EG degasser The IC Cube is installed in the Doc 065342 06 12 11 7 Dionex ICS 5000 Operator s Manual upper compartment of the DC For a dual system two IC Cubes can be
373. tem Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Application Templates Yes standard feature Automation Support of Third Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Customizable System Control Panels Yes standard feature Signal Channels Electrochemical and total electrochemical signals Data Trending Plots Yes all device numerical parameters plotted Doc 065342 06 12 11 A DC Specifications ICS 5000 ED Electrochemical Detector Specifications Continued System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature System Trigger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory present and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance Yes optional Physical Dimensions 6 9 x 16 7 x 9 9 cm 2 7 x 6 5 x 3 9 in h x w x d Weight 400 g 1 6 Ib Doc 065342 06 12 11 431 Dionex ICS 5000 Operator s Manual 432 Doc 065342 06 12 11 mam TC Specifications ICS 5000 TC Thermal Comp
374. tems only PEEK 13 cm 5 in 1 in Proportioning eluent valve to inlet check valve 0 159 cm 0 0625 in Yellow 063268 Peristaltic pump to primary ID PharMed 1 in pump head 0 15 cm 0 060 in ID Colorless 064079 Peristaltic pump to seal Tygon 2075 tubing 1 in wash reservoir e Between pump heads for seal wash 1 58 mm 0 062 in ID Colorless 014157 Eluent reservoirs PTFE 1 in e Vacuum degassing assembly 1 58 mm 0 062 in ID Colorless 047203 Secondary pump head to polyurethane 1 in waste Table 9 1 DP SPTubing and Fittings 306 Doc 065342 06 12 11 9 DP SP Service Tubing Size and Type Color P N Used to connect 10 mm 0 39 in ID Colorless 055075 Drip tray drain hose polyethylene 1 16 in fitting bolt Tan 052230 Inlet check valve fitting 1 16 in ferrule Tan 062511 1 8 in fitting bolt Tan 052267 Eluent reservoir fittings 1 8 in ferrule Yellow 048949 High pressure 10 32 Blue 074449 Capillary pumps only Pulse fitting bolt damper to EGC or injection valve High pressure 10 32 Blue 074373 Use with high pressure fitting ferrule double cone bolts 10 32 fitting bolt Black 043275 All other tubing fittings 10 32 ferrule double Tan 043276 cone Table 9 1 DP SPTubing and Fittings Continued Notes e For tightening requirements for the 10 32 fitting bolt P N 043275 and ferrule P N 043276 refer to Installation of Dionex Liquid Line Fi
375. terclockwise to loosen it and then pull the cable straight out of the EGC 1 or EGC 2 bulkhead connector Remove the backpressure tubing from the waste container and remove the waste container Replace the 10 32 plug in the EGC vent opening Lift the EGC out of the holder turn it upside down and place it on the drip tray in the service position see Figure 9 17 Disconnect the backpressure coil from the EGC OUTLET port Connect the EGC OUT line to the OUTLET port Turn the EGC right side up and check for bubbles in the eluent generation chamber If necessary shake and tap the cartridge to remove bubbles Install the EGC in the holder Remove the 10 32 plug from the vent opening and reinstall the luer adapter and vent line Reconnect the EGC electrical cable 9 15 Replacing the CR TC The CR TC replacement procedure consists of Removing the old CR TC see Section 9 14 1 Installing and hydrating the new CR TC see Section 9 15 2 Completing the plumbing for the new CR TC see Section 9 15 3 Doc 065342 06 12 11 349 Dionex ICS 5000 Operator s Manual Refer to Figure 9 18 for a flow schematic of the EG and CR TC for capillary IC and to Figure 9 22 for analytical IC 9 15 1 Removing the Old CR TC 1 Turn off the pump flow This turns off the power to the EGC 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
376. the cause of the error contact Technical Support for Dionex products for assistance 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 compares 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 download the existing firmware cannot be erased from memory To troubleshoot Flash memory cannot be serviced by the user Contact Technical Support for Dionex products for assistance Doc 065342 06 12 11 283 Dionex ICS 5000 Operator s Manual A Error during storing of the card data to the chip card This error occurs 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 30 Error programming flash memory This error occurs if during a firmware download the new firmware cannot be program
377. 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 upper DC compartment to a high of 60 C Temperature Compensation 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 To change the temperature compensation factor 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Select the conductivity detector 4 Select the Temperature_Compensation property and enter the value 5 For Chromeleon 6 8 click Execute 70 Doc 065342 06 12 11 2 DC Description 2 14 2 Suppressor The suppressor reduces the eluent conductivity and enhances the conductivity of the sample ions thereby increasing detection sensitivity Installation of a suppressor is optional The capillary and analytical CDs can operate with the following suppressors Available Suppr
378. the error appears again contact Technical Support for Dionex products for assistance ED cell current exceeds limits error This error can have multiple causes for example a cell potential that is too high for a given salt concentration a cell potential that is too high because the reference mode is incorrect injection of excessive amounts of electroactive Doc 065342 06 12 11 261 Dionex ICS 5000 Operator s Manual analytes a damaged or incorrectly installed cell gasket or an electrical short between two of the three electrodes To troubleshoot 1 Turn off the cell voltage Excessive currents can change or even damage the working electrode 2 Turn off the pump flow 3 Disassemble the cell see Section 9 28 3 and check for evidence of liquid and salt bridges that can cause shorts Rinse the cell surface and dry it with a clean lint free towel Replace the cell gasket 4 Verify that the correct electrode material waveform potentials and reference mode are selected for the application being run 5 Restart the flow and select DC amperometry mode Apply cell potential in steps increasing toward the detection potential the potential of the integration period in integrated amperometric detection If the current becomes excessive again try a new working electrode or another cell if available ED cell option disconnected This error indicates that the electrochemical detector is unplugged To troubles
379. 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 2 Check fittings for overtightening Check tubing for crimping and replace it as necessary see Section 9 3 Be careful not to overtighten fittings Doc 065342 06 12 11 235 Dionex ICS 5000 Operator s Manual If the low pressure limit was tripped 1 Verify that the Minimum Pressure setting is set to the correct value 2 Make sure there are no liquid leaks in the flow system To find and eliminate the source of a leak see Section 8 15 If an Audit Trail error message is displayed refer to the troubleshooting steps listed for the particular message 8 14 DP SP Stops Instrument method or 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 7 instrument method the Chromeleon 6 8 program or other remote signal source If you do not want the pump to stop take the appropriate preventive action edit the instrument method the program or the settings of the other remote signal source Low pressure limit was tripped Refer to the troubleshooting steps for the Audit Trail message Pressure fallen below lower limit on page 231 High pressure limit was tripped Refer to the troubleshooting steps for the Audit Trail message The system pressure exceeded th
380. 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 Rotor Lever BA Figure 6 1 Peristaltic Pump for Seal Wash 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 Doc 065342 06 12 11 183 Dionex ICS 5000 Operator s Manual 184 Doc 065342 06 12 11 feel 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 EGC and the suppressor is off IMPORTANT Supplying power to the EGC when there is no eluent flow can severely damage the cartridge 3 Store the EGC in the EG during the shutdown To restart the EG 1 Select the parameters for the analysis on the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset For EG startup information see Section 4 9 2 In an analytical IC system if the EG has been shut d
381. then to the remainder of the chromatography system 28 Doc 065342 06 12 11 2 Description 2 3 2 Gradient Pump Flow Schematic Figure 2 6 illustrates the liquid flow path through a gradient pump OUTLET CHECK VALVE ELUENT ELUENT A B ELUENT ELUENT Cc D SECONDARY PRIMARY PUMP PUMP HEAD HEAD STATIC MIXER PROPORTIONING VALVE TO ELUENT GENERATOR OR INJECTION VALVE Figure 2 6 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 eluent generator if installed or injection valve and then to the remainder of the chromatography system Doc 065342 06 12 11 29 Dionex ICS 5000 Operator s Manual 2 4 DP SP Rear Panel Figure 2 1 illustrates the rear panel of the DP SP Tubing Chase 2 Main Power Switch Fuse Holder and Power Receptacle Digital 1 0 Port o Analog Pressure Output
382. there is a slimy film on the interior follow the cleaning instructions in Section 9 4 Flush the system with ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Replace all end line filters P N 045987 See Section 4 6 for instructions Prepare new stock solution 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 that meets the specifications listed in Section 1 5 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 that meets the specifications listed in Section 1 5 The column may be the source of the problem Refer to the column manual for troubleshooting assistance Column manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 The injection valve may be the source of the problem Rebuild the injection valve see Section 9 22 Doc 065342 06 12 11 219 Dionex ICS 5000 Operator s Manual 8 4 Peak Retention Times Are Too Early Eluent concentration setting is too high The correct eluent concentration setting depends on several factors the flow rate EGC type et
383. tical in function Relay_Com Relay_N O Digital Input Digital_GND Not Used Not Used N O Normally open contact Figure 2 63 Digital VO Connector When the relay is activated the connection is between Com and N O Connection Description Digital Input lt gt Digital GND 0 to 5 V Relay_Com lt gt Relay_N O Switching voltage 100 VDC Switching current 0 25 A Carry current 1 0A Switching capacity 3 W Contact resistance Max 150 megohms 120 Doc 065342 06 12 11 2 TC Description Use the 6 pin mini DIN signal cable P N 6000 1004 provided in the TC Ship Kit P N 064789 to connect the TC to an external device For details about the pin assignments refer to Table 2 5 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 5 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 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
384. ting 046985 Mini screwdriver 440 Doc 065342 06 12 11 mean DC Reordering Information Part Number Item Valves and Accessories 074525 High pressure injection 4 port 061961 High pressure injection or switching valve 6 port 061962 High pressure injection or switching valve 10 port 061971 Low pressure valve 3 way 061745 Low pressure valve 2 way 042949 Sample loop 10 uL 042857 Sample loop 25 uL 044105 Filter high pressure inline for sample filtering 024305 Luer adapter fitting 1 4 28 for manual injections 016388 Syringe 1 cc for manual injections 074698 Valve rebuild kit 4 port 057896 Valve rebuild kit 6 port 061759 Valve rebuild kit 10 port IC Cube and Accessories for Capillary IC 072000 Dionex IC Cube 072186 IC Cube tubing kit includes precision cut tubing for column connections 074459 EG degas cartridge capillary Can be used with system pressures up to 35 MPa 5000 psi 072052 ACES 300 Anion Capillary Electrolytic Suppressor 072053 CCES 300 Cation Capillary Electrolytic Suppressor 072055 Suppressor bypass cartridge 072054 CRD 200 Carbonate Removal Device Capillary 072056 CRD bypass cartridge Doc 065342 06 12 11 441 Dionex ICS 5000 Operator s Manual Part Number Item Conductivity Detector for Capillary IC 072041 Dionex ICS 5000 Conductivity Detector Capillary
385. tivated and continue to report a leak to the Audit Trail e Check the waste container and empty as needed 7 7 EG Weekly Maintenance e Check all lines for crimping Move or reroute pinched lines and replace damaged lines see Section 9 12 For help in isolating the cause of a tubing restriction see Section 9 13 e Monitor the system backpressure A gradual increase in backpressure can indicate clogging of the EGC inlet frit from particulates in the eluent water 7 8 EG Annual Maintenance e Check the expiration date and remaining lifetime of the EGC on the EG ePanel in Chromeleon 7 or the Control panel in Chromeleon 6 8 Doc 065342 06 12 11 197 Dionex ICS 5000 Operator s Manual 198 Doc 065342 06 12 11 si DC Routine Maintenance This section describes routine maintenance procedures for the Dionex ICS 5000 Detector Chromatography Module DC that users may perform All other maintenance procedures must be performed by Thermo Fisher Scientific personnel 7 9 DC Daily Maintenance e 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 that meets the specifications listed in Section 1 5 e Check the waste container and empty as needed NOTE If you are using an electrochemical detector also see the spe cial maintenance considerations that are described in Section 4 1 2
386. tment Heated conductivity cell IC Cube capillary column heater RCH 1 Reaction Coil Heater installed in an AM The temperatures achieved for a particular zone can vary from the control range depending on the ambient temperature see Table 2 3 Temperature Control Achieved Temperatures Based on Ambient Zone Range Upper 10 to e Ifno temperature controlled devices CD cell compartment 40 C IC Cube heater or RCH 1 are on Minimum temperature gt ambient 22 C e If a temperature controlled device is set to 60 C or above Minimum temperature gt ambient 17 C Note The achieved temperature can be reduced another few degrees by setting the DC upper compartment fan speed to high see page 64 e Maximum temperature gt ambient 20 C Lower 10 to Minimum temperature gt ambient 15 C compartment 70 C Maximum temperature gt ambient 50 C CD cell 15 to Minimum temperature gt upper compartment 60 C temperature 5 C IC Cube column 15 to Minimum temperature gt upper compartment heater 80 C temperature 5 C RCH 1 20 to Minimum temperature gt upper compartment 80 C temperature 5 C Table 2 3 Achieved Temperatures per DC Temperature Zone Doc 065342 06 12 11 63 Dionex ICS 5000 Operator s Manual Minimum temperatures are also affected by the ambient humidity If the humidity is high the minimum temperatures achieved for a tempera
387. to the opening in the DC and press firmly to ensure the electrical connection is secure 8 Reconnect the cell inlet and outlet lines 9 Reinstall the suppressor see Section 9 27 2 10 Turn on the DC power and restart the pump flow 9 27 4 Removing Trapped Air from the Conductivity Cell IC Air bubbles in the cell can cause pulsations of the baseline random noise and low readings Air may result from outgassing of the eluent In an analytical IC system follow the steps below to remove trapped air from the cell These steps are not required for a conductivity cell in a capillary IC system Doc 065342 06 12 11 383 Dionex ICS 5000 Operator s Manual 1 3 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 9 for the appropriate type and number of backpressure tubing coils required Suppressor Column Flow Rate Backpressure Type Format mL min Coils Dionex 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 Dionex SRS or 2mm or 3 mm lt 0 25 2 red Dionex MMS 2mmor3 mm 0 25 to 0 50 1 red with fittings The red coil P N 045878 consists of 0 125 mm 0 005 in ID PEEK tubing Table 9 9 Backpressure Coil Requirements Table 9 10 lists the correct pressure range for each type of suppressor Suppressor Type 0 14 to 0 70 MPa 20 to 100 psi Dionex AES Pressure Rang
388. to the power supply 3 If you cannot identify the cause of the error contact Technical Support for Dionex products for assistance 292 Doc 065342 06 12 11 8 TC Troubleshooting 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 Technical Support for Dionex products 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 A 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 To reinitialize the chip card open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Under TC select the column name and select the FormatChipCard command 4 For Chromeleon 6 8
389. trol electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components cannot be serviced by the user 244 Doc 065342 06 12 11 8 EG Troubleshooting EG1 invalid activation date Or EG2 invalid activation date This error occurs if the activation date for the EGC is not a valid date This may indicate a problem with the memory chip in the EGC To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance EG1 invalid concentration or EG2 invalid concentration This error occurs if the eluent concentration is outside the range allowed by the EG This may indicate corrupted memory or a problem in the EG instrument control firmware To troubleshoot Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components and instrument control firmware cannot be serviced by the user Doc 065342 06 12 11 245 Dionex ICS 5000 Operator s Manual EG1 invalid flow or EG2 invalid flow This error occurs if the flow rate is set to a value the EG does not support To troubleshoot Set the flow rate to a value within the allowed range Refer to Appendix A for flow ra
390. ts NOTE A Virtual Column Separation Simulator is available in Chromeleon that can help you determine the best oper ating parameters column eluent flow rate tempera ture for a particular analysis Refer to the Chromeleon Help for details 172 Doc 065342 06 12 11 5 Operation 5 2 1 Creating a New Sequence in Chromeleon 7 In Chromeleon 7 two methods are available for creating a new sequence eWorkflows and the Sequence Wizard e eWorkflows provide predefined templates and rules for creating new sequences If they have been defined for your laboratory eWorkflows are the preferred method for creating a new sequence e If eWorkflows are not available use the Sequence Wizard Using eWorkflows 1 On the Console click the eWorkflows category bar see Figure 5 2 In the Navigation Pane click the eWorkflow name 2 In the work area click the instrument name and then click Launch P Chromeleon Console mX Create File Edt View Tools Help eWorkflows Anions Anions Description This is an example eWorkflow for anion analyses on Type IC an ICS 5000 system Status Approved for Use No attachments Launch lt Run Anions on instrument ICS 5000 gt Edit Ni Instrument Name Instrument Status Sequence Status la Queue Status Hin Instruments E Ics 5000 Idle Er Data eWorkflow Anions selected Figure 5 2 eWorkflow View in Chromeleon 7 3 The eWor
391. ttings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 e For tightening requirements for the high pressure fitting bolt P N 074449 and ferrule P N 074373 see Section 9 2 e 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 072011 Refer to the instructions provided with the cutter Doc 065342 06 12 11 307 Dionex ICS 5000 Operator s Manual 9 4 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 that meets the specifications listed in Section 1 5 If a reservoir still appears dirty or has a slimy film on the inside clean it as instructed below Bey Clean reservoirs in a capillary IC system every 3 months as instructed below 1 Dispose of any remaining chemicals according to municipal regulations 2 Rinse the reservoir inside and out with ASTM Type I 18 megohm cm filtered and deionized water 3 Rinse the inside of the reservoir with isopropyl alcohol or methanol 4 If algae 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
392. ture zone is not as low as those achieved in a low ambient humidity environment NOTE ADC 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 com partments and to recalibrate if required To set the fan speed of the DC upper compartment to high 1 Open the Chromeleon 7 Instrument Configuration program or Chromeleon 6 8 Server Configuration program 2 Double click the DC icon under the instrument or timebase 3 Click the Thermal Controls tab and then double click Compartment_TC 4 Under Fan Speed click High Speed see Figure 2 23 DC Detector Chromatography ICS 5000 Device Configuration Device Name Compartment_TC Instrument 50 y Fan Speed I Enable Fan On Low Speed High Speed Description Control the fan speed Low For standard environment temperature 0 to 30 C less fan noise High For higher environment temperature above 30 C cr OK Cancel pi Help Figure 2 23 Setting the DC Upper Compartment Fan Speed 64 Doc 065342 06 12 11 2 DC Description 2 13 High Pressure Valves Up to four high pressure valves can be installed in the DC The following valve models are available 4 port P N 074525 6 port P N 061961 and 10 port P N 061962 ay In a capillary IC system one 4 port high pressure valve is installed on each IC Cube This valve i
393. u are installing a high pressure fitting blue bolt and ferrule follow the instructions below to tighten the fitting 304 Doc 065342 06 12 11 any 9 2 Tightening Guidelines for High Pressure Fittings Follow these guidelines when tightening a high pressure fitting bolt P N 074449 and high pressure ferrule P N 074373 1 First use your fingers to tighten the fitting bolt as tight as you can Then use a wrench to tighten the fitting an additional 3 4 turn 270 degrees 2 If leaks occur replace the fitting bolt ferrule and tubing Doc 065342 06 12 11 305 Dionex ICS 5000 Operator s Manual are DP SP Service 9 3 Replacing Tubing and Fittings The DP SP is plumbed with the tubing and fittings listed below Tubing Size and Type Color P N Used to connect Pump outlet tubing Black 068658 Pulse damper outlet assembly 0 25 mm capillary pumps or static 0 010 in ID PEEK valve outlet standard bore 86 cm 34 in analytical pumps to EGC inlet or injection valve 0 125 mm 0 005 in ID Red 044221 Microbore analytical pumps PEEK 86 cm 34 in 1 in only Static valve outlet to EGC inlet or injection valve 0 25 mm 0 010 in ID Black 042690 Primary and secondary PEEK 10 cm 4 in 1 in pump heads 0 51 mm 0 020 in ID Orange 042855 Microbore systems only PEEK 13 cm 5 in 1 in Proportioning eluent valve to inlet check valve 1 02 mm 0 040 in ID Tan 054410 Standard bore sys
394. uL Anion CES 0 4 mm lt 1 0 pL Cation CES 0 4 mm lt 1 0 pL System Software Software Chromeleon Chromatography Data System requires Microsoft Windows XP or Vista Automated Procedure Wizards Yes standard feature System Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Application Templates Yes standard feature Doc 065342 06 12 11 425 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 DC Detector Chromatography Compartment Specifications Automation Support of Third Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Customizable System Control Panels Yes standard feature Signal Channels Detector signals detector background signals temperatures Data Trending Plots Yes all device numerical parameters plotted System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature System Trigger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory current and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance
395. uard cartridges Refer to the installation and troubleshooting guide for the Dionex OnGuard cartridge for instructions The guide is located on the Thermo Scientific Reference Library DVD 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 concentrations are so low that dilution is not necessary To dilute the sample use eluent or ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 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 148 Doc 065342 06 12 11 4 Startup 4 3 4 4 4 4 4 1 4 4 2 Filling the Autosampler Vials and Loading the Sample Tray Follow the instructions in the autosampler manual to fill the vi
396. ubing the eluent is directed to the injection valve and then to the guard and separator columns The EG degas capillary cartridge also contains plumbing connections that route the regenerant flow from the suppressor out of the IC Cube to the regenerant inlet port of the Continuously Regenerated Trap Column Capillary in the EG If the system does not include an EG the eluent inlet line from the EG degas cartridge is connected directly to the pump outlet The regenerant outlet line is directed to waste 58 Doc 065342 06 12 11 2 DC Description IC Cube Eluent and Regenerant Flow The numbers on the schematic shown in Figure 2 19 indicate the flow path of eluent and regenerant through the plumbing connections on an IC Cube configured for conductivity detection To CR TC Regen In Port From CR TC Eluent Out Port Conductivity Detects Capillary Figure 2 19 IC Cube Eluent and Regenerant Flow Schematic for Conductivity Detection NOTE For the complete conductivity detection flow path including the flow through components installed inside the IC Cube cartridges see Section 2 14 3 Doc 065342 06 12 11 59 Dionex ICS 5000 Operator s Manual The numbers on the schematic shown in Figure 2 20 indicate the flow path of eluent and regenerant through the plumbing connections on an IC Cube configured for electrochemical detection Cio A To CR TC 2 Re
397. ubleshoot Select a flow rate within the DP SP flow rate range For the flow rate range for each type of DP SP refer to Section 1 5 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 065342 06 12 11 229 Dionex ICS 5000 Operator s Manual 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 see Section 9 3 Be careful not to overtighten fittings 2 Inspect the outlet check valve for blockage Replace the check valve cartridge if needed see Section 9 6 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 Technical Support for Dionex products for assistance Motor position error The motor is overloaded
398. uent reservoirs If an EG is not installed prepare the eluent for the application For instructions refer to the manual for the column Column manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 Fill the reservoirs with prepared eluent or deionized water if an EG is installed Locate the end line filters P N 045987 provided in the pump ship kit Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 072111 SP Ship Kit Capillary or Analytical 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 the eluent lines Hand tighten the caps Doc 065342 06 12 11 153 Dionex ICS 5000 Operator s Manual 4 7 NOTE A 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 out let and the eluent inlet port on the injection valve For details see the instructions provided with the inline filter Setting Up the Piston Seal Wash System Replumb
399. up when inserting the reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings 8 Align the fitting on the end of the PdH reference electrode so that the knobs on the fitting align with the grooves in the reference electrode well see Figure 9 70 9 Insert the fitting into the well PdH Reference Electrode Knobs Grooves Figure 9 70 Inserting the PdH Reference Electrode Fitting into the Reference Electrode Well 10 Screw the nut on the PdH reference electrode into the reference electrode well and tighten it fingertight see Figure 9 71 After fingertightening use a wrench to tighten the nut an additional 20 to 30 degrees L Figure 9 71 Installing the PdH Reference Electrode Nut Doc 065342 06 12 11 403 Dionex ICS 5000 Operator s Manual 11 12 13 14 Orient the cell assembly with the yoke knob on the left and then push the cell onto its mounting location on the ED Connect the reference electrode cable and the cell cable Reconnect the cell inlet and outlet fittings Condition the PdH reference electrode refer to the instructions below Conditioning the PdH Reference Electrode Condition the PdH reference electrode after plumbing the cell 1 On the Chromeleon 7ePanel Set or Chromeleon 6 8 panel tabset select the following settings a Pump panel Set the pump flow rate to 0 01 mL min This turns on the pump fl
400. upport for Dionex products for assistance The EGC control electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components cannot be serviced by the user 248 Doc 065342 06 12 11 8 EG Troubleshooting EG1 wrong cartridge error or EG2 wrong cartridge error This error occurs when an EGC is plugged into the EG that is not one of the supported types To troubleshoot Refer to Table 2 2 for a list of the supported EGC types for capillary and analytical IC systems The EG mode is off due to pump pressure alarm or leak This error occurs if the pump flow is turned off because of a pump pressure alarm or leak The EG is automatically turned off to prevent damage to the EG To troubleshoot Check the troubleshooting information for the pump in Section 8 14 and Section 8 15 The EG mode is off for a virtual pump This error occurs when a live EG is linked to a virtual pump and you try to turn on the EGC To prevent damage to the EGC the mode is automatically turned off to ensure that the EG does not operate when there is no flow EG mode will be turned off for invalid flow This error occurs when the flow to the EG is out of range or there is no pumped linked to the EG To troubleshoot 1 Set the flow rate to a value within the allowed range Refer to Appendix A for flow rate specifications Doc 065342 06 12 11 249 Dionex
401. ur application 2 Set EGC_2 Target Concentration to the concentration of KHCO3 required The K COs3 cartridge generates the total of the two target concentrations and the EPM modifies the total to achieve the K CO3 KHCO eluent mixture that you require For example For a 3 50 mM K C03 1 00 mM KHCO eluent set EGC_1 to 3 50 mM and EGC_2 to 1 00 mM The KCO cartridge generates 4 50 mM KCO indicated in the Applied Concentration field for the K CO3 EGC The EPM modifies the 4 50 mM KCO eluent to achieve the required 3 50 mM K C03 1 00 mM KHCO mixture 164 Doc 065342 06 12 11 meee DC Startup 4 11 Starting the DC 1 Press the POWER button on the front of the DC 2 Onthe Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the DC tab to display the DC panel see Figure 4 9 ICS 5000 Home Pump EG AS DC CD ED Audit Startup Queue Q conse Detector Compartment Compartment Column IC Cube 1 e Serial Number 123456789012 j dl j _ i oe Staue Head se poot se 000 C e se 50t gl aoua 0 Actual 30 00 Actual a500 ee e 39 10 Unknown CD_1 sE Unknown CD_1_Total Unknown Pump_1_Pressure Inj 2 LoadPosition Unknown Pump_2_Pressure spo Unknown ED Suppressor Unknown ED1_Total Type None v zz n 250 Mode Dif be Current OmA gt 0 Pump_1 Flow_detected 250 Suppressor 2 Type None v 500 Mode Oft v
402. ure 2 62 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 33 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 TC and is easily accessible CAUTION Doc 065342 06 12 11 119 Dionex ICS 5000 Operator s Manual 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 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 iden
403. urrent pressure is out of limits defined for the Warning page 281 column Current temperature is out of limits defined for Warning page 281 the column Data buffer overrun Abort page 281 Device control feature is not available Please Abort page 282 check key code and CM Features see About Chromeleon in the client s Help menu Device is not remote Abort page 282 Device not found on the USB Abort page 283 Either the current date is later than the Warning page 283 expiration date for x or the program or batch will end later than 24 hours before the expiration time for y Error deleting flash memory Abort page 283 Error during storing of the card data to the chip Error page 284 card Table 8 4 TC Error Messages Continued 210 Doc 065342 06 12 11 8 Troubleshooting TC Related Audit Trail Error Message Default Severity Level Error finishing download Abort page 277 Error programming flash memory Abort page 284 Executing this command will reset associated Warning page 284 counter values stored in the module Firmware download failed Abort page 285 Firmware download in progress Please wait Error page 285 Gas leak detected Error page 285 Humidity leak detected Error page 285 Illegal parameter Abort page 286 Invalid date time format Either use DD MMM Error page 286 YYYY or current Nyear s Nmonth s Nday s Example
404. ut Connect for either normally open N O or normally closed N C Note Relays are capable of switching 2 A at 24 VDC TTL Output 1 332 Q pull up to 5 V 100 mA sink Ground TTL Output 1 332 Q pull up to 5 V 100 mA sink Ground Connector Position Pin Function 1 O Analog 2 o Det1 3 O Analog 4 o Det2 5 oll 5v 6 O Gnd 7 o NO 8 O COM Rly 1 9 Ol NC 10 O N o 11 O com Riy2 12 O n c 1 O rt cut 2 o Gnd 3 ILO TTL out 4 O Gnd 5 o TTL Int 6 O TTL In2 7 O TTL In3 8 O TTL n4 9 O TTL Ins 10 O TTL n6 11 O TTL in7 12 O TTL In8 TTL Input 1 Note TTL input functions are assigned in software TTL Input 2 TTL Input 3 TTL Input 4 TTL Input 5 TTL Input 6 TTL Input 7 TTL Input 8 Figure 2 32 Optional Rear Panel I O Connector Strips Doc 065342 06 12 11 83 Dionex ICS 5000 Operator s Manual 2 17 1 CAUTION I O Option Connections 1 Locate the twisted pair of wires P N 043598 and 12 sa I Position 1 position connector plugs tock P N 923686 see DARI Figure 2 33 provided with the T O option board Position 12 Figure 2 33 12 Position Connector Plug 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 l
405. valid ion count Abort page 246 EG2 invalid ion count EG1 invalid serial number Abort page 247 EG2 invalid serial number EG1 over current Abort page 247 EG2 over current EG1 over power Abort page 248 EG2 over power EG1 over voltage Abort page 248 EG2 over voltage EG1 wrong cartridge error Abort page 249 EG2 wrong cartridge error The EG mode is off due to pump pressure alarm Abort page 249 or leak The EG mode is off for a virtual pump Warning page 249 EG mode will be turned off for invalid flow Warning page 249 Table 8 2 EG Error Messages Continued 206 Doc 065342 06 12 11 8 Troubleshooting EG Related Audit Trail Error Message Default Severity Level EG mode will be turned off for invalid flow Flow Abort page 250 range for analytical EGC 0 100 3 000 mL min capillary EGC 0 001 0 100 mL min EGC 1 is not linked to a compatible pump Warning page 250 EGC 2 is not linked to a compatible pump EGC cannot be used due to invalid ion count Abort can t page 251 be changed EGC is either not installed or invalid cartridge Abort page 251 number Please install a capillary EGC EGC is either not installed or invalid cartridge Abort page 251 number Please install an analytical EGC EGC is either not installed or invalid cartridge Abort page 252 number Please install an EGC Leak sensor wet Warning page 252 pH modifier must be used with
406. ve LOAD POSITION INJECT POSITION To Waste To Waste Sample In Sample In 1 To Column To Column From Pump From Pump Eluent Sample Figure 2 64 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 122 Doc 065342 06 12 11 2 TC Description 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 1 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 65 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 Pumpin 7 Firas To Waste Sample In Carrier Pump In Sample In N Carrier Pump In To Wast
407. vided on the Thermo Scientific Reference Library DVD P N 053891 for instructions If this does not eliminate the problem replace the column Doc 065342 06 12 11 233 Dionex ICS 5000 Operator s Manual 4 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 Technical Support for Dionex products 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 Thermo Fisher Scientific 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 Inspect the tubing for blockage or crimping replace as needed see Section 9 3 Be careful not to overtighten fittings 2 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 On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset set the Flow rate to 0 01 mL min for a capillary IC system or 1 0 mL min for an analytical IC system and r
408. w 328 Doc 065342 06 12 11 9 DP SP Service 9 10 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 when the valve is closed 1 Turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following e Disconnect the pump from the software by clicking Connected on the Pump panel e Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump Open the front door of the DP SP Five red Phillips screws are installed on the component mounting panel before shipment from the factory Remove these screws if present Use the handles on the component mounting panel to pull the panel forward until it reaches the stop The priming valve knob is located on the secondary pump head see Figure 9 11 To remove the knob turn it counterclockwise all the way and then pull it straight off the pump head PUMF 7 1 Priming Valve Secondary Pump Head Figure 9 11 DP SP Priming Valve Doc 065342 06 12 11 329 Dionex ICS 5000 Operator s Manual 7 Pull the old seal off the end of the priming valve knob 8 Hold the new seal P N 063382 with the groove in the priming valve seal facing away from the knob see
409. with aqueous and reversed phase eluents safe from metal contamination Doc 065342 06 12 11 1 Introduction e Carousel and moving needle design to guarantee reliable sampling from a variety of vial sizes and well plates e 10 mL polystyrene sample vials with wide openings for large volume injections and trace analysis e High sample capacity from 81 10 mL vials to 1152 three 384 position well plates e Sample preparation function to automate sample and standard preparations saving time and labor Optional features of the AS AP include sample tray temperature control simultaneous injections sequential injections sample preparation or fraction collection and reinjection and 6 port or 10 port valves Dionex AS DV Autosampler The AS DV is a basic autosampler that is capable of delivering between 0 1 and 5 0 mL of sample in 0 1 mL increments to the sample loop or concentrator column in an ion chromatography system The Dionex ICS 5000 holds 50 vials either 0 5 mL or 5 0 mL or a combination of the two sizes Vials can be sampled in any order and multiple samples can be taken from each vial The Dionex AS DV remembers the vial size and volume delivered for each vial position allowing multiple samples to be taken from a vial non sequentially Dionex AS Autosampler AS The AS is a powerful full featured autosampler that precisely delivers from 1 0 to 100 uL in 0 1 uL increments or 100 to 8000 uL in 1 uL increme
410. ystem release 6 8 SR9a or later Chromeleon 7 and Chromeleon 6 8 provide complete instrument control data acquisition and data management Optionally the Dionex ICS 5000 system can be controlled by a PC configured with Chromeleon Xpress Chromeleon Xpress provides real time control and monitoring of Dionex chromatography instruments but does not include data management capabilities In Chromeleon 7 an ePanel Set provides centralized system control You can use the ePanel Set to view system status information and issue commands for controlling each module In Chromeleon 6 8 these functions are available on a panel tabset In both the ePanel Set and the panel tabset a convenient Home panel shows the overall system status and provides basic module control functions Individual tabs provide quick access to additional functions for each module and detailed status and diagnostics functions Figure 1 2 shows Doc 065342 06 12 11 11 Dionex ICS 5000 Operator s Manual the Home panel in Chromeleon 7 and Figure 1 3 shows the Home panel in Chromeleon 6 8 Home CD Left Sampler Pump EluentGenerator DC Audit Startup Queue Instrument_3 Injection Number Run Time Sequence Method 1000 i _ oil A 7504 oiin O soo Pump Top Wor 2504 oo of 0 000 ml min it Ops R 250 q Ji Pump Bottom si mo 4 7804 joo sie 0 000 ml min oooie _
411. ytical Drip Tray Slide Release Latch 0 0 O Figure 2 10 Example EG Interior Components for an Analytical IC System System 2 of a Dual Channel EG Shown 40 Doc 065342 06 12 11 2 EG Description Eluent Generator Cartridge EGC Table 2 2 lists the versions of eluent generator cartridges available for use with the EG Each EGC contains an electrolyte concentrate solution appropriate for the particular eluent generation Each EGC is designed to be used in either a capillary IC system or an analytical IC system An EGC designed for a capillary IC system cannot be used in an analytical IC system and vice versa Analytical IC systems require EGC III cartridges and if used the EPM III Le Electrolytic pH Modifier Previous versions of EGC or EPM are not compatible with the Dionex ICS 5000 Eluent Generator EGC Version Part Function Number Eluent Generator Cartridges for Capillary IC Systems EGC KOH Capillary 072076 Generates potassium hydroxide eluent for anion exchange separations EGC MSA Capillary 072077 Generates methanesulfonic acid eluent for cation exchange separations Eluent Generator Cartridges and Accessories for Analytical IC Systems EGC III K2C03 074536 Generates potassium carbonate eluent for anion exchange separations EPM III Electrolytic 080135 Produces a carbonate bicarbonate pH Modifier mixture when installed with the EGC III K5C03 Requires a carbonate

ICS-5000 Ion Chromatography System Operator`s Manual

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