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Dionex ICS-5000+ Ion Chromatography System Operator`s Manual

1. EGC VENT Ce EGC RFIC Eluent y Degasser To Waste via EG Veni rear wall Eluent Eluent Out In Inlet Outlet EGC To IN Waste TO PUMP si val rear wal OUT Coupler TO INJ VALVE P Coupler TO SRS AES REGEN OUT WASTE GAS qa REGEN OUT SEPARATOR blue label DI CRTC Figure 2 15 EG Flow Schematic Example for Standard Pressure Analytical IC 52 Doc 065446 01 11 12 2 EG Description EGC VENT RFIC EGC Eluent Degasser To Waste via EG rear wall Inlet f i Outlet EGC EGC TO PUMP IN OUT TO INJ VALVE P TO SRS AES REGEN OUT WASTE GAS 1 SEPARATOR To Waste via EG rear wall Coupler Figure 2 16 EG Flow Schematic Example for High Pressure Analytical IC NOTE Refer to the Dionex EGC CO Mixer manual for a flow sche matic showing the components required to generate a carbon ate bicarbonate mixture The manual is provided on the Thermo Scientific Reference Library DVD P N 053891 Doc 065446 01 11 12 53 Dionex ICS 5000 Operator s Manual 54 Doc 065446 01 11 12 se 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 17 includes buttons for controlling certain DC functions as well as LEDs that indicate the
2. Pin Number Signal Name Signal Level Description 7 Relay 1 Out Potential free Common 8 Relay 2 Out Potential free Common 9 Gnd Ground Ground 10 Gnd Ground Ground 11 Gnd Ground Ground 12 Gnd Ground Ground se 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 17000 ee 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 Start 250 e Not used Table 2 2 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 Doc 065446 01 11 12 33 Dionex ICS 5000 Operator s Manual 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 l 2 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset Pr
3. IC Cube 1 heater over safe temperature Error page 270 IC Cube 2 heater over safe temperature Lower door opened Warning page 271 Lower leak sensor wet Warning page 271 Reaction coil open circuit Abort page 271 Reaction coil over safe temperature Abort page 272 Suppressor over current Abort page 272 Suppressor over power Abort page 272 Suppressor over voltage Abort page 273 Suppressor stopped for flow rate Warning page 273 Upper door opened Warning page 273 Table 8 3 DC Error Messages Continued 212 Doc 065446 01 11 12 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 see the page indicated in the table TC Related Audit Trail Error Message Default Severity Level AcqOff without previous AcqOn Error page 279 Acquisition is still on at program end Error page 279 All samples scheduled for run on timebases x Error page 279 need to specify the same value for property nominal Temperature All samples scheduled for run on timebases x Error page 279 need to specify the same value for property TempCtrl All samples scheduled for run on timebases x Error page 280 need to specify the same value for property y Can t execute Disconnect command during Warning page 280 data acquisition Can t execute Standby command during data Warning page
4. 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 438 Doc 065446 01 11 12 ka TC 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 50 C and 50 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 optional Exchangers Leak Detection Humidity and vapor sensors TTL and Relay Inputs Two digital inputs outputs and Outputs Two relay outputs Control Chromeleon Chromatography Data System requires Microsoft Windows 7 Windows Vista or Windows XP 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 h x w x d Doc 065446 01 11 12 439 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Thermal Compartment Specifications
5. TTL_Input_1 TTL_Input_2 TTL_Input_3 TTL_Input_4 TTL_Input_5 TTL_Input_6 TTL_Input_ Description TTL Input 1 TTL Input 2 TTL Input 3 TTL Input 4 TTL Input 5 TTL Input 6 TTL Input 7 Deactivate check boxes to remove unused devices Hit F2 to edit selection or double click it Low Pressure Valves Error Levels Cancel Appl Help Figure 2 39 DC Server Configuration Properties TTL Inputs 4 Select the name of the input and press the F2 key or double click the name 94 Doc 065446 01 11 12 2 DC Description 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 Injectalve_Right position 4 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 40 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 can send a signal to the input to trigger the selected functions 6 By default several functions are selected Scroll down the list and disable all unwanted functions TTL Input Control Types The DC T
6. 182 5 3 3 Loading Samples with a Vacuum Syringe Pull Method 183 5 4 Autosampler Commands for Loading and Injecting Samples 184 6 Shutdown DPISP Shutdown 5 2 sic ced ee ia ei pai 187 EG Shutdown sr scot o ctectin Beart Ria Sot eae Mea 189 6 1 Short term Shutdown LL 189 6 2 Long term Shutdown 0 00 cece eens 189 DC Shutdown che eds es Core eaten eee en eee tent 191 6 3 Consumables Storage 0 ccc eee es 191 6 4 ED Cell Storage tse hus it ne ei 191 6 4 1 ED Cell Short term Storage 191 vi Doc 065446 01 11 12 Contents 6 4 2 pH Ag AgcCI Reference Electrode Long term Storage 191 TC Shutdown oaea Raa Dda gi 193 6 5 Consumables Storage 0 cece eee ees 193 6 6 Short term Shutdown eit vie ken Pg ey eee 193 6 7 Long term Shutdown 0 0 0 cece een ees 193 7 Maintenance 7 1 System Maintenance Checklists LL 195 7 1 1 Daily Maintenance 00 cece eee ee 195 7 1 2 Weekly Maintenance 195 7 1 3 Periodic Maintenance LL 196 7 1 4 Annual Maintenance 00 0c eee ee eee 196 DP SP Routine Maintenance 199 7 2 DP SP Daily Maintenance 00 0 cee eee eee 199 7 3 DP SP Weekly Maintenance 0 000 c ec eee 199 7 4 DP SP Periodic Maintenance 00 0 eee eee eee 200 7 5 DP SP Annual Maintenance 2 0 00 e eee eee eee 200 EG Rout
7. Physical Dimensions 41 x 23 x 56 cm 16 x 8 75 x 21 5 in h xw xd Weight DP 24 1 kg 55 Ib SP 20 4 kg 45 Ib Flow Path All polymeric PEEK anion or cation configuration Environmental Operating Temperature 4 40 C 40 104 F Operating Humidity 5 95 relative humidity noncondensing Doc 065446 01 11 12 423 Dionex ICS 5000 Operator s Manual 424 Doc 065446 01 11 12 oa EG Specifications Dionex ICS 5000 Eluent Generator Specifications Minimum and Maximum Eluent Concentrations Analytical 0 1 100 mM Capillary 0 1 200 mM Flow Rates Analytical 0 100 3 000 mL min Capillary 0 001 0 030 mL min Eluent Types Standard Pressure KOH LiOH NaOH Carbonate Analytical Carbonate Bicarbonate Carbonate with pH modifier MSA Eluent Types KOH High Pressure MSA Analytical Eluent Types KOH Capillary MSA Maximum Operating Pressure 35 MPa 5000 psi 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 Dionex RFIC Eluent Degasser Analytical Eluent degasser housed in the EG module System Software Software Chromeleon Chromatography Data System
8. Mixer To waste Mae Piston lal B Seal la cD Wash lo na AQ _ Oz 9 Mixer toe Gc A Y To waste _ _ EGC RFIC standard Eluent Degasser pressure In Out Of Out Eluent CR TC Figure 3 8 Analytical IC Single RFIC EG System with Matrix Elimination Using a DP and a 6 Port Valve Doc 065446 01 11 12 143 Dionex ICS 5000 Operator s Manual To pump 2 inlet via the pump rear chase T 1 inlet A via thi n Pump front view Injection Valve io pump inlet via the pump rear chase DP a Connections Key a sed a Wash aq Concentrator Pump 3 Ya To column E Pump 2 DI Sample in Eluent in I pump not to scale Carrier pump in To waste Deionized Deionized y Pump 1 Water Water carrier From the suppressor Regen Out via the DC rear chase ss To waste DC front view EG left side view EGC RFIC standard Eluent Degasser pressure Cell In Cell Out Eluent 4 Eluent Out Y Vr In Waste Regen Q Eluei i In Regenin Buen CR TC Concentrator AY To the CR TC Regen RAUL EG rear chase i x Backpressure Device From AS AP N ima P lt 4 Large Loop To AS AP Waste To Waste Gil 144 Figure 3 9 Analytical IC Single RFIC EG System with Matrix Elimination Using an SP and a 10 Port Valve Doc 065446 01 11 12 3 Configurations To pump 2 inlet via the pump rear chase
9. 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 Ina To e be A A Piston pa B Seal o c Deionized aa a Deionized To the Pump 1 Water Reagent Water absorbance Regen or PDA detector 109 Y oO Oc de From the suppressor Regen Out via the DC rear chases we ee To waste DC front view EG plug 4 left side view Reagent in bod YS s fr 2 from pump p P A f RCH 1 D 4 x Ee To waste ul RFIC Eluent Degasser EGC standard pressure Eluent y Vio A Eluent Out In Waste i i Separator mH S L gt Osea th Y W C 6 3 N Backpressure Fi Si ac From ASAP ML Pe Device To the CR TC Regen In via the EG rear chase To AS AP Waste lt lt gr 4 To Waste Figure 3 10 Analytical IC Single RFIC EG System with Post Column Reagent Addition Bromate Doc 065446 01 11 12 145 Dionex ICS 5000 Operator s Manual Pump front view Seal Wash Pump To the pump inlet via the pump rear chase SP pump not to scale na Deionized Water f b i N A PONEO t Ballast i Bottle To the i VP j To waste Sd DC front view a 3 left side view 3 Q P 3 EGC RFIC amp standard Eluent Degass
10. The data format stored on the chip card is Error page 297 unsupported format version x The injections limit for the column has been Warning page 298 exceeded The injections limit will be exceeded for the Warning page 298 column x The nominal temperature must be set within the Error page 298 current limits The nominal temperature value is out of range Error page 298 defined by the active column ID The oven is not fully operable yet Check the Error page 298 values of Standby Ready Door and CardState The primary column ID property x will be Warning page 299 changed The property can t be changed in the future The upper limit must be higher than the lower Error page 299 limit The Warning threshold must be higher than the Error page 300 Limit threshold The Warning threshold must be lower than the Error page 300 Limit threshold There was already an AcqOff command for this Warning page 300 channel before There was already an AcqOn command for this Warning page 300 channel before This function cannot be adjusted by the user Abort page 301 This operation may affect the oven s operation Warning page 301 on timebase x which is currently running a batch Table 8 4 TC Error Messages Continued Doc 065446 01 11 12 217 Dionex ICS 5000 Operator s Manual TC Related Audit Trail Error Message Default Severity Level Two AcqOn commands fo
11. Doc 065446 01 11 12 309 Dionex ICS 5000 Operator s Manual 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 Dionex EGC or injection valve High pressure 10 32 Blue 074373 Use with high pressure fitting ferrule double cone bolts 10 32 fitting bolt Blue 074449 All other tubing fittings 10 32 ferrule double Blue 074373 cone Table 9 1 DP SPTubing and Fittings Continued Notes e For tightening requirements for the high pressure 10 32 fitting bolt P N 074449 and 10 32 double cone 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 that 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 for details 310 Doc 065446 01 11 12 9 DP SP Service 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 a
12. EG Related Audit Trail Error Message Default Severity Level Concentration out of range The maximum value Error page 245 at time 1 is 2 Concentration out of range The maximum value Error page 245 is 1 CR TC1 open circuit Abort page 245 CR TC2 open circuit CR TC1 over current Abort page 246 CR TC2 over current CR TC1 stopped because EGC1 OFF Abort page 246 CR TC2 stopped because EGC2 OFF CR TC1 stopped due to zero flow Abort page 247 CR TC2 stopped due to zero flow The CR TC mode is off for a virtual pump Abort page 247 CR TC mode will be turned off for invalid flow Abort page 247 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 248 capillary EGC Table 8 2 EG Error Messages Doc 065446 01 11 12 209 Dionex ICS 5000 Operator s Manual EG Related Audit Trail Error Message Default Severity Level Current linked pump is analytical Please install Abort page 248 an analytical EGC EG1 cartridge disconnected Abort page 248 EG2 cartridge disconnected EG1 invalid activation date Abort page 249 EG2 invalid activation date EG1 invalid concentration Abort page 249 EG2 invalid concentration EG1 invalid flow Abort page 249 EG2 invalid flow EG1 invalid flow rate concentration Abort page 250 EG2 invalid flow rate concentrati
13. Figure 2 34 Optional Rear Panel I O Connector Strips 86 Doc 065446 01 11 12 2 DC Description 2 17 1 CAUTION I O Option Connections l Locate the twisted pair of wires P N 043598 and 12 ae I Position 1 position connector plugs ua P N 923686 see 2 Figure 2 35 provided with the T O option board Position 12 Figure 2 35 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 locations See Figure 2 34 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
14. Anions a 2 2 None A 2 RA2 3 None A 3 RAS 4 None Ba RA4 5 None As RAS 6 None Bs RBI 7 None 37 i Unknown RB2 25 0 25 0 25 0 25 0 25 0 25 0 AS12A Product AS12A Product AS12A Product AS12A Product AS12A Product AS124 Product Balle cess Brenta UNO serre BEI o aa an usa 025 0 RA ctr Aia sir Volume ul Instrument Metho Processin Status AST2A Idle ASIZA Idle AS124 Idle AS124 Idle AS124 Idle ASIZA Idle 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 Select the sequence from the list and click Open The sequence is added to the Sequence table 3 Click Start Batch see Figure 5 7 33 Panel Tabset1 ICS 5000 23 Home Sequence Control Status Gradient Pumps Eluent Generator Detector Compartment AS DV Cond Detector System Log Audit Trail 9 33 45 AM Manually acquired samples will be stored temporarily in sequence SEQ AMARQUARDT2_locallCS S000 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 control over timebase ICS 5000 Run Time Elapsed Create Program Create Sequence 20 0 00 Continue Pump_1_Pressure Pump_2_Pressure 0
15. 0 c eee cence 228 8 10 Low Detector Output 228 viii Doc 065446 01 11 12 Contents 8 11 High Background 0 0 teens 229 DP SP Troubleshooting 231 8 12 Troubleshooting DP SP Error Messages 231 8 13 DP SP Does Not Start 239 8 14 DP SP Stops Unexpectedly cee 240 8 15 DP SP Liquid Leaks Leak Alarm 241 8 16 Vacuum Degassing Module Low Vacuum 4 242 8 17 Vacuum Degassing Module Does Not Run 242 8 18 DP SP Digital I O Port Inoperative 0 0 00 000 243 EG Troubleshooting 245 8 19 Troubleshooting EG Error Messages 0 00 cece neces 245 8 20 EG ALARM LED Is Lighted iii 257 8 21 EG POWER LED Fails to Light 0 00 0 c ee eee 258 8 22 Liquid Leaks in the EG 258 8 23 UNO FIOW raed stent aia 8S a en te ee a 259 8 24 EG Stops Operation LL 260 DC Troubleshooting 0 eee eee 263 8 25 Troubleshooting DC Error Messages 00 cece 263 8 26 Liquid Leaks from DC Components 2 0000 274 8 27 VALVE Button Not Working 275 8 28 ED Cell Troubleshooting LL 275 8 28 1 ED Cell pH Readout Always 7 0 275 8 28 2 Cannot Set ED Cell pH Readout to 7 0 276 8 28 3 Shift in ED Cell pH Readout 276 Doc 065446 01 11 12 ix Dionex ICS 5000
16. 8 Disconnect the tubing connections from the inlet and outlet check valves 9 Usinga 1 2 inch open end wrench loosen both check valve assemblies 10 Remove both check valve assemblies from the pump head 316 Doc 065446 01 11 12 9 DP SP Service 9 6 2 Installing the New Check Valves 1 The inlet check valve assembly ZS housing has a 1 4 28 port Inlet Check Valve 1 4 28 Port Inspect the new inlet 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 2 The outlet check valve assembly a housing has a smaller 10 32 port ff Outlet Check Valve 10 32 Port Inspect the new outlet check valve Single hole assembly to verify that fhe single ouia creck 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 Doc 065446 01 11 12 317 Dionex ICS 5000 Operator s Manual 6 NOTE The pump cannot operate properly unless the car tridges are installed in their respective housings in the correct orientation Liquid enters the check valve through the large single hole and exits throu
17. Flow Rate Accuracy lt 0 1 at 14 MPa 2000 psi Pressure Ripple Analytical lt 1 0 at 1 0 mL min typical Capillary lt 0 2 with damper or lt 1 0 without damper at 10 uL min Pressure None required Vacuum Degasser Integrated degasser with 1 channel for isocratic pump or 4 channels for quaternary pump optional Piston Seal Wash Automatic operation standard Gradient Formation Quaternary low pressure Analytical only or electrolytic eluent generation at high pressure Analytical and Capillary RFIC EG Gradients Analytical 0 1 100 mM Capillary 0 1 200 mM Gradient Profiles Any combination of an unlimited number of linear convex and concave positive and negative gradient profiles Doc 065446 01 11 12 421 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Single Pump Dual Pump Specifications Continued 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 Eluent generation RFIC EG optional Eluent On Off Valve Electrically actuated standard Leak Sensor Optical standard System Software Software Chromeleon Chromatography Data System requires Microsoft Windows 7 Windows Vista or Windows XP Automated Procedure Wizards Standard feature Sys
18. Data Trending All detector numerical parameters System Status Virtual Channels Standard feature Power Failure Protection Standard feature System Trigger Commands and Conditionals Standard feature Daily Audit Trail Standard feature Sample Audit Trail Standard feature System Calibration Storage Factory present and previous completely user settable Customized Reporting Standard feature with unlimited report workbooks GLP Compliance Optional package provides security system modification history and electronic signatures 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 065446 01 11 12 435 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 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 n
19. LOAD POSITION Loop Loading Concentrator To Column Eluent INJECT POSITION Concentrator Loading Concentrator To Column Eluent e Pump In ppi Pump In Large Large L Loop INR Loop NI AJ eo To Waste GL OO renali A To Waste AU I Sample Vv z Sample y In Carrier In Carrier To Waste Pumpin To Waste Pumpin Sample Eluent se Carrier Figure 2 28 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 28 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 Doc 065446 01 11 12 71 Dionex ICS 5000 Operator s Manual 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
20. TO INJ VALVE C Red microbore Black standard bore Injection Valve Plumbing 6 Port Valve 8 Turn on 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 Ifthe valve electronics require service contact Thermo Fisher Scientific Electronics related repair procedures must be performed by a Technical Support Representative for Dionex products NOTE Substitution of non Dionex Thermo Scientific parts may impair valve performance and void the product warranty Doc 065446 01 11 12 417 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT Turn off the pump flow from the ePanel in Chromeleon 7 or the Control panel inChromeleon 6 8 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 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 Open the TC door Disconnect each liquid line connected to the valve
21. Verify that the current to the Dionex EGC and the suppressor is off Supplying power to the Dionex EGC when there is no eluent flow can severely damage the cartridge If you plan to store the Dionex 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 Dionex EGC from the EG and the instructions in Section 9 14 3 to store the Dionex EGC To restart the EG 1 5 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 Condition the Dionex EGC For instructions see Conditioning the Capillary EGC on page 346 or Conditioning the Analytical EGC on page 352 Hydrate the Dionex CR TC see Installing and Flushing the New CR TC on page 355 Hydrate the suppressor as instructed in the product manual Suppressor manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 Let the system equilibrate before collecting data Before shipping the EG 1 Follow the instructions in Section 9 14 1 to remove the Dionex EGC from the EG Plug all fittings Tighten the vent fitting capillary Dionex EGC or high pressure analytical Dionex EGC or cap the vent port standard pressure analytical Dionex EGC This will prevent the evaporation of
22. 2 Use a wrench to unscrew the PdH reference electrode nut and then remove the nut from the reference electrode well see Figure 9 67 Figure 9 67 Unscrewing the PdH Reference Electrode Nut 3 Pull the reference electrode out of the well see Figure 9 68 PdH Reference Electrode Figure 9 68 Removing the PdH Reference Electrode from the Reference Electrode Well 408 Doc 065446 01 11 12 9 DC Service 4 Using tweezers remove the PdH reference electrode gasket from the well see Figure 9 69 PdH Reference Electrode Gasket Figure 9 69 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 70 To avoid deforming the gasket cutout do not place the tweezer tips on the cutout Cutout DA PdH Reference Electrode Gasket 4 Figure 9 70 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 then press the gasket into the well Doc 065446 01 11 12 409 Dionex ICS 5000 Operator s Manual 7 9 10 To avoid any hydraulic pressure buildup when inserting the reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings Align the fitting on the end of the PdH reference electrode so that the knobs
23. A DC Specifications Dionex ICS 5000 Detector Chromatography Compartment Specifica tions Continued Electrolytic Suppression Self Regenerating 0 4 mm with optional IC Cube 2 mm and 4 mm 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 4 mm 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 Dionex AMMS ICE Available in 2 mm and 4 mm versions Carbonic Acid Removal for Anions Dionex ASRS and Dionex AMMS plus Dionex CRD 300 for 2 mm and 4 mm versions Dionex CRD 0 4 mm for capillary suppressors Suppression Capacities Dionex Suppressors Anion SRS 300 4 mm 200 peg min Cation SRS 300 4 mm 110 peg min Anion SRS 300 2 mm 50 peg 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 Doc 065446 01 11 12 431 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Detector Chromatography Compartment Sp
24. Fr a Re a ae rorro _ rrnr __r ro rr _ n os 1038 10 50 O75 1100 1128 1150 1138 1200 1225 1220 1276 1200 19 28 na 12 76 1399 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 baseline Chromeleon can calculate a baseline I t plot for each data point of a peak Each I t plot measured at a given retention time can be corrected by subtracting the calculated baseline I t plot from the 3D amperometry data By definition if baseline correction is enabled 3D amperometry data is zero unless a peak is present To enable baseline correction select Baseline correction on the General tab page of the 3D Amperometry Decoration dialog box Doc 065446 01 11 12 117 Dionex ICS 5000 Operator s Manual 118 Doc 065446 01 11 12 ka 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 insid
25. 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 82 Doc 065446 01 11 12 2 DC Description 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 16 DC Rear Panel Figure 2 33 illustrates the rear panel of the DC Gre lai TITTI MINI Ee IAT oe TIKI III ITITTITTIKMKI Seni MW TT beve HERE 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 O88 Figure 2 33 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 Doc 065446 01 11 12 83 Dionex ICS 5000 Operator s Manual CAUTION Switched AC Sockets The two AC receptacles can be used to control the power to external devices Use Chromeleon to switch the pow
26. N Nite ta ESS ku Re are highty A Figure 9 15 Capillary Dionex EGC Vent Fitting If you are removing a standard pressure analytical Dionex EGC a Remove the VENT line EGC from the Dionex EGC by Vent Line unscrewing the 10 32 luer fuer adapter see Figure 9 16 Adaptor NOTE If necessary use a wrench to hold the luer adapter in place while unscrewing the vent line Figure 9 16 Analytical Dionex EGC Vent Line Standard Pressure Cartridge Shown b Locate the 10 32 plug P N 053981 removed from the Dionex EGC vent opening during installation Install the plug in the vent opening If you are removing a high pressure analytical Dionex EGC tighten the vent fitting in the top of the Dionex EGC 6 Lift the Dionex EGC straight up and off the cartridge holder 340 Doc 065446 01 11 12 9 EG Service 7 Turn the Dionex EGC upside down and place it on the EG drip tray see Figure 9 17 This is the service position for the cartridge EGC Standard Pressure Analytical EGC High Pressure Analytical Drip Tray Figure 9 17 Dionex EGC Service Position 8 Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET ports on the Dionex EGC 9 14 2 Disposing of the Old EGC If the Dionex EGC is expended follow these steps to dispose of it 1 Hold the cartridge with the eluent generation chamber see Figure 9 17 on top Unscrew the eluent generation chamber from the ele
27. PdH reference electrode 072214 Gasket for PdH reference electrode 079850 ED gold conventional working electrode with gasket and polishing kit 079851 ED platinum conventional working electrode with gasket and polishing kit 079854 ED glassy carbon conventional working electrode with gasket and polishing kit 448 Doc 065446 01 11 12 B DC Reordering Information Part Number Item 079856 ED silver conventional working electrode with gasket and polishing kit 045972 Gasket PTFE 0 001 in for conventional working electrode 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 f
28. e Dionex CR TC ELUENT OUT to EG degas ELUENT IN High pressure 10 32 Blue 074373 Use with high pressure fitting ferrule double cone bolts Table 9 3 Tubing and Fittings for a Capillary IC EG Channel Continued e Notes for capillary IC channels e Do not cut the 0 062 mm 0 0025 in ID blue PEEK tubing used for capillary IC connections To ensure good chromatographic results this tubing must be cut at the factory using a specialized precision cutter If you need to replace any tubing of this type order the appropriate precision cut tubing assembly listed in Table 9 3 e When replacing capillary tubing make sure the 10 32 fitting bolt P N 074449 and 10 32 double cone ferrule P N 074373 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 10 32 fitting bolt P N 074449 and 10 32 double cone ferrule P N 074373 see Section 9 2 336 Doc 065446 01 11 12 9 EG Service gg 9122 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 Dionex EGC to pump PEEK tubing 1 in e Dionex EGC to Dio
29. 0 0025 in ID H PEEK Tubing Assembly EGC P N 072204 OUT ELUENT IN wea TO PUMP DAMPER p To Waste Ea 1 58 mm 0 062 in ID ETFE Tubing Assembly P N 072225 0 25 mm 0 010 in ID PEEK Tubing Temporary connection Figure 9 27 Plumbing for Hydrating a Capillary Dionex CR TC 356 Doc 065446 01 11 12 9 EG Service 3 Ifyouare installing a Dionex CR TC in an analytical IC system IC Locate the CR TC Hydration Tubing Kit P N 063487 provided in the EG Ship Kit b Referto Figure 9 28 to plumb the four ports on the Dionex CR TC a From EGC Out Port Analytical CR TC Flushing Pump at application flow rate To Waste lt for 10 min CR TC Hydration Kit Tubing Assembly P N 063487 Temporary connection Figure 9 28 Plumbing for Hydrating an Analytical Dionex 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 Dionex 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 Doc 065446 01 11 12 357 Dionex ICS 5000 Operator s Manual e Analytical pumps Set the flow rate recommended for your application This turns on the pump flow als
30. 031759 the flier shipped with the suppressor NOTE Instructions for the pressure test are in the suppressor manual also Suppressor manuals are provided on the Thermo Scien tific Reference Library DVD P N 053891 3 Ifabubble 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 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 53 Doc 065446 01 11 12 391 Dionex ICS 5000 Operator s Manual NOTE Fora capillary IC system disconnect the cell inlet line from the ELUENT OUT port of the IC Cube column cartridge Cables Inlet Line Outlet line Figure 9 53 Disconnecting the ED Cell Cell configured for analytical IC shown 4 Grasp the cell by the cell body and pull straight out to remove it from the detector 392 Doc 065446 01 11 12 9 DC Service 9 28 2 Replacing an ED Cell Disposable
31. 065446 01 11 12 349 Dionex ICS 5000 Operator s Manual 3 Turn the cartridge upside down and place it on the EG drip tray in the service position see Figure 9 16 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 Dionex 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 075780 7 Connect one end of the backpressure coil to the Dionex EGC OUTLET port leave the other end of the coil unconnected see Figure 9 24 This is a temporary connection Figure 9 24 Dionex EGC Outlet Connection for Cartridge Conditioning Standard Pressure Analytical Cartridge Shown 8 While holding the Dionex 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 350 Doc 065446 01 11 12 9 EG Service 9 Slide the Dionex EGC with the electrolyte reservoir on top into the holder in the EG see Figure 9 25 EGC Standard Pressure Analytical EGC High Pressure Analytical hae A Figure 9 25 Analytical Dionex EGC Installed in Holder 10 Remove the 10 32 plug standard pressure analytical Dionex EGC or fitting high pressure analytical Dionex EGC from the vent opening and install a 10 32 luer
32. 3 IC Cube System 2 Conductivity Detector Conductivity Detector 2 Capillary System 1 4 Capillary System 2 Figure 2 19 Example DC Interior View Upper Compartment of a Dual IC System Shown ey 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 AM can not 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 065446 01 11 12 59 Dionex ICS 5000 Operator s Manual Cartridges for the following components are available carbonate removal device Dionex CRD suppressor guard and separator columns and EG degasser NOTE Ifthe IC Cube does not include a Dionex CRD or suppressor bypass cartridges must be installed Bypass cartridges pro vide the internal plumbing connections required for eluent and regenerant flow between IC Cube components Figure 2 20 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 Injectio
33. 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 182 Doc 065446 01 11 12 5 Operation Loading Samples with a Syringe Push Method l 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 to the sample port on the injection valve If not see 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 several 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 bef
34. 500 psi Table 9 5 EG Backpressure Coils 362 Doc 065446 01 11 12 9 EG Service 9 18 DANGER DANGER ACHTUNG Changing the EG Main Power Fuses l 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 13 Disconnect the main power cord from both its source and from the EG rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the EG HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du EG HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des EG The fuse drawer is located above the main power switch see Figure 9 31 A small 5 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 31 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 065446 01 11 12 363 Dionex ICS 5000 Operator s Manual 364 Doc 065446
35. AM Components Available Separately 98 Doc 065446 01 11 12 2 DC Description gg 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 075917 and 10 port P N 075918 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 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 See Chapter 3 for the configuration schematic for your application Valves are controlled by Chromeleon see Section 2 18 3 Doc 065446 01 11 12 99 Analytical IC Dionex ICS 5000 Operator s Manual 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 2 44 OFF POSITION konf 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 p
36. Continued Weight 15 4 kg 34 Ib Environmental Operating Temperature 10 35 C 50 95 F Operating Humidity 5 80 relative noncondensing 440 Doc 065446 01 11 12 ICS 5000 DP SP B Reordering Information DP SP Reordering Information Part Number Item Pump Head Components 074447 capillary 075047 analytical Primary pump head 074444 capillary 075044 analytical Secondary pump head 044541 capillary 045722 analytical Inlet check valve assembly for primary pump head includes inlet nut and 1 8 in cartridge 044540 capillary 045721 analytical Outlet check valve assembly for primary pump head includes outlet nut and 1 8 in cartridge 075493 capillary 075768 analytical Main piston seal 074371 capillary 074370 analytical Backup ring 040695 O ring for capillary or analytical pump 074446 capillary 075767 analytical Seal wash body 068628 capillary 063382 analytical Piston seal wash seal 068627 capillary 062092 analytical Retainer for piston seal wash seal 068646 capillary 079857 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 065446 01 11 12 441 Dionex ICS 5000 Operator s Manual
37. Dionex ICS 5000 Operator s Manual Water deionized requirements 20 Water dip 154 Water samples 153 Waveform Editor 112 Waveforms 109 Cyclic voltammetry 109 Defining 112 Integrated amperometry 111 Integrated amperometry example 108 Maximum length 111 Pulsed amperometry example 107 Weekly maintenance DC 203 DP SP 199 EG 201 TC 205 Well plates 152 Filling 152 Wellness 133 Wireframe plot 116 Working electrodes 78 Maintenance 149 Materials 79 Polishing procedure 396 Z Zero position analog out 89 Index 20 Doc 065446 01 11 12
38. Operator s Manual 8 28 4 No ED Cell pH Readout or Intermittent Readout 277 8 28 5 Leak in pH Ag AgCl Reference Electrode Compartment 278 8 28 6 Shift in Ag AgCl Reference Potential 278 TC Troubleshooting 279 8 29 Troubleshooting TC Error Messages 000 20 eee 279 8 30 TC ALARM LED Is Lighted vue iat eet exile ade eis 303 8 31 Liquid Leaks from TC Components 0 000 e eee 304 8 32 TC Temperature Does Not Increase 305 8 33 TC Temperature Stabilizer Not Operating Properly 305 9 Service 9 1 Connecting Tubinga 307 9 2 Tightening Guidelines for High Pressure Fittings 308 DP SP Servite ingoio palo Lai 309 9 3 Replacing Tubing and Fittings cece ee eee 309 9 4 Cleaning Eluent Reservoirs 0 0 cc eects 311 9 5 Priming the DP SP 0 eee nes 311 9 5 1 Priming with the PUMP PRIME Button 312 9 5 2 Priming from the Chromeleon Panel 313 9 6 Replacing the Check Valves 0 0 ccc eee ees 315 9 6 1 Removing the Check Valves 0 0000 e eae 315 9 6 2 Installing the New Check Valves 317 9 7 Replacing Piston Seals 0 0 ccc cece ees 319 9 7 1 Removing the Pump Head and Piston 320 Doc 065446 01 11 12 Contents 9 7 2 Cleaning the Piston 323 9 7 3 Removing the Main Piston Seal 323
39. P N 079857 326 Doc 065446 01 11 12 9 DP SP Service Before beginning locate the 3 0 mm hex key P N 062338 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 ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 9 8 1 Removing the Pump Head and Piston When disassembling and reassembling the pump head see 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 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 Doc 065446 01 11 12 327 Dionex ICS 5000 Operator s Manual 9
40. Part Used to Connect Quantity Number Precision cut 0 062 mm 65mm 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 75mm 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 25 mm 0 010 in ID 914 mm 042696 Inject valve waste to PEEK tubing black 36 in Dionex AS AP waste port located near the injection port 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 column 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 Table 9 7 Contents of the IC Cube Tubing Kit P N 072186 366 Doc 065446 01 11 12 9 DC Service ey Notes for Capillary IC systems e The 0 062 mm 0 0025 in ID blue
41. Specifications Dual Temperature 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 for sample pre concentration All valves and heater upgradeable and field installable Doc 065446 01 11 12 429 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Detector Chromatography Compartment Specifica tions Continued 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 IC C
42. Three versions of Dionex EGC are available one for capillary IC systems one for analytical standard pressure IC systems and one for analytical high pressure IC systems The recommended maximum operating pressure for the EG in an analytical IC system is 35 MPa 5000 psi if a Dionex EGC 500 is installed or 21 MPa 3000 psi if a Dionex EGC 300 is installed Excessive backpressure may rupture the tubing inside the Dionex RFIC Eluent Degasser A Thermo Scientific Dionex Continuously Regenerated Trap Column Dionex CR TC to remove any extraneous contaminants from the deionized water source The Dionex CR TC is electrolytically regenerated which allows it to operate for extended periods without chemical regeneration The Dionex CR TC is available in two versions one for capillary IC systems and one for analytical IC systems A high pressure gas removal device that removes electrolysis gases created during eluent generation 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 nonstop operation RFIC ER uses carbonate carbonate bicarbonate or MSA methanesulfonic a
43. and deionized water that meets the specifications listed in Section 1 5 to prepare eluent and regenerant or to rinse eluent reservoirs 2 IfanEGisnotinstalled 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 3 Fill the reservoirs with prepared eluent or deionized water if an EG is installed 4 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 5 Install an end line filter on the end of each reservoir s eluent line 6 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 065446 01 11 12 159 Dionex ICS 5000 Operator s Manual NOTE A Dionex High Pressure Inline Filter P N 044105 can be used to remove particulates down to 0 45 micron from eluent Connect the inline filter between the pump outlet and the eluent inlet port on the inje
44. capillary EGC 0 001 0 100 mL min This error occurs when the flow to the Dionex CR TC is out of range or there is no pump linked to the Dionex EGC To troubleshoot 1 Set the flow rate to a value within the allowed range See Appendix A for flow rate specifications 2 Check the Dionex EGC configuration properties in the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program to verify that the pump and Dionex EGC are linked Doc 065446 01 11 12 247 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 Dionex EGC does not match the Dionex EGC type A capillary Dionex EGC can only be used with a capillary pump an analytical Dionex EGC can only be used with an analytical pump To troubleshoot 1 Install the correct type of Dionex EGC for the pump type 2 Fora hybrid system a dual system with both an analytical and a capillary pump check the Dionex EGC configuration properties in the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program to verify that the correct pump is linked to the Dionex EGC EG1 cartridge disconnected Or EG2 cartridge disconnected This error occurs if Chromeleon sends a command to set an EG parameter when th
45. 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 the 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 Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 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 282 Doc 065446 01 11 12 8 TC Troubleshooting 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
46. for assistance Doc 065446 01 11 12 285 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 select 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 instruments 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 required licenses Contact 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 286 Doc 065446 01 11 12 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
47. front view EG EG right side view Y left side view System 1 System 2 EGC standard pressure RFIC Eluent Degasser RFIC Eluent Degasser EGC standard pressure Cell In Cell Out Eluent Eluent Out y Vi Ain Out Eluent y Vi eae aseyo 93 au e uj UaBaY Z OL YO au OL Waste Waste N _ _ a To the degasser 2__ Regen am To inject valve 2 port P 2 ee oo Eluei Separator 2 A To the CR TC 1 In Separator 1 3 To inject sara wr Eluent ae valve 1 Regenn Su eau cRIC 6 Stabilizer T From ASAP ISS REJA P Toasapnaste pg S i ToAS APMWaste lt 4 Ee a To waste L 5 System 1 System 2 Figure 3 7 Analytical IC Dual RFIC EG System CD ED 142 Doc 065446 01 11 12 3 Configurations 6 3 Large Loop avs wo _ ISEWAY SY OL To inject valve sample port Cell In Cell Out Regen Out Eluent Out luent In Regen In lo pump 2 inlet via the pump rear chase To pump 1 inlet A via the pump rear chase Pump 2 pump not to scale Deionized Deionized Pump 1 Water Water carrier From the suppressor Regen Out nathe DC rear chase DC front view EG left side view Separator Backpressure Device Temp gt Stabilizer Wi di To AS AP Waste Pump front view DP
48. 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 Amperometry View window see Figure 2 57 To open the window 114 Doc 065446 01 11 12 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 Ble EGR Yew Workspace Qualification Window Help 2x OSU SHS REN PF ei E eA N T EAN E EEEN aren Ut ia Chromatogram Plot tne 5 Injection Data Mera lwaloht 100 l t Plot current vs waveform time Waveform Plot 1079741 10797410 na 125 na 7 727 man 210 00 me 74 ra 0 530 v Piarik 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
49. iii pr 24 2 2 2 Pressure Transducer e eee eee eee eee 25 2 2 3 Proportioning Valves Gradient pump only 25 2 2 4 Vacuum Degassing Module 0 00205 25 2 2 5 Piston Seal Wash System 26 Doc 065446 01 11 12 i Dionex ICS 5000 Operator s Manual 2 2 6 Static Mixer Analytical IC only 27 2 2 7 High Pressure Trap Column Analytical IC only 27 2 2 8 Pulse Damper Capillary IC only 28 2 3 DP SPFlow Schematics LL 29 2 3 1 Isocratic Pump Flow Schematic 45 29 2 3 2 Gradient Pump Flow Schematic 30 24 DP SPRearPanel pini ae Soe es oR oh Ra ed T 31 2 9 Eluent Reservoirs M stesso ei io ke BS RS abies i 35 2 5 1 EO Optional 0 0 ccs 35 2 5 2 Pressurizing Eluent Reservoirs 0 05 35 2 5 3 Filtering Eluent a piglia ah cand anki acd a ata 37 EG Description Freri vee ne a eon a ease ewer terse aes 39 2 6 EG Front Features one cenni e narea e a ees 39 2 7 EG Interior Components 40 2 8 EG Rear Panel oiie aee an le rta 48 2 9 EG Flow Schematics ss nengoa sanies cece eee eens 50 DC Description aris eahecg masa illa 55 2 10 DC Front Features r erocino iya aa po i pela 55 2 11 DC Interior Components 57 2 11 1 DC Interior Components for Capillary IC 58 2 11 2 IC Cube for Capillary IC 2 eee 59 2 11 3 DC Interior Components for Analytical IC 64 2 12 DC Temperature C
50. 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 Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 3 Under TC select the column name and select the FormatChipCard command 4 For Chromeleon 6 8 click Execute Doc 065446 01 11 12 297 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 displays an appropriate message shown above when the injections limit has been exceeded or is about to be 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 Temper
51. parameters especially apparent when operating at high sensitivities Allow a longer system equilibration time up to 2 hours before starting operation Doc 065446 01 11 12 219 Dionex ICS 5000 Operator s Manual Noisy Baseline CD Only Analytical IC PVE IC Incorrect suppressor operating conditions Refer to the suppressor manual for troubleshooting information Suppressor manuals are provided 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 provided 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 modes Air bubbles
52. see page 163 Set the pressure limits see page 164 OOaddaaqgqagdga If an EG is installed start the EG and set the eluent concentration see page 165 Start the DC see page 169 or TC see page 173 Equilibrate the system and verify operational readiness DC see page 170 TC see page 174 OO 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 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 152 Doc 065446 01 11 12 4 Startup 4 3 2 4 3 3 these can leave traces of ions on the container walls The ions may interfere with the analysis If samples will not be analyzed on the day they are collected filter them through clean 0 45 micron filters immediately after collection otherwise bacteria in the samples may cause the ionic concentrations to change over time Refrigerating the samples at 4 C 39 F will reduce but not eliminate ba
53. 0 22 Pump_1 C Value 0 0 23 Pump_1 D Value 0 0 Pump_1 Curve Figure 5 10 Commands for Loading and Injecting Sample with a Dionex AS DV 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 Doc 065446 01 11 12 185 Dionex ICS 5000 Operator s Manual 186 Doc 065446 01 11 12 6 Shutdown ICS 5000 a 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 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 th
54. 0 33 mm 0 013 in ID Blue 049714 Dionex AS AP sample PEEK tubing 1 in transfer line to injection valve or diverter valve 10 32 fitting bolt Blue 074449 Dionex AS AP sample 10 32 ferrule double Blue 074373 transfer line to injection cone valve or diverter valve 10 32 fitting bolt Black 062980 Dionex AS AP sample Split cone ferrule Black 062978 transfer line to injection port push modes 1 16 in flangeless fitting Tan 052230 Dionex AS AP sample bolt transfer line to needle pull Two piece ferrule Clear 062511 modes cone tan flat 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 074449 All other tubing fittings 10 32 ferrule double Tan 043276 cone Table 9 8 Tubing and Fittings for an Analytical IC DC System Doc 065446 01 11 12 9 DC Service 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 that 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 t
55. 0 Guard Column Guard Column Inlet Precision Cut Tubing Figure 9 43 Separator and Guard Columns Installed in Column Cartridge Figure 9 44 shows the column cartridge when only a capillary separator column is installed Separator Column Outlet Separator Column Separator Column Inlet Precision Cut Tubing oo 8 Figure 9 44 Separator Column Only Installed in Column Cartridge Doc 065446 01 11 12 381 Dionex ICS 5000 Operator s Manual 6 Remove the guard column if present and separator column from the column clips Lift up the separator column outlet fitting see Figure 9 45 slightly to free it from the clips and then slide it out of the cartridge 7 Remove the columns from the cartridge 8 Disconnect the tubing from the columns Save the tubing J n Figure 9 45 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 specialized 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 9 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 49 382 Doc 065446 01 11 12 9 DC Service 10 I
56. 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 Temperature 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 Analytical 0 7 uL Capillary 0 02 uL 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 7 Windows Vista or Windows XP Automated Procedure Wizards Standard feature Doc 065446 01 11 12 A DC Specifications Dionex ICS 5000 Conductivity Detector Specifications Continued System Smart Startup and Shutdown Standard feature System Wellness and Predictive Performance Standard feature Application Templates Standard feature Automation Support of Third Party Instruments Fully controls over 300 different instruments including GC HPLC and MS from more than 30 manufacturers Customizable System Control Panels Standard feature Signal Channels Conductivity total conductivity
57. 01 11 12 ICS 5000 esi DC Service 9 19 Replacing Tubing and Fittings Ea 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 0 33 mm 0 013 in ID Blue 049714 Dionex AS AP sample PEEK tubing 1 in transfer line to injection valve or diverter valve ED Cell Inlet Tubing Kit N A 074221 ED cell inlet to column outlet High pressure 10 32 Blue 074449 Dionex AS AP sample fitting bolt transfer line to injection High pressure 10 32 Blue 074373 valve or diverter valve ferrule double cone 10 32 fitting bolt Black 062980 Dionex AS AP sample Split cone ferrule Black 062978 transfer line to injection port push modes 1 16 in flangeless fitting Tan 052230 Dionex AS AP sample bolt transfer line to needle pull Two piece ferrule Clear 062511 modes cone tan flat High pressure 10 32 Blue 074449 Suppressor eluent out fitting bolt Dionex CRD eluent in High pressure 10 32 Blue 074373 CD cell inlet and outlet ferrule double cone ED cell outlet e Injection valve sample in and sample out Table 9 6 Tubing and Fittings for a Capillary IC DC System Doc 065446 01 11 12 365 Dionex ICS 5000 Operator s Manual Be Table 9 7 lists the tubing and fittings in the IC Cube Tubing Kit P N 072186 Part Length
58. 12 329 Dionex ICS 5000 Operator s Manual d Pullon the fitting slightly to remove the PharMed tubing from the upper notch on the pump mounting plate 006000 PharMed Tubing P N 063268 Rotor Lever Mounting Plate Tygon 2075 Tubing P N 064079 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 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 330 Doc 065446 01 11 12 9 DP SP Service 8 10 11 12 Connect the new tubing pieces to the seal wash reservoir and pump heads see Figure 9 10 Push the tubing onto the fitting that was removed in Step 5 Connect the PharMed tubing to the peristaltic pump as follows a Push the tubing into the lower notch on the pump mounting plate b Lift the lever to the right and hold it in that position with one hand c Wit
59. 280 acquisition Can t find download image TC3000 HEX Abort page 280 Can t start acquisition at negative retention Error page 281 times Can t start acquisition The server configuration Abort page 281 does not fulfill the license conditions Can t start TC firmware A firmware download Abort page 281 may be necessary Can t use device x as a source of the column Error page 282 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 065446 01 11 12 213 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 282 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 283 Command is not available in demo mode Abort page 283 Communication error x Abort page 283 Communication time out Abort page 284 Configuration doesn t match X not installed Warning page 284 Configuration mismatch x CM uses y Abort page 284 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 284 column Current pressure is out of li
60. 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 troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 Ifyou cannot identify the cause of the error contact Technical Support for Dionex products for assistance Doc 065446 01 11 12 283 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 Ifyou 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 Pr
61. 5000 Operator s Manual TEM 2 18 4 RCH 1 Reaction Coil Heater os The RCH 1 Reaction Coil Heater P N 079849 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 a Chromeleon 6 8 program S 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 Temperature 35 00 20 00 80 00 C O Wait Ready Off NA BAO sms Code sre nahn AL Anzi aR SANA th a ttt Aa AE to Am Bat artim rc py rn Mln nti 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 8 104 Doc 065446 01 11 12 2 DC Description 2 19 Electrochemical Detection Modes The Dionex ICS 5000 ED can perform the following electrochemical detection modes e DC amperometry see Section 2 19 1 e Integrated amperometry including pulsed amperometric detection PAD and integrated pulsed amperometric detection IPAD see Section 2 1
62. 7 ePanel or Chromeleon 6 8 Control panel 2 Turn off the Dionex ICS 5000 IC 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 If the 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 Dionex ICS 5000 IC system is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot See Appendix A for environmental specifications 270 Doc 065446 01 11 12 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 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 34 If liquid accumulates in the tray the sensor signals the problem and this error message appears To troubleshoot 1 Locate the sou
63. 9 7 4 Removing the Piston Seal Wash Seal 324 9 7 5 Installing the Piston Seals and O Ring 324 9 7 6 Reinstalling the Piston and Pump Head 326 9 8 Replacing the Piston 326 9 8 1 Removing the Pump Head and Piston 327 9 8 2 Installing the New Piston 328 9 8 3 Reinstalling the Pump Head 00055 328 9 9 Replacing the Piston Seal Wash Tubing 004 329 9 10 Replacing the DP SP Priming Valve Knob Seal 332 9 11 Changing the DP SP Main Power Fuses 5 333 EG SCIVICEs ici I a eae aaa 335 9 12 Replacing Tubing and Fittings LL 335 9 12 1 Tubing and Fittings for Capillary IC EG Channels 335 9 12 2 Tubing and Fittings for Analytical IC EG Channels 337 9 13 Isolating a Restriction in the Liquid Lines 338 9 14 Replacing the EGC cen ees 338 9 14 1 Removing the Old EGC 0 00 339 9 14 2 Disposing of the Old EGC 0 0 0 cee eee 341 9 14 3 Storing the Old EGC 0 eee 342 9 14 4 Installing and Conditioning a New Capillary EGC 343 9 14 5 Installing and Conditioning a New Analytical EGC 347 Doc 065446 01 11 12 xi Dionex ICS 5000 Operator s Manual 9 15 Replacing the CR TC ene es 354 9 15 1 Removing the Old CR TC 00 00 0020 354 9 15 2 Installing and Flushing the New CR TC 355 9 15 3 Completing the
64. Chromeleon 7 or the Commands dialog box Chromeleon 6 8 You can access all commands available for the system from here Doc 065446 01 11 12 175 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 reports NOTE A Virtual Column Separation Simulator is available in Chromeleon that can help you determine the best oper ating parameters column eluent flow rate and tem perature for a partic
65. Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab 2 Gradient pump only Enter 100 for the channel A B C or D to be primed 3 Select the priming flow 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 4 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 5 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 runvir E Priming Valve Secondary Pump Head Priming Waste Line o Figure 9 2 DP SP Priming Valve 312 Doc 065446 01 11 12 9 DP SP Service 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 ove
66. 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 Ba If you are installing the pH Ag AgCl reference electrode in a capillary IC system go on to page 403 If you are installing the pH Ag AgCl reference electrode in an analytical IC Ie system go on to page 405 402 Doc 065446 01 11 12 9 DC Service Be Installing the pH Ag AgCI 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 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 60 pH Ag AgCl Reference Electrode O Ring Remove for capillary IC Figure 9 60 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 61 Reference Electrode Gasket for Capillary IC Figure 9 61 Reference Electrode Gasket for Capillary IC Doc 065446 01 11 12 403 Dionex ICS 5000 Operator s Manual 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
67. Doc 065446 01 11 12 ICS 5000 nasa 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 Dionex 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 Dionex 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 systems 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 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
68. Error messages Audit trail description 207 DC summary 211 DP SP summary 208 EG summary 209 TC summary 213 Error messages DC 263 273 CD cell disconnected 263 CD cell over safe temperature 264 Column open circuit 264 Column over safe temperature 264 270 Compartment open circuit 265 Compartment over safe temperature 265 ED cell disconnected 265 268 High pressure valve error 269 Lower leak sensor wet 271 Reaction coil open circuit 271 Reaction coil over safe temperature 272 Suppressor over current 272 Suppressor over power 272 Suppressor over voltage 273 Upper leak sensor wet 273 Error messages DP SP 232 238 Abnormal drive current 231 Camshaft index too early 232 Camshaft index too late 232 Camshaft sensor always alight 232 Degasser malfunction 232 Excessive drive current 233 Function cannot be adjusted by user 238 Invalid flow value 233 Leak detected 233 Maximum purge pressure exceeded 236 Motor malfunction 234 Motor position error 234 Pressure fallen below lower limit 235 Pressure in working cylinder exceeded safety limit 237 Program with this name already exists 231 Pump block carryover pressure too high 234 Relay 4 configured for inject synchronization 236 System pressure exceeded safety limit 237 Upper pressure limit exceeded 238 Error messages EG 245 257 CR TC mode is off for a virtual pump 247 CR TC over current 246 CR
69. Pressure Valve Maintenance Kit 079053 10 Port High Pressure Valve Maintenance Kit Doc 065446 01 11 12 451 Dionex ICS 5000 Operator s Manual 452 Doc 065446 01 11 12 Symbols Offset analog out 89 5V output DC 86 90 Numerics 10 port valve AM 99 DC 68 70 TC 127 See also High pressure valves 2D data Integrated amperometry 111 113 Pulsed amperometry 113 3D amperometry data 115 117 3D plot description 116 117 Chromatogram 115 Definition 114 Displayed in Chromeleon 114 Isoamperometric plot description 116 I t plot 115 3 way low pressure valve See Low pressure valves 4 port valve 69 6 port valve DC 68 99 TC 126 128 See also High pressure valves See also Injection valves A AAES 74 AC sockets DC 84 ACES 300 Capillary 61 74 Acetonitrile 80 Ag AgCl half cell 80 Index Air bubbles conductivity cell 390 Air particulate samples 153 Air pressure requirements 152 160 Alarm LED DC 55 LED is lighted 55 Alarm LED DP SP 22 LED is lighted 22 Alarm LED EG LED is lighted 47 Troubleshooting 257 260 Alarm LED TC LED is lighted 119 Troubleshooting 303 Amperometry cell Cell design 79 Cell gasket replacement 393 Description 78 79 Electrodes 79 Maintenance 149 Monitoring the pH readout 81 Operating precautions 149 pH cannot be set to 7 0 276 pH limits 151 Polishing the working electrode 396 Reord
70. Relay control DC Control panel 90 DC relay output configuration 90 Operating failure 243 Tube fitting installation 308 Tubing Replacing DC 365 Replacing DP SP 309 Replacing EG 335 Replacing TC 413 U Upper compartment DC Description 64 Upper oven LED 55 USB cables DC 84 DP SP 34 EG 49 Reordering DC 450 Reordering DP SP 443 Reordering EG 446 Reordering TC 451 TC 125 USB communication error Troubleshooting 261 283 284 287 292 296 USB connections DC 84 DP SP 34 EG 261 TC 125 Vv Vacuum degassing module 25 Daily maintenance 199 On off control 26 Vacuum is low 242 VALVE buttons DC 56 Enabling disabling 56 Troubleshooting 275 Valve LEDs DC LED is flashing 56 LED is lighted 56 Valve LEDs TC LED is flashing 119 303 LED is lighted 119 Valves See High pressure valves See Injection valves See Low pressure valves Variable Wavelength Detector 3 9 Regulator Bracket Kit 36 Vials 152 Filling 152 154 Virtual Column Separation Simulator 176 180 Voltammetry 109 See also Cyclic voltammetry VP Vacuum Pump 146 W Waste container EG Preventing gas buildup 148 Waste disposal 205 Waste lines CD Gas separator waste tube 75 Waste lines DC 85 Blocked 274 Waste lines DP SP 34 Waste lines EG 49 50 Blocked or incorrectly installed 257 259 Waste lines TC Blocked 304 Doc 065446 01 11 12 Index 19
71. Reordering 447 Replacing mechanical parts pod 373 Types available 65 Injection valves TC 126 Flow schematics 10 port valve 127 Flow schematics 6 port valve 126 Leaking 304 Operation 126 127 Plumbing 6 port valve 128 Rebuilding 372 416 Replacing mechanical parts pod 417 Types available 121 Inline filter 37 Instrument methods Chromeleon 7 176 Autosampler control 182 Creating methods 176 Integrated amperometry 106 3D data 113 Data storage 113 Integration interval 108 111 Waveform characteristics 111 Waveform example 108 Interior components DC 57 Analytical IC components 64 Conductivity Detector CD 58 64 Electrochemical Detector ED 58 64 IC Cube 59 Lower compartment description 65 Suppressor types 65 Upper compartment description for analytical IC 64 Upper compartment description for capillary IC 58 Inverted edge TTL input control DC 96 Inverted pulse TTL input control DC 96 TonPac ATC HC Trap Column 45 IonPac CTC 1 Trap Column 45 IPAD See Integrated amperometry I t plot 115 L Leak sensor EG 47 256 Leak sensors DC Lower leak sensor wet alarm 271 Replacement 370 Upper leak sensor wet alarm 273 Leak sensors TC Gas 130 289 Humidity 130 289 Leaks Conductivity cell 274 DC 274 EG 47 256 Gas 119 130 289 303 Humidity 119 130 289 303 Injection valve DC 274 Injection valve TC 304 Reference electrode 278 Suppressor 27
72. Safety icons 36 Safety messages 15 36 Salt crystals preventing 201 Sample analysis overview 176 Sample loading With a syringe 183 With an autosampler 182 Sample loop DC Injecting 69 70 72 Loading 71 182 183 Reordering 447 Sample loop TC Injecting 127 Injection valve connections 128 Loading 126 127 Reordering 451 Sample processing 176 Sample tray Loading 152 154 Doc 065446 01 11 12 Index 15 Dionex ICS 5000 Operator s Manual Samples Collecting and storing 152 Diluting 153 Filtering 153 Loading 182 184 Pretreating 153 See also High pressure valves See also Injection valves Self Regenerating Suppressor SRS 50 65 Gas separator waste tube 75 Hydrating 189 190 Start up procedure 189 190 See also Suppressor Sensor gas TC 119 130 289 Sensor humidity TC 119 130 289 Sequence Wizard Chromeleon 6 8 178 Creating a new sequence 179 Sequence Wizard Chromeleon 7 177 Creating a new sequence 178 Service procedures DC Amperometry cell gasket replacement 393 Capillary column replacement 380 385 CD cell air removal 390 CD cell calibration 386 Conductivity detector replacement 389 Electrochemical detector replacement 411 Fuse replacement 377 IC Cube cartridge replacement 379 Injection valve pod replacement 373 Injection valve rebuilding 372 416 Leak sensor replacement 370 PdH reference electrode replacement 407 pH Ag AgcCI refe
73. Server The icon changes to gold SG 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 is not on the Windows taskbar click Start gt All Programs gt Chromeleon gt Server Monitor to open the Server Monitor and click Start 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 EE toolbar button 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 Doc 065446 01 11 12 157 Dionex ICS 5000 Operator s Manual number of device functions can be controlled directly from this panel and the audit trail can be accessed from here isson 3 Sequence Conto Statua Autoamcie Giasert Pump Esnt Geneeatce Detects Compartment Cond Detector EC Detector 30 Amo Prot ms Audi Tat Smp SrueOown gute fn ES Elapsed Time Figure 4 4 Example Chromeleon 6 8 Panel Tabset 158 Doc 065446 01 11 12 ICS 5000 nua DP SP Startup 4 6 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
74. Support Representative for Dionex products perform the performance qualification PQ procedure for IC systems For detailed periodic maintenance instructions for each module see DP SP page 200 DC page 203 TC page 205 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 e DP SP Analytical Preventive Maintenance Kit P N 075970 e DP SP Capillary Preventive Maintenance Kit P N 075039 196 Doc 065446 01 11 12 7 Maintenance e The DC TC preventive maintenance procedure consists of rebuilding each high pressure valve installed in the module The following kits are available 0 4 uL Internal Loop High Pressure Valve Maintenance Kit P N 075040 6 Port High Pressure Valve Maintenance Kit P N 075974 10 Port High Pressure Valve Maintenance Kit P N 079053 NOTE There is no Preventive Maintenance Kit for the EG Doc 065446 01 11 12 197 Dionex ICS 5000 Operator s Manual 198 Doc 065446 01 11 12 ICS 5000 DP SP 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 a Technical Support Representative for
75. Switched AC sockets DC 84 Syringe Reordering 447 Syringe injection 183 Vacuum 183 System configuration drawings 135 146 Analytical IC RFIC EG dual CD and ED system 142 Analytical IC RFIC EG dual CD system 141 Analytical IC RFIC EG single CD system 140 Analytical IC system non RFIC 139 Analytical RFIC EG with post column reagent addition 145 146 Capillary IC RFIC EG dual CD and ED system 137 Capillary IC RFIC EG dual CD system Doc 065446 01 11 12 Index 17 Dionex ICS 5000 Operator s Manual 136 Hybrid RFIC EG dual CD analytical and CD capillary system 138 Matrix elimination 143 144 System Wellness 133 T TC VWD PDA Regulator Bracket Kit 36 Technical Support for Dionex products 307 Temperature calibration DC 67 Temperature control CD 72 Minimizing the effect of variations 73 Temperature compensation 73 Temperature control DC 66 Cell heater 73 Temperature control TC 122 131 Temperature stabilizer TC 8 122 Liquid leaks 304 Operating problem 305 Thermal Compartment TC 3 8 See also Error messages TC Alarm LED is lighted 119 Column ID system 129 Digital I O connectors 124 Front description 119 120 Maintenance 205 206 Moduleware update 282 Oven LED is flashing 120 Oven LED is lighted 120 Predictive Performance functions 133 Rebuilding the injection valve 416 Regulator Bracket Kit 36 Replacing the injection valve pod 417 Service proc
76. TC stopped due to zero flow 247 EG cartridge disconnected 248 EG invalid concentration 249 EG invalid flow 250 Doc 065446 01 11 12 Index 7 Dionex ICS 5000 Operator s Manual EG invalid flow rate concentration 250 EG over current 251 EG over power 252 EG over voltage 252 253 Leak sensor wet 256 Error messages TC AcqOff with previous AcqOn 279 Acquisition still on at program end 279 All samples must specify same value 279 Can t execute Disconnect command 280 Can t execute Standby command 280 Can t find TC3000 HEX image 280 Can t start acquisition 281 Can t start TC firmware 281 Can t use device x 282 Card data checksum error 283 Command unavailable in demo mode 283 Communication error 283 Communication interface is closed 296 Communication time out 284 Compartment door is open 297 Configuration doesn t match 284 Configuration mismatch 284 Counter x exceeded its limit 297 Current flow out of limits 284 Current pressure out of limits 285 Current temperature out of limits 285 Data buffer overrun 285 Data format on chip card unsupported 297 Device control feature not available 286 Device is not remote 286 Device not found on USB 287 Either the current date is 287 Error deleting flash memory 287 Error during storing of card data 288 Error finishing download 281 Error programming flash memory 288 Executing this comm
77. The Dionex EGC contains one of the following a corrosive base KOH LiOH or NaOH a corrosive acid MSA or a concentrated K2C03 solution Wear protective eyewear and gloves when handling the cartridge La cartouche de Dionex EGC contient un de ce qui suit une base corrosive KOH LiOH ou NaOH un acide corrosif MSA ou une solution concentr e de KCO Porter des lunettes et des gants protectives en manipulant la cartouche Die Dionex EGC Kartusche enthalt eine korrodierende Base KOH LiOH oder NaOH eine korrodierende Saure MSA oder eine konzentrierte K C03 L sung Tragen Sie daher beim Umgang mit Kartusche eine Schutzbrille und Handschuhe 9 14 1 Removing the Old EGC l Turn off the pump flow This turns off the power to the Dionex 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 Dionex EGC electrical cable counter clockwise to loosen it and then pull the cable straight out of the EGC 1 or EGC 2 tuo bulkhead connector see Figure 9 14 EGC Cables Figure 9 14 Dionex EGC Cables Doc 065446 01 11 12 339 Dionex ICS 5000 Operator s Manual Analytical IC 5 Close or cap the Dionex EGC vent opening to prevent leakage when you turn over the cartridge in Step 7 If you are removing a capillary Dionex EGC tighten the vent fitting on the top of the Dionex EGC see Figure 9 15 A n wARNI
78. 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 065446 01 11 12 131 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT 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 Maximum temperature 70 C above ambient For example if the ambient air temperature in the lab is 30 C and you set the temperature to 5 C the actual temperature achieved will be about 12 C 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 132 Doc 065446 01 11 12 2 TC Description 2 26 1 Predictive Performance The Predictive Performance feature of the TC provides va
79. Use this POWER button for routine on off control of the DC When the power is on this LED is lighted To turn off the DC press and hold this POWER button for 2 seconds Note The main power switch is on the DC rear panel Does not flash NOTE The VALVE 1 and VALVE 2 buttons can be enabled and disabled in Chromeleon When disabled you can con trol the valve only from the software To enable or dis able a button press the F8 key to open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 select the Advanced or Expert user level and select the ValvelButton or Valve2Button property in the list of DC properties The two sample loading ports on the front of the DC see Figure 2 18 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 56 Doc 065446 01 11 12 2 DC Description injection the DC can be connected to an autosampler For more information about sample injection see Section 5 2 Sample Loading Ports mr e a Figure 2 18 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
80. 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 provided on the Thermo Scientific Reference Library DVD P N 053891 e Disposable Silver Electrode Installation Guide for ED Document No 065137 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 be sure to install the correct IMPORTANT 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 electrodes P N 045972 e Gloves e Blunt end tweezers Doc 065446 01 11 12 393 Dionex ICS 5000 Operator s Manual ED Cell Gasket Replacement Procedure NOTE Always wear gloves when handling the ED cell Never t
81. a LE Dionex ICS 5000 Electrochemical Detector ED Mounting tabs for 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 con nect a gas separator waste tube P N 045460 to the suppres sor waste line during installation For details refer to Dionex ICS 5000 Ion Chromatography System Installation Instruc tions Document No 065447 2 14 3 System Flow Schematics for Conductivity Detection Figure 2 30 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 provided on the Thermo Scientific Reference Library DVD P N 053891 NOTE Thebasic 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 Dionex CRD are not visible Doc 065446 01 11 12 75 Dionex ICS 5000 Operator s Manual COND CELL For anion suppression only optional SUPPRESSOR SEPARATOR COLUMN TEMP STABILIZER Eluent Flow Regenerant Flow For analytical IC only PUMP or WASTE VALVE ELUENT Inject Position ELUENT GENERATOR Figure 2 30 DC Flow Schematic for Con
82. adapter P N 063517 in the vent opening The luer adapter is shipped with the cartridge Remove the luer cap NOTE Store the 10 32 plug or fitting in a safe place The plug or fitting is required when shipping or storing the car tridge 11 Push the Dionex 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 12 Connect the VENT line removed from the old cartridge to the vent opening in the new cartridge see Figure 9 16 Doc 065446 01 11 12 351 Dionex ICS 5000 Operator s Manual Conditioning the Analytical EGC IC Analytical EGC Conditioning EGC VENT Pump at 1 0 mL min for 30 min EGC concentration at 50 mM EGC M 0 5 mL min 7 MPa 1000 psi Backpressure Coil PW B bou TT PIN 053765 et f Temporary connection EGC IN y To Waste Figure 9 26 Flow Schematic for Conditioning an Analytical Dionex EGC High Pressure Version Shown 1 Seta small temporary waste container for example a beaker next to the EG Direct the yellow backpressure coil from the Dionex 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 Eluent Generator panel Verify that the Dionex CR TC is of
83. an invalid value for the DP SP flow rate in Chromeleon To troubleshoot Select a flow rate within the DP SP flow rate range For the flow rate range for each type of DP SP see 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 065446 01 11 12 233 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 assista
84. are small round openings in the bottom of the well see Figure 9 62 Reference Electrode Well Inlet Reference Electrode Well Outlet Figure 9 62 Reference Electrode Well with Reference Electrode Gasket for Capillary IC Installed 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 Screw the pH Ag AgcCI reference electrode into the reference electrode well and tighten it fingertight see Figure 9 63 Figure 9 63 Installing the pH Ag AgCI Reference Electrode In the Reference Electrode Well 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 lines 404 Doc 065446 01 11 12 9 DC Service 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 W Analytical IC System l S OPV O A To avoid any hydraulic pressure buildup when inserting the reference electrode into the cell make sure that fitting plugs are not installed on the cell inlet and outlet fittings Verify that the pH Ag AgcCI reference electrode O ring is present see Figure 9 64 and then screw the pH Ag AgCl reference electrode into th
85. drawer is located above the main power switch see Figure 9 40 Fuse A small tab locks the fuse drawer in Drawer place Using a small screwdriver Tb press the tab in and then 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 10 A IEC 60127 2 slow blow fuses P N 954772 Thermo Fisher Scientific recommends always replacing both fuses Figure 9 40 DC 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 378 Doc 065446 01 11 12 9 DC Service 9 26 IC Cube Service Procedures 9 26 1 Replacing an IC Cube Cartridge l 2 CAUTION MISE EN GARDE VORSICHT 7 Turn off the pump flow 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 Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren Open the DC upper door Disconnect each liquid line connected to the IC Cube cartridge to be replaced Loosen the two thumbscrews on the cartridge se
86. 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 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 238 Doc 065446 01 11 12 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 Ifthe 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 Chrome
87. environment in which the temperature is greater than 40 C 104 F To troubleshoot 1 See Appendix A for environmental specifications 2 Verify that the compartment set point is at least 5 C less than the CD cell set point 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 Column over safe temperature This error occurs when the temperature of the column compartment exceeds the maximum allowed This error may occur if the Dionex ICS 5000 IC system is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot See Appendix A for environmental specifications 264 Doc 065446 01 11 12 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 w
88. 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 l Connect enough backpressure tubing to the cell outlet to shrink bubbles and allow them to pass more easily through the cell See Table 9 9 for the appropriate type and number of backpressure tubing coils required Dionex Sup Column Flow Rate Backpressure pressor Type Format mL min Coils AES 2 mm 0 25 to 0 50 2 red 3 mm 0 50 to 1 00 2 red 4 mm 1 00 to 2 00 1 red SRS or MMS 2 mm or 3 mm lt 0 25 2 red 2 mm or 3 mm 0 25 to 0 50 1 red The red coil P N 045878 consists of 0 125 mm 0 005 in ID PEEK tubing with fittings Table 9 9 Backpressure Coil Requirements Table 9 10 lists the correct pressure range for each type of suppressor Dionex Suppressor Type Pressure Range AES 0 14 to 0 70 MPa 20 to 100 psi SRS or 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 390 Doc 065446 01 11 12 9 DC Service Suppressors Document No
89. 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 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 Dionex 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 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 detec
90. in the DP SP 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 degassing module is either single channel in an isocratic pump or quad channel in a gradient pump The module consists of e A degas chamber with degassing membranes with internal capacity of 670 uL per channel e A dual stage diaphragm vacuum pump e An on board vacuum sensor Doc 065446 01 11 12 25 Dionex ICS 5000 Operator s Manual 2 2 5 e The electronics required to operate the vacuum pump e Tubing fittings and other
91. lists the versions of eluent generator cartridges available for use with the EG Each Dionex EGC contains an electrolyte concentrate solution appropriate for the particular eluent generation Each Dionex EGC is designed to be used in either a capillary IC system or an analytical IC system A Dionex EGC designed for a capillary IC system cannot be used in an analytical IC system and vice versa Analytical IC systems typically include Dionex EGC 500 cartridges e Although it is possible to operate high pressure analytical systems with Dionex EGC 300 cartridges and if required for the application the Thermo Scientific Dionex EPM 300 Electrolytic pH Modifier this will limit the Doc 065446 01 11 12 43 Dionex ICS 5000 Operator s Manual operating pressure to 21 MPa 3000 psi Thermo Fisher Scientific does not currently offer a Dionex EPM for high pressure systems Dionex 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 Standard Pressure EGC 300 K2C03 074536 Generates potassium carbonate eluent for anion exchange separations EPM 300 Electrolytic 080135 Produces a carbonate bicarbonate pH Modifier mixtur
92. mm diameter columns 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 IMPORTANT f you intend to operate the Dionex ICS 5000 system at pressures above 21 MPa 3000 psi all installed consumables must be designed for high pressure operation This includes the Dionex eluent generator cartridge eluent degasser CR TC and if required for the application trap column Operation of standard pressure consumables at pressures above 21 MPa 3000 psi will cause leakage It will also result in irrevocable damage to the consumables and void the product warranty 2 Doc 065446 01 11 12 1 Introduction 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 Pump Product Name Page Dionex ICS 5000 Dual Pump page 4 Dionex ICS 5000 Single Pump age 4 Eluent Generator Dionex ICS 5000 Eluent Generator Eluent Organizer Dionex ICS 5000 Elue
93. 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 l Click Start on the sequence control bar see Figure 5 5 Anions i New CD Bicsso00 r dle i ll save Studio Print gt PUP Se Insert Row APYFillDown Lock NZ Filtering Grouping f Report Columns z Chromatogram Name Type Position Volume pl Instrument Metho Processin Status 1 None JAn i Unknown RAI 20 0 AS12A Product AS12A Idle 2 None 3 2 i Unknown RA2 20 0 AS124 Product AS124 Idle 3 None le 3 i Unknown RA3 20 0 ASTZA Product AS12A Idle 4 None a4 i Unknown Rad 20 0 45124 Product AS12A Idle 5 None fal 5 i Unknown RAS 20 0 AS124 Product AS12A dle 6 None ds i Unknown RBI 20 0 AS124 Product AS124 Idle Liene pte ga n AEO para oann sen AR Ai Podul ASIA deman Figure 5 5 Starting a New Sequence in Chromeleon 7 180 Doc 065446 01 11 12 5 Operation 2 The sequence is appended to 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 see Figure 5 6
94. 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 5 Analog Output Configuration Settings 88 Doc 065446 01 11 12 2 DC Description Analog Output VEWUGS Description Setting Recorder Zero Full Scale Use this setting to calibrate a calibration Normal 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 For applications in which the analyte output is lower than the background signal the polarit
95. on the fitting align with the grooves in the reference electrode well see Figure 9 71 Insert the fitting into the well PdH Reference Electrode Knobs Grooves Figure 9 71 Inserting the PdH Reference Electrode Fitting into the Reference Electrode Well Screw the nut on the PdH reference electrode into the reference electrode well and tighten it fingertight see Figure 9 72 After fingertightening use a wrench to tighten the nut an additional 20 to 30 degrees Figure 9 72 Installing the PdH Reference Electrode Nut 410 Doc 065446 01 11 12 9 DC Service 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 see the instructions below Conditioning the PdH Reference Electrode Condition the PdH reference electrode after plumbing the cell 1 On the Chromeleon 7 ePanel 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 flow also b Eluent Generator panel Enter 100 mM in the Target Concentration field This turns on the power to the Dionex 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 vo
96. port high pressure injection valve 075963 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 valve 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 126 Doc 065446 01 11 12 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 an
97. 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 analysis This allows the DP SP to stabilize the flow rate 314 Doc 065446 01 11 12 9 DP SP Service 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 Additional items e Cleanroom gloves lint free particle free and oil free e 1 2 inch open end wr
98. requires Microsoft Windows 7 Windows Vista or Windows XP Automated Procedure Wizards Standard feature Doc 065446 01 11 12 425 Dionex ICS 5000 Operator s Manual Dionex ICS 5000 Eluent Generator Specifications Continued System Smart Startup and Shutdown Standard feature System Wellness and Predictive Performance Standard feature Application Templates Standard feature Automation Support of Third Party Instruments Fully controls over 300 different instruments including GC HPLC and MS from more than 30 manufacturers Customizable System Control Panels Standard feature Signal Channels Eluent concentration Data Trending Plots Numerical device parameters plotted System Status Virtual Channels Standard feature Power Failure Protection Standard feature System Trigger Commands and Conditionals Standard feature Daily Audit Trail Standard feature Sample Audit Trail Standard feature Eluent Cartridge Information Storage Serial number and expiration date Customized Reporting Standard feature with unlimited report workbooks GLP Compliance 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 powe
99. requires at least 14 MPa 2000 psi of system backpressure to ensure 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 Analytical IC systems typically include Dionex EGC 500 cartridges Although it is possible to operate high pressure analytical systems with Dionex EGC 300 cartridges and if required for the application the Dionex EPM 300 Electrolytic pH Modifier this will limit the operating pressure to 21 MPa 3000 psi If the backpressure is too low install a backpressure coil see Table 9 5 between the injection valve and the OUTLET port on the Dionex EGC Doc 065446 01 11 12 361 Dionex ICS 5000 Operator s Manual 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 The EG Ship Kit P N 075780 includes four backpressure coils see Table 9 5 Part Backpressure Flow Rate Approximate Number Coil Description Backpressure Added AAA 053762 4mm ID 2 0 mL min 3 5 MPa 500 psi 1 0 mL min 1 75 MPa 250 psi AAA 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
100. status of several DC components and functions e 9 CONNECTED ALARM 2 UPPER LOWER erase SUPPRESSOR OVEN VALVE 1 LOAD INJECT LOAD INJECT e VALVE 2 Figure 2 17 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 a Chromeleon 6 8 timebase ALARM The leak sensor is wet or a Does not flash valve or suppressor error occurred Check the Chromeleon audit trail for the cause SUPPRESSOR 1 The suppressor is on and Does not flash 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 set temperature is transitioning to the set temperature The compartment is not ready for operation Doc 065446 01 11 12 55 Dionex ICS 5000 Operator s Manual Button LED Label VALVE 1 LOAD VALVE 2 LOAD VALVE 1 INJECT VALVE 2 INJECT If the LED Is On Use the VALVE 1 and VALVE 2 buttons to manually switch the position of the DC injection valves The LEDs indicate whether the valve is in the Load or Inject position If the LED Is Flashing Valve error See Section 8 25 for troubleshooting POWER
101. 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 48 Doc 065446 01 11 12 2 EG Description One 1 8 m 6 ft USB cable P N 960777 is provided in the EG Ship Kit P N 075780 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 on unless instructed to turn it off for example before performing a service procedure NOTE Forroutine 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 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 wichti
102. the problem continues contact Technical Support for Dionex products for assistance Leaking suppressor Refer to the suppressor manual for troubleshooting procedures Suppressor manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 274 Doc 065446 01 11 12 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 7 or Chromeleon 6 8 in order to use them to manually switch the inject valves To enable a button open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 and select the ValvelButton 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 065446 01 11 12 275 Dionex ICS 5000 Operator s Manual 8 28 2 Cannot Set ED Cell pH Rea
103. 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 fit tings 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 detect any reference potential shift that may occur over time This allows you to determine when the pH Ag AgCI reference electrode needs to be regenerated or replaced 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 Doc 065446 01 11 12 81 Dionex ICS 5000 Operator s Manual 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 t
104. 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 Manager or the Chromeleon 6 8 Server Configuration program see Section 2 17 4 Doc 065446 01 11 12 87 Dionex ICS 5000 Operator s Manual 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 33 The analog outputs supply a voltage signal proportional to the current measured by the detector cell The outputs can be connected to an analog to digital A D converter such as an integrator or other recording device See 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 5 describes the settings You select the preferred settings on the detector panel in the Chromeleon 7 ePanel Set see Figure 2 36 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
105. tighten it an additional one quarter turn with the 1 2 inch wrench 5 Ifthe check valve continues to leak it is defective Replace both check valve cartridges see Section 9 6 e Eluent proportioning valve leaks gradient pump only Tighten loose fittings If there are no loose fittings the proportioning valve assembly should be replaced For assistance contact Technical Support for Dionex products Doc 065446 01 11 12 241 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 For assistance contact Technical Support for Dionex products 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 See the troubleshooting steps on page 237 for this audit trail message The system pressure exceeded the safety limit 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
106. 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 328 Doc 065446 01 11 12 9 DP SP Service 3 Reconnect all tubing connections to the pump head Tighten connections fingertight and then tighten an additional one quarter turn only 4 Push the component mounting panel back into the enclosure using the handle in the center of the panel Close the DP SP door 5 Press the POWER button on the front of the DP SP to turn on the pump 6 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 Doc 065446 01 11
107. used with an analytical pump To troubleshoot 1 Install the correct type of Dionex EGC for the pump type 2 Fora hybrid system a dual system with both an analytical and a capillary pump check the Dionex EGC configuration properties in the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program to verify that the correct pump is linked to the Dionex EGC EGC cannot be used due to invalid ion count This error occurs if the ion count reported by the Dionex EGC is invalid This may indicate a problem with the memory chip in the Dionex EGC To troubleshoot 1 Make sure the Dionex 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 Dionex EGC cartridge is connected to the EG or if an analytical Dionex EGC is connected to a capillary IC system To troubleshoot 1 Verify that a capillary Dionex EGC is installed Doc 065446 01 11 12 255 Dionex ICS 5000 Operator s Manual 2 Verify that the Dionex 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 Dionex EG
108. 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 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 128 Doc 065446 01 11 12 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 4 e i e Thermo Column Identification System 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 Manager 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 avail
109. water in the electrolyte reservoir Make sure the Dionex EGC packaging conforms to hazardous material shipping requirements Refer to the Material Safety Data Sheet MSDS shipped with the Dionex EGC for the chemical description 190 Doc 065446 01 11 12 a DC Shutdown 6 3 6 4 6 4 1 6 4 2 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 ED Cell Storage ED Cell Short term Storage 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 AgCl reference electrode frit may partially dry out If this occurs regenerate the electrode by soaking it in a solution containing 1 M KCI and 1 M HCl pH Ag AgCI Reference Electrode Long term Storage If the cell will not be used for 2 days or more remove the pH Ag AgCI reference electrode and store it in a solution of saturated KCI 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 specification
110. whenever they become discolored if bacterial buildup is evident or if eluent flow is blocked Doc 065446 01 11 12 199 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 9 Be 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 Bey e Clean eluent reservoirs every 3 months with methanol or isopropyl alcohol see Section 9 4 7 5 DP SP
111. with the connection between the TC and the Chromeleon server or the power supply To troubleshoot 1 Check the USB connections 2 Check the connection from the TC to the power supply 3 Ifyou cannot identify the cause of the error contact 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 column 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 065446 01 11 12 287 Dionex ICS 5000 Operator s Manual 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 Thermo Fisher Scientific name on the card faces up and the LED on the memory slot is green If this error occurs when the chip card is prope
112. 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 required for up to two IC systems The following configurations are possible e Single system one capillary IC system or one analytical IC system e Dual system two capillary IC systems two analytical IC systems or one system of each type a hybrid Doc 065446 01 11 12 57 Dionex ICS 5000 Operator s Manual puy 2 11 1 DC Interior Components for Capillary IC In capillary IC 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 ICS 5000 IC Cubes IC Cubes 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 58 Doc 065446 01 11 12 2 DC Description Figure 2 19 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
113. 0 Vpc 0 25 A 3 W White Dig Out GND Black Shield Table 2 8 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 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 065446 01 11 12 125 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 075960 TC with one 2 position 6 port high pressure injection valve 075961 TC with two 2 position 6 port high pressure injection valves 075962 TC with one 2 position 6
114. 00 psi 2 mm 053765 Backpressure coil 0 5 mL min 1000 psi 2 mm Miscellaneous AAA 074459 EG degas cartridge for capillary IC systems 072133 Dionex EGC capillary mounting adapter 075522 Dionex RFIC Eluent Degasser for standard pressure and high pressure analytical IC systems 954773 Fuse IEC 60127 2 slow blow rated at 2A 250V 063246 USB cable 1 m 3 ft long 074373 Ferrule fitting 10 32 double cone 074449 Fitting bolt 10 32 for double cone ferrule fitting 046985 Mini screwdriver 446 Doc 065446 01 11 12 E DC Reordering Information Part Number Item Valves and Accessories 074525 High pressure injection 4 port 075917 High pressure injection or switching valve 6 port 075918 High pressure injection or switching valve 10 port 061971 Low pressure valve 3 way 079848 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 075973 Valve rebuild kit 6 port 079054 Valve rebuild kit 10 port IC Cube and Accessories for Capillary IC 072000 Dionex ICS 5000 IC Cube 072186 IC Cube tubing kit includes precision cut tubing for column connections AAA 074459 EG degas cartridge for capillary 072052 Dion
115. 000 and 5000 psi if a Dionex EGC 500 is installed or between 14 and 21 MPa 2000 and 3000 psi if a Dionex EGC 300 is installed If necessary increase the system backpressure by installing a backpressure coil between the injection valve and the ELUENT OUT port on the Dionex EGC For instructions see Section 9 17 The recommended maximum operating pressure for the EG in an analytical IC system is 35 MPa 5000 psi if a Dionex EGC 500 is installed or 21 MPa 3000 psi if a Dionex EGC 300 is installed Excessive backpressure may rupture the tubing inside the Dionex RFIC Eluent Degasser Doc 065446 01 11 12 147 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 production of small amounts of oxygen or hydrogen gas To ensure that the gas is not trapped in a closed container and allowed to concentrate install a 1 3 cm 0 52 in ID black gas separator waste tube P N 045460 in an uncapped waste container Connect the Waste Gas Separator line to the waste tube CAUTION NE FERMEZ PAS LE CONTENEUR DE GAZ R SIDUEL Le Dionex ICS 5000 Eluent Generator EG le Atlas Electrolytic Suppressor et le Self MISE EN GARDE Regenerating Suppressor SRS travaillent avec un proces d lectrolyse qui produit des petites quantit s de gaz d oxyg ne ou d hydro
116. 01 in ID tan PEEK tubing P N 074582 in the IC Cube Ship Kit P N 072003 Connect one end of this line to the Dionex EGC INLET port 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 Dionex EGC setup procedure Connect a piece of 0 25 mm 0 010 in ID black PEEK tubing to the Dionex 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 Dionex EGC 344 Doc 065446 01 11 12 9 EG Service 8 10 11 12 13 Slide the Dionex EGC with the electrolyte reservoir on top into the cartridge holder see Figure 9 20 Figure 9 20 Capillary Dionex EGC Installed on Holder Push the Dionex 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 Dionex EGC a few turns to vent the
117. 065446 01 11 12 a 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 Eluent Generator tab to display the Eluent Generator panel see Figure 4 8 Home Sampler DP EluentGenerator DC CD Left ED Right Audit pe o Q comes EG1 Control U Target Concentration 0 00 mM Applied Concentration 0 00 CRIC c EGC1 Information Serial Number 123456789012 Cartridge Type EGC 500 KOH i Expiration Date N A EGC Remaining 100 0 o SO r Ni AN e e ae et Figure 4 8 Example EG Panel Chromeleon 7 Version Shown 3 Entera 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 Dionex EGC also 4 Ifthe 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 Dionex EGC at the selected Target Concentration value Doc 065446 01 11 12 165 Dionex ICS 5000 Operator s Manual 4 10 5 Ifthe CR TC switch is off click the switch to turn on the power to the Dionex CR TC Selecting the Eluent Concentration The allowable eluent concentration depends on several factors the flow rate suppressor type Dionex EGC type and car
118. 075974 10 port valve P N 079053 contains all required replacement parts NOTE Substitution of non Dionex Thermo Scientific parts may impair valve performance and void the product warranty NOTE If you prefer you can replace the injection valve pod instead of rebuilding the valve Replacing the pod is easier and faster than rebuilding the valve 1 Turn off the pump flow 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 T r ffnen bzw Wartungs oder Servicearbeiten durchf hren VORSICHT 3 Open the TC door 4 Disconnect each liquid line connected to the injection valve 5 Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 416 Doc 065446 01 11 12 9 TC Service 6 Reconnectall liquid lines to the injection valve see Figure 9 76 Green T TO INJECT VALVE W 25 uL SAMPLE LOOP Orange TO INJECT VALVE P Figure 9 76 7 Turn on the power to the TC SAMPLE IN from door inject port or autosampler
119. 1 12 401 Dionex ICS 5000 Operator s Manual 4 Click the Calibration button The Wellness panel opens see Figure 9 59 Electrochemical Detector Wellness Calibration ED 5000 Instrument System_2 PH Electrode Calibration Current and Previous Values Instructions Current pH Electrode Offset 0 00 Place the pH electrode in a pH buffer solution Press the pH 7 Offset Calibration button to calibrate the pH offset Wait until the calibration has finished Current pH Electrode Slope 59 17 5 7 Current Calibration Date 5 14 2012 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 s 9 Calibration button to calibration the pH slope Previous pH Electrode Offset 0 00 Current pH Reading 10 00 Previous pH Electrode Slope 59 17 pH 7 Offset Calibration Offset Calibration Blevins Aaaaton ote ATEN pH Slope Buffer Value 10 00 ES PH Slope Calibration 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 Figure 9 59 Wellness Panel Dionex ICS 5000 Electrochemical Detector Chromeleon 7 Version Shown 5 Follow the instructions on the Wellness panel to calibrate the electrode 6
120. 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 122 Doc 065446 01 11 12 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 Figure 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 065446 01 11 12 123 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
121. 2 Camshaft sensor always alight Abort page 232 Camshaft sensor missing or dark Abort page 232 Degasser malfunction Warning page 232 Excessive drive current Camshaft x x Abort page 233 Invalid flow value Abort page 233 Leak detected Flow stopped Abort page 233 Left hand pump block carryover pressure is too Abort page 234 high Motor malfunction Abort page 234 Motor position error The motor is overloaded Abort page 234 Pressure fallen below lower limit Abort page 235 Relay 4 is configured for inject synchronization Abort page 236 Please change pump configuration Right hand pump block carryover pressure is Abort page 234 too high The maximum purge pressure was exceeded Abort page 236 The pressure in the left hand working cylinder Abort page 237 exceeded the safety limit The pressure in the right hand working cylinder Abort page 237 Table 8 1 DP SP Error Messages 208 Doc 065446 01 11 12 8 Troubleshooting DP SP Related Audit Trail Error Message Default Severity Level The system pressure exceeded the safety limit Abort page 237 This function cannot be adjusted by the user Abort page 238 Upper pressure limit exceeded Abort page 238 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 see the page indicated in the table
122. 2 253 Dionex ICS 5000 Operator s Manual 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 pump linked to the EG To troubleshoot 1 Set the flow rate to a value within the allowed range See Appendix A for flow rate specifications 2 Check the Dionex EGC configuration properties in the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program to verify that the pump and Dionex 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 Dionex EGC is out of range or there is no pump linked to the Dionex EGC To troubleshoot 1 Set the flow rate to a value within the allowed range See Appendix A for flow rate specifications 2 Check the Dionex EGC configuration properties in the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program to verify that the pump and Dionex EGC are linked 254 Doc 065446 01 11 12 8 EG Troubleshooting EGC 1 is not linked to a compatible pump OF O EGC 2 is not linked to a compatible pump This error occurs if the type of pump linked to the Dionex EGC does not match the Dionex EGC type A capillary Dionex EGC can only be used with a capillary pump an analytical Dionex EGC can only be
123. 4 Enter the Flow rate required for your application This starts the pump flow also 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 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 If your system includes a capillary pump linked to a Dionex EGC using the standard EG degas capillary cartridge P N AAA 074459 the high pressure limit must be changed to 21 MPa 3000 psi Pump Configuration Default Low Default High Pressure Limit Pressure Limit Capillary pump not linked 0 41 MPa 6000 psi to a Dionex EGC Capillary pump linked to a 1 4 MPa 200 psi 34 MPa 5000 psi Dionex EGC Analytical pump not linked 0 41 MPa 6000 psi to a Dionex EGC Analytical pump linked to a 1 4 MPa 200 psi 21 MPa 3000 psi Dionex EGC Analytical pump linked to 1 4 MPa 200 psi 34 MPA 5000 psi high pressure Dionex EGC Table 4 1 Default Pressure Limits for DP SP Pumps a Change the default high pressure limit to 21 MPa 3000 psi 164 Doc
124. 4 Temperature stabilizer TC 304 LED descriptions DC 55 56 119 LED descriptions DP SP 21 22 LED descriptions EG 39 40 LED descriptions TC 119 120 Lithium hydroxide eluent 44 Load command 184 Loading samples 182 Instrument method example 184 Program example 184 With a syringe 183 With a vacuum syringe 183 With an autosampler 182 Loading the autosampler tray 152 Low detector output 228 Low pressure limit Selecting 164 Doc 065446 01 11 12 Index 11 Dionex ICS 5000 Operator s Manual Lower compartment DC Description 65 Lower oven LED 55 Low pressure valves 85 Controlling 101 External valve outputs DC 85 Flow schematic 100 Installed in AM 97 Reordering 447 Luer adapter fitting Reordering 447 M Main power receptacle DC 84 TC 205 Manuals for ICS 5000 system 13 15 Mark analog output 89 Matrix elimination 64 97 System configuration 143 144 Methanesulfonic acid eluent 44 Methanol 80 Methods See Instrument methods Chromeleon 7 Microbore IC applications 2 MicroMembrane Suppressor MMS 65 74 See also Suppressor Mixer static 27 Mobile phases See Eluents Moduleware 207 MSQ Plus Mass Spectrometer 3 10 DP SP 31 EG 49 TC 123 Main power switch N DC 84 Nitrite in samples 153 DP SP 31 Noisy baseline 219 EG 49 Normal edge TTL input control DC 96 TC 123 Normal pulse TTL input control DC 96 Ma
125. 446 01 11 12 iii Dionex ICS 5000 Operator s Manual 2 19 3 Cyclic Voltammetry Li 109 2 19 4 Waveforms a a eee eee 109 2 19 5 Storing and Reprocessing Amperometry Data 113 TC Description os sn VERRI oe Ken ees 119 220 TC Front Features cipria viola i ballar asta si cato 119 2 21 TC Interior Components 121 2225 TC Rear Panel sormesi eia aes aa A A ni 123 223 Injection Valvestino e ii ia aa E ariana 126 2 23 1 Injection Valve Operation LL 126 2 23 2 Injection Valve Plumbing 0 00 128 2 24 Column Identification ID System 129 2 25 Gas and Humidity Sensors 0 ccc ee ene 130 2 26 TC Theory of Operation 131 2 26 1 Predictive Performance 000 e eee eee eee 133 3 Configurations Sl OMGTVASW hous E Popa Sy um este MW ace eta ey aay hae Whee eos er nn 135 4 Startup 4 1 Operating Precautions 0 0 cece eens 147 4 1 1 EG Operating Precautions 02 00 00 147 4 1 2 ED Cell Operating Precautions 4 149 4 2 System Startup Checklist 0 0 00 eee eee eee eee 152 Doc 065446 01 11 12 Contents 4 3 Preparing Samples 00 cect teens 152 4 3 1 Collecting and Storing Samples 152 4 3 2 Pretreating Samples 00 0 e eee 153 4 3 3 Diluting Samples 153 4 3 4 Filling Sample Containers and Loading the Sample Tray 154 44 Starting Chromeleon 7 155 4 4 1 St
126. 449 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 Maintenance Kit 075974 6 Port High Pressure Valve Maintenance Kit 079053 10 Port High Pressure Valve Maintenance Kit 450 Doc 065446 01 11 12 E TC Reordering Information Part Number Item Valves and Accessories 075973 Injection Valve Rebuild Kit for 6 port valve includes valve seal hexagon wrench and instructions 079054 Injection Valve Rebuild Kit for 10 port valve includes valve seal hexagon wrench and instructions 075917 Injection valve head including seal for 2 position 6 port valve 075918 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 1m 3 ft 6000 1004 6 pin mini DIN signal cable 5 m 16 4 ft 064792 TC VWD PDA Regulator Bracket Kit Maintenance Kits 075040 0 4 uL Internal Loop High Pressure Valve Maintenance Kit 075974 6 Port High
127. 50 1 00 1 Create Application 2 Prepare System 3 Execute Application System Maintenance Daily Audit Trail Consumable Change Edit Program Eluent Change oe Single Standard 1 Single Sample 1 Single Sample 2 Single Sample 3 Sinale Samnle 4 on 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 065446 01 11 12 181 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 or well plates 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 P N 053891 3 Create a sequence in Chromeleon that specifies the vials or well plates from which to take sample injections and the order in which the injections should be run
128. 73 for all tubing connections For tightening requirements 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 that there are no nicks or burrs on the end Doc 065446 01 11 12 413 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 you want to monitor To select the column to be monitored 1 Start the Chromeleon 7 Instrument Configuration Manager 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 73 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 73 TC Proper
129. 77 Fuses DP SP 31 Replacement procedure 333 Fuses EG 49 Replacement procedure 363 Fuses TC 123 Replacement procedure 419 G Gas leak in TC 119 130 289 Gas sensor TC 130 289 Adjusting sensor sensitivity 130 Alarm troubleshooting 130 Gas separator waste tube 75 Installation 148 Reordering 448 Gas vent line EG 49 RFIC Eluent Degasser 49 Glassy carbon electrodes 79 GM 4 Static Mixer 27 223 442 Gold electrodes 79 Gradient proportioning valves 25 H Half cells 80 Heater Conductivity cell 72 Doc 065446 01 11 12 Index 9 Dionex ICS 5000 Operator s Manual Reaction coil 104 High pressure limit Limit is tripped 237 238 Selecting 164 High pressure fittings 308 High pressure inline filter 37 High pressure valve error 269 High pressure valves AM Controlling 101 Flow schematics 99 Installed in AM 97 98 Rebuilding 372 Reordering 447 Replacing 373 High pressure valves DC 68 10 port valve 71 4 port valve 69 6 port valve 70 For analytical IC system 68 For capillary IC system 68 High pressure valves TC 121 126 Reordering 451 Humidity leak in TC 119 130 289 Humidity sensor TC 130 289 Adjusting sensor sensitivity 130 Alarm troubleshooting 130 Hybrid system configuration 135 138 I T O option DC 85 86 450 5V output 86 Analog outputs 86 Connections 87 Power output 90 Relay outputs 86 TTL inputs and outputs 86 IC C
130. 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 connections 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 Reconnectthe 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 for capillary pump P N 068646 for analytical pump
131. 8 Troubleshooting Analytical Ad 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 Dionex 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 following changes to operating
132. 8 2 9 8 3 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 Disconnect all tubing connections to the pump head with the damaged piston Using the 3 0 mm hex key P N 062338 loosen the Allen screws on the pump head with the damaged piston Remove the Allen screws and then carefully remove the head and place it on a clean surface If the piston was not removed with the pump head in Step 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 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 Installing the New Piston Slide the new piston for capillary pump P N 068646 for analytical pump P N 079857 partway into the pump head approximately 6 mm 1 4 in of the sapphire part of the piston should extend from the head Reinstalling the Pump Head 1 Place the pump head back on the pump 2 Reinstall the screws in the pump head Using the 3 0 mm hex key P N 062338
133. 9 2 e Cyclic voltammetry see Section 2 19 3 NOTE Cyclic voltammetry is supported in Chromeleon 6 8 but not Chromeleon 7 Doc 065446 01 11 12 105 Dionex ICS 5000 Operator s Manual 2 19 1 2 19 2 DC Amperometric Detection In DC amperometry a constant potential is applied to the working electrode The potential can be entered in a Chromeleon 7 instrument method see Figure 2 49 or a Chromeleon 6 8 program amp Instrument Method Wizard Options ED EDet1 EDet1 Options EDetl Options for Options ED EDet1 Channels Amperometry Cell Data Collection Rate Autozero vw a Total oi 0 S e ay of No Voltage V Retention min Yoltage 1 Initial Time 0 0000 2 0 000 0 0000 Insert Delete At salta annati Figure 2 49 DC Amperometry Instrument Method Wizard Page in Chromeleon 7 The applied voltage can be changed up to 10 times during a run The actual number of potential changes allowed depends on the available data storage capacity which is determined by the length of the run and the data sampling rate 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 seri
134. Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The following kits are available e DP SP Analytical Preventive Maintenance Kit P N 075970 e DP SP Capillary Preventive Maintenance Kit P N 075039 200 Doc 065446 01 11 12 a 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 a Technical Support Representative for Dionex products For information about maintenance procedures for the Dionex EGC trap column or suppressor refer to the appropriate product manual These manuals are provided 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 activated 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 M
135. C cartridge is connected to the EG or if a capillary Dionex EGC is connected to an analytical IC system To troubleshoot 1 Verify that an analytical Dionex EGC is installed 2 Verify that the Dionex 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 EGC This error occurs if no Dionex EGC cartridge is connected to the EG or if the cartridge serial number is not valid for the type of IC system To troubleshoot 1 Verify that a Dionex EGC of the correct type capillary or analytical is installed 2 Verify that the Dionex 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 256 Doc 065446 01 11 12 8 EG Troubleshooting 2 Tighten fittings or replace tubing and fittings as required see Section 9 12 See 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 8 20 This error occurs if you attempt to configu
136. CR TC back plate with the ball studs on the mounting plate and then push the Dionex CR TC firmly onto the mounting ball studs The Dionex CR TC clicks into place when properly installed 9 Push the Dionex 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 10 Push the tray into the module until it locks into place Close the EG door 360 Doc 065446 01 11 12 Analytical Analytical IC 9 EG Service 9 16 Replacing the RFIC Eluent Degasser Turn off the pump flow Open the front door of the EG Push down on the slide release latch and pull the tray forward until it reaches the stop Grasp the old Dionex RFIC Eluent Degasser by the sides and pull it straight off the ball studs that secure it to the component mounting panel Disconnect the three lines connected to the degasser fittings ELUENT OUT ELUENT IN and VENT Connect these lines to the new Dionex RFIC Eluent Degasser P N 075522 Align the two mounting holes on the back plate of the new Dionex RFIC Eluent Degasser with the ball studs on the component mounting panel Push the degasser firmly onto the mounting ball studs The degasser clicks into place when properly installed Push the tray into the module until it locks into place Close the EG door Dispose of the old degasser 9 17 Installing a Backpressure Coil In an analytical IC system the Dionex EGC
137. CS 5000 Conductivity 2 Detector EG Dionex ICS 5000 Detector Chromatography Module DC 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 results In combination with capillary columns at flow rates of 0 010 mL min Doc 065446 01 11 12 1 Dionex ICS 5000 Operator s Manual 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 minimize 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 analytical 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
138. CS 5000 Operator s Manual Pulse damper for capillary pump 28 Shutdown procedure 187 Spare parts 441 Specifications 421 Static mixer 27 Status bar buttons and LEDs 21 System configurations 135 143 USB connections 34 Waste lines 34 See also Error messages DP SP Dual system configuration 138 141 142 E EC cell See Amperometry cell ED cell See Amperometry cell ED cell disconnected error 265 268 EGC See Eluent generator cartridges Electrochemical detection DC amperometry 106 Integrated amperometry 106 Pulsed amperometry 106 Electrochemical Detector ED 3 7 78 436 3D data 115 117 Amperometric cell description 78 Data storage 113 Description 64 78 Detection modes 78 105 Palladium hydrogen PdH reference electrode 82 pH Ag AgcCI reference electrode 80 Reordering information 448 Replacement procedure 411 Shutdown procedure 191 Working electrodes 78 See also Amperometry cell Electrodes 79 Reference 78 Working 78 Electrolysis gases Purging from eluent 46 62 147 Venting from system 49 Eluent concentration 165 167 Eluent generation Electrolysis gases 46 62 Eluent Generator EG 3 4 Alarm LED is lighted 257 260 Analytical IC system 42 43 Backpressure 46 Backpressure coil 219 Capillary IC system 41 Component description 40 43 45 46 Degas cartridge for IC Cube 62 Electrical connections for consumables 47 Eluent concentratio
139. 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 compartment of the DC see Figure 2 23 The CD is available in two versions e Acapillary CD P N 072041 for use in systems running capillary flow rates e An analytical CD P N 079829 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 there may be 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 ai
140. Dionex EGC To ensure proper ventilation always loosen the fitting on the top of the capillary Dionex 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 Eluent Generator panel Verify that the Dionex CR TC is off To avoid damaging the suppressor and Dionex CR TC always turn them off before flushing the Dionex EGC The pump flow is on during flushing however no flow reaches the suppressor or Dionex CR TC c Pump panel Set the flow rate to 0 02 mL min This turns on the pump flow also Flush the capillary Dionex EGC for 20 minutes and then turn off the pump flow Disconnect the temporary tubing from the Dionex EGC OUTLET port Doc 065446 01 11 12 345 Dionex ICS 5000 Operator s Manual fe 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 Dionex CR TC to the Dionex EGC OUTLET port see Figure 9 21 2 Disconnect the lines from the ELUENT OUT and REGEN IN port of the Dionex 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 Sio Pump at 0 02 mL min for 15 min EGC concentration at 50 mM EGC AIN 0 062 mm 0 0025 in ID n PEEK Tubing A
141. Dionex 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 See Section 8 23 to determine why there is no flow 2 Ifthe error message appears again contact Technical Support for Dionex products for assistance The Dionex EGC control electronics may have malfunctioned NOTE The Dionex ICS 5000 IC system electronics components cannot be serviced by the user 252 Doc 065446 01 11 12 8 EG Troubleshooting EG1 wrong cartridge error or EG2 wrong cartridge error This error occurs when the Dionex EGC plugged into an EG is not supported for use with your system To troubleshoot See Table 2 3 for a list of the supported Dionex 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 if you try to turn on the Dionex EGC when a live EG is linked to a virtual pump To prevent damage to the Dionex EGC the mode is automatically turned off to ensure that the EG does not operate when there is no flow Doc 065446 01 11 1
142. Dionex ICS 5000 Operator s Manual 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 Thermo Scientific Dionex Suppressors Capillary CD ACES 300 Capillary CCES 300 Capillary Analytical CD AAES CAES AMMS 300 CMMS ASRS 300 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 provided 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 29 The suppressor cable plugs into the connector next to the detector Conductivity Detector Suppressor Optional ASRS 300 model shown Suppressor Cable fn Se Figure 2 29 Analytical Conductivity Detector with Suppressor System 1 74 Doc 065446 01 11 12 2 DC Description NOTE Itis also possible to control an analytical suppressor with
143. Dionex ICS 5000 lon Chromatography System Operator s Manual Document No 065446 Revision 01 November 2012 2012 Thermo Fisher Scientific Inc All rights reserved AES Atlas Chromeleon IonPac OnGuard and SRS are registered trademarks of Thermo Fisher Scientific Inc in the United States Acrobat Adobe and Adobe Reader are registered trademarks of Adobe Systems Incorporated 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 Corporation KIMWIPES is a registered trademark of Kimberly Clark Corporation PharMed and Tygon are registered trademarks of Saint Gobain Performance Plastics Ultem is a registered trademark of General Electric Company Ultrajet is a registered trademark of ITW Chemtronics PEEK is a trademark of Victrex PLC TitanHP is a trademark of Rheodyne LLC 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 this document is for reference purposes on
144. Dionex products 7 2 DP SP Daily Maintenance Analytical 9 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 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 a Dionex EGC to generate carbonate bicarbonate eluent When the end line filters are new they are pure white Replace the filters
145. Doc 065446 01 11 12 385 Dionex ICS 5000 Operator s Manual 9 27 CD Service Procedures 9 27 1 Calibrating the CD Cell NOTE Do not use this procedure to calibrate a new cell New cells are calibrated at the factory Items Needed Description 1 0 mM KCI solution Prepare by dissolving 0 07456 g of reagent grade 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 Click the CD tab on the Chromeleon 7 ePanel Set or the Cond Detector tab on the Chromeleon 6 8 panel tabset 2 Under Detector Settings click Calibration The Wellness panel opens see Figure 9 50 ES Conductivity Detector Wellness External Conductivity Cell Calibration Update Wellness Database Press for instructions Instructions Press for instructions Instructions Cond Cell Calibration Calibrate Settings to Download Current X Log Cell 1 Cal Value Log nownload in Process Log Cell 2 Cal Value Log Cell Serial Number Current Calibration Date 4 22 2010 Last Calibration Date 4 22 2010 Dummy Cell Control Cell Control Normal gt Service Wellness Figure 9 50 Wellness Panel Dionex ICS 5000 Conductivity Detector Chromeleon 6 8 Version Shown 386 Doc 065446 01 11 12 9 DC Service 3 On the Wellness panel under External Conductivity Cell Calibration click Instructions
146. From autosampler fi ee _ ot CI e To waste Figure 3 3 Hybrid System Dual RFIC EG System CD Analytical CD Capillary 138 Doc 065446 01 11 12 3 Configurations 10 We pump met via we pump rear cnase __ Eluent Pump front view DC front view ump Cell In Cell Out Jajui dung lt _ 5 S L 4 Temp w f Stabilizer 6 3 On Off Valve WL Pla R AS AP j rom gt t ah To AS AP Waste Figure 3 4 Analytical IC Single System with no EG CD Doc 065446 01 11 12 139 Dionex ICS 5000 Operator s Manual Pump front view To the pump inlet via the pump rear chase SP pump not to scale TANIA Deionized Water i To waste gt From the suppressor Regen Out via the DC rear chase DC front view EG left side view EGC RFIC high pressure Eluent Degasser Cell In Cell Out Regen Out Eluent Out Za luent In Regen In Separator m 4 Backpressure Device From AS AP To AS AP Waste To Waste ee Figure 3 5 Analytical IC Single RFIC EG System CD 140 Doc 065446 01 11 12 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 mm E lol B Seal o Wash l B a 03 i pump not to sca
147. ICS 5000 Si DC Startup 4 11 Starting the DC 1 Press the POWER button on the front of the DC 2 On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the DC tab to display the DC panel see Figure 4 9 Home Sampler DP EluentGenerator DC CD Left ED Right Audit Startup Queue Qui a Detector Compartment T09 Serial Number 123456789012 us TDI Status Ready 7504 HS CD_1_Total nA EDI Cube Inj 1 oadPositi LoadPosition 5 o AM_LP1 Closed f AM_LP2 Closed Paro AM_LP3 Closed AM_LP4 Closed 500 AM_LPS Closed AM_LP6 Closed 750 Valves Relays TTL Compartment Suppressor Left Suppressor Right 5 gt 8 2 Type None v Type None Pi Set 3500 C Curent Om amp Curent fim Actual 35 00 ER Eluent ER Eluent Suppressor 1 Suppressor 2 15 80 Message Time 519 2012 34532 PM Initializing driver DP Dual Pump ICS 5000 3 5 15 2012 345 32 PM Driver DP Dual Pump ICS 5000 3 simulation mode activated 515 2012 34506 PM DC Column_TC Exclusive access finished DC 5 15 2012 34506 PM DC Compartment_TC Exclusive access finished di resse Figure 4 9 DC Control Panel Chromeleon 7 Version Shown Doc 065446 01 11 12 169 Dionex ICS 5000 Operator s Manual 3 For each of the
148. 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 Doc 065446 01 11 12 221 Dionex ICS 5000 Operator s Manual 8 3 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 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 Reproducibility Liquid l
149. Matrix Elimination page 143 Using a DP and a 6 Port Valve Analytical IC Single RFIC EG System with Matrix Elimination page 144 Using an SP and a 10 Port Valve Analytical IC Single RFIC EG System with Post Column page 145 Reagent Addition Bromate Analytical IC Single RFIC EG System with ED and VP for page 146 Carbohydrate Analysis Doc 065446 01 11 12 135 Dionex ICS 5000 Operator s Manual Deionized Water Deionized Water DC front view To pump 2 inlet via the pump rear chase Pump front view DP re psy To waste aa a a To pump 1 inlet via the pump rear chase System 2 pump not to scale To EGC A 2 In Piston Seal Wash System 1 From IC Cube 2 EG Degas Regen Out From autosampler System 1 e EGC capillary Conduct oend Coplay System 1 capillary To IC Cube 2 EG Degas Eluent ll EG right side view System 2 EGC To waste From IC Cube 1 EG Degas Regen Out Regen Out Regen In y To IC Cube 1 i EG Degas Eluent In Eluent Out To waste Regen Out gt Eluent In Figure 3 1 Capillary IC Dual RFIC EG System CD CD 136 Doc 065446 01 11 12 3 Configurations Pump front view To pump 2 inlet via the pump rear chase T
150. N 075971 10 port P N 075972 CAUTION MISE EN GARDE VORSICHT NOTE Substitution of non Dionex Thermo Scientific parts may impair valve performance and void the product warranty NOTE Electronics related repair procedures must be per formed by Technical Support for Dionex products 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 Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance Um Verletzungen zu vermeiden warten Sie bitte bis der DC abgek hlt ist ehe Sie die Tur ffnen bzw Wartungs oder Servicearbeiten durchf hren Doc 065446 01 11 12 373 Dionex ICS 5000 Operator s Manual 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 3 Open the DC door 4 Disconnect each liquid line connected to the valve 5 Unscrew the locking ring on the outside of the valve see Figure 9 36 and remove the ring Locking Ring Figure 9 36 Unscrew the Locking Ring Valve 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 37 Valve pods are keyed to fit only one way one slot is narrower than the other Verify that the slots are aligned with their matchin
151. N 079803 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 was not removed in Step 3 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 Ifthere are no bubbles repeat Step 3 Doc 065446 01 11 12 323 Dionex ICS 5000 Operator s Manual 9 7 4 Removingthe Piston Seal Wash Seal 1 Remove the O ring P N 040695 and the backup ring capillary pump P N 074371 analytical pump P N 074370 from the seal wash body 2 Follow these steps to remove the piston seal wash seal from the seal wash body a Usinga 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 scratc
152. Nday s Examples 31 Dec 1999 current 1year 6months Invalid enumerated value Warning page 290 Next qualification of this module is due in x Warning page 291 day s due date is date Next qualification of this module is overdue due Warning page 291 date was date Next qualification of this module is overdue due Error page 291 date was date Module may no longer be used Next qualification of this module was due on Warning page 291 date Allowing x more grace day s Next service of this module is due in x day s Warning page 291 due date is date Next service of this module is overdue due date Warning page 291 was date No chip card in the reader for the column x Error page 292 No response from x for x seconds Warning page 292 No response from x for x seconds Device Abort page 292 disconnected Table 8 4 TC Error Messages Continued Doc 065446 01 11 12 215 Dionex ICS 5000 Operator s Manual TC Related Audit Trail Error Message Default Severity Level Operating columns above 70 C could affect Warning page 293 column performance Verify recommended column operating conditions before setting temperature above 70 C Parameter x value exceeded its allowed range Warning page 293 Set to closest valid value y Primary property x is already assigned and Error page 294 cannot be changed Properties cannot be changed A
153. Neutralization device AThermo Scientific Dionex 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 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 detectors e Injection valves 6 Doc 065446 01 11 12 1 Introduction e Switching valves e Guard and separator columns e Suppressors e Dionex ICS 5000 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 Thermo Scientific Dionex Chromeleon 6 8 Chromatography Data System release 6 8 SRIle or later the ED is also capable o
154. New CR TC Plumbing 359 9 16 Replacing the RFIC Eluent Degasser 361 9 17 Installing a Backpressure Coil 361 9 18 Changing the EG Main Power Fuses 02 0 000 363 DC SErViCe errati aid neh tt 365 9 19 Replacing Tubing and Fittings LL 365 9 19 1 Tubing and Fittings for Capillary IC Systems 365 9 19 2 Tubing and Fittings for Analytical IC Systems 368 9 20 Connecting a Sample Loading Port to the Injection Valve 369 9 21 Replacing the Leak Sensor 370 9 22 Rebuilding a High Pressure Injection Valve 372 9 23 Replacing a High Pressure Injection Valve Pod 373 9 24 Installing or Replacing an I O Option Board 376 9 25 Changing the DC Main Power Fuses 0200 0005 377 9 26 IC Cube Service Procedures susino 379 9 26 1 Replacing an IC Cube Cartridge 379 9 26 2 Replacing Capillary Columns 2 4 380 9 27 CD Service Procedures illa ita 386 9 27 1 Calibrating the CD Cell 00 00 0008 386 9 27 2 Replacing an Analytical Suppressor 387 927 3 R placing a CD vias stapia a E bri 389 xii Doc 065446 01 11 12 Contents 9 27 4 Removing Trapped Air from the Conductivity Cell 390 9 28 ED Service Procedures LL 391 9 28 1 Disconnecting the ED Cell 391 9 28 2 Replacing an ED Ce
155. Not Run Electrical connections incorrectly installed There may be a problem with the connections from the vacuum degassing module to the CPU board For assistance contact Technical Support for Dionex products NOTE The Dionex ICS 5000 IC system electronics compo nents cannot be serviced by the user 242 Doc 065446 01 11 12 8 DP SP Troubleshooting 8 18 DP SP Digital I O Port Inoperative TTL input related error l 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 065446 01 11 12 243 Dionex ICS 5000 Operator s Manual 244 Doc 065446 01 11 12 a 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 Th
156. 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 that 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 for details e For tightening requirements for the 10 32 fitting bolt P N 074449 and 10 32 double cone ferrule P N 074373 see Section 9 2 Doc 065446 01 11 12 367 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 Dionex PEEK 1 in AS AP waste port located near the injection port
157. 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 tubing 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 AAA 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 049135 GM 4 Static Mixer 074373 Ferrule fitting 10 32 double cone 074449 Fitting bolt 10 32 for double cone ferrule fitting 062511 Ferrule fitting 1 16 in 052230 Fitting bolt 1 16 in 042772 Plug 079803 Syringe 10 cc 442 Doc 065446 01 11 12 B Reordering Information Part Number Item 954773 Fuse IEC 60127 2 slow blow rated at 2A 250V 063246 USB cable 1 m 3 ft long 005 9001A Cinch connector 2 pin Maintenance Kits 075970 DP SP Analytical Annual Preve
158. Queue ICS 5000 Injection Number Run Time Chromeleon Administrator Sequence Method 1000 pal Pump_1_Pressure 800 HS CD_1 pus CD_1_Total 6003 28 Pump_2_Pressure nA Sn D1 A 3 so0d ED_1_Total re zoo Pump Top Bor Prime 2 010 200 0 100 ml min mA 400 Opsi Jy Pump Bottom 600 JB oii 200 010 ri 0 100 ml min mA 1000 7 x m 0 00 1 25 2 50 3 75 5 00 6 25 7 50 895 10 00 DP o ipsi k Q Q IC Cube Right U Q 3500rc 3500 EGC Left EGC Righ U LoadPosition N 7 CDTot Left Compartment EDTot Right DCAmp 00 1 00 15 00 C Injection State Off 3 926 5 i 000 lEscs cKO Cell Heater 35 00 C AgCI Vial Position RAT Suppressor Lel uppressor Right z DS Injection Type PushFull Wom mpm Left Valve Right Valve 0 00 mM 0 00 mM Injection Volume 25 0 Vai DI to ile lerale bs olumn bs S Mea oorge amp ta TB BOI ASAP DC LoadPosition LoadPosition EG lt mm Figure 4 3 Example Chromeleon 7 ePanel Set 156 Doc 065446 01 11 12 4 Startup 4 5 4 5 1 4 5 2 Starting Chromeleon 6 8 NOTE All references in Chromeleon to Dionex ICS 5000 systems apply equally to Dionex ICS 5000 systems Starting the Chromeleon 6 8 Server To start the Chromeleon 6 8 Server right click the Chromeleon Server Monitor icon Se which is crossed out in red on the Windows taskbar and click Start
159. Rear panel EG 48 Exhaust fan 48 Index 14 Doc 065446 01 11 12 Index Fuse cartridge 49 Gas vent line 49 50 Power switch 49 USB connections 48 Waste lines 49 50 Rear panel TC Description 123 Digital I O connectors 124 Fuses 123 Power switch 123 USB connections 125 Waste line 125 Rear seal wash See Piston seal wash system Recorder Analog output setting 89 Calibrating 89 Recycle mode 76 Redox reactions 80 Reference electrode 78 Contaminated 276 Faulty 278 Leaking 278 Preventing from drying out 81 Reordering information 448 Shutdown procedure 191 Reference Library DVD 13 Reference potential shift 81 278 Regulator Bracket Kit TC VWD PDA 36 Regulator Kit EO 36 Relay connectors DC 85 87 Configuring 90 Relay outputs DC 85 Controlling 92 Reordering information DC 447 DP SP 441 EG 445 TC 451 Reprocessing amperometry data 113 Reproducibility Affected by amperometry cell pH 81 Affected by temperature changes 73 Reproducibility is poor 222 Reservoirs eluent 35 Cleaning 218 223 311 Installation in EO 6 35 36 Pressurizing 35 Retention time Troubleshooting 224 Variations 122 Reversed phase solvents 79 RFIC Eluent Degasser 46 50 Gas vent line 49 Leaks 258 259 Pressure requirements 5 147 Replacement procedure 361 Tubing rupture 5 147 227 259 RFIC ER 5 RFIC ESP 6 Running samples 176 See also Sample processing S
160. Replace the Dionex EGC see Section 9 14 e Electrical error The EG current and or voltage may have become unstable Contact Technical Support for Dionex products for assistance NOTE The Dionex ICS 5000 IC system electronics compo nents cannot be serviced by the user 8 21 EG POWER LED Fails to Light e No power Check that the POWER button on the front of the EG is turned on Check that the EG main power switch on the rear panel is turned on Check that the main power cord is plugged into both the EG rear panel connector and the power source Check that the wall outlet has power If the POWER LED still fails to light contact Technical Support for Dionex products for assistance 8 22 Liquid Leaks in the EG e Leaking fitting Locate the source of the leak Tighten or replace liquid line connections as needed see Section 9 12 258 Doc 065446 01 11 12 8 EG Troubleshooting Analytical IC 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 Dionex EGC see Section 9 14 Analytical IC only RFIC Eluent Degasser leaks Replace the analytical IC system Dionex RFIC Eluent Degasser see Section 9 16 8 23 No Flow MEN 9 IC DP SP power is off Turning off the DP SP automatically turns off the EG and the suppressor Current to th
161. TL inputs respond to four types of signals allowing them to accommodate a variety of Normal edge Inverted edge controlling devices The default control type Normal pulse Normal edge is compatible with the output signals Inverted pulse provided by Dionex 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 Doc 065446 01 11 12 95 Dionex ICS 5000 Operator s Manual 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 40 Normal Edge In normal edge operation the negative falling Action Off or No Effect sv 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 detector and the rising edge stops it For the detector mark and offset functions the falling edge turns on the function and the rising edge has no effect I
162. TTL outputs from the DC ePanel in Chromeleon 7 see Figure 2 38 or the DC Control panel in Chromeleon 6 8 Home Sampler DP EluentGenerator DC CD Left ED Right Audit Startup Queue DC Relays Inputs Relays Inputs DC 5000 Instrument 1CS 5000 Output Relays and TTLs Input TTLs CD_I CD_1_Total DC_TTL2 DC_Relay_1 DC_Relay_2 DC_ACRelay_1 TTL2 TTL3 TTL4 TTL TILE DE_TTLI Ta _ EDI ED_1_Total TIL DC_ACRelay 2 ma AM_LP3 Closed f AM_LP4 Closed AM_LPS Closed f AM_LP6 Closed Valves Relays TTL Compartment _ 7 1 6 0 8 0 10 9 Column n wo Set 300 C a 20 00 gt O n 10 2 10 70 Suppressor Left Suppressor Right IC Cube Left 2 2 e oc Type None v Type None v Set 35 00 C Curent Om Curen Om Actual 35 00 ER Eluent ER Eluent 15 80 Ss inca 1 Suppressor 2 e ae ati Aeg store n I a Act n ratori A sorta Figure 2 38 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 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 e Injection valves left and right load inject e AM high pressure valves A
163. Turn the Dionex 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 Dionex EGC in the holder For a standard pressure analytical Dionex EGC Remove the 10 32 plug from the vent opening and reinstall the luer adapter and vent line Doc 065446 01 11 12 353 Dionex ICS 5000 Operator s Manual For a high pressure analytical Dionex EGC Reinstall the vent line Unscrew the fitting on the top of the Dionex EGC a few turns to allow venting of the EG To ensure proper ventilation always loosen the fitting on the top of the high pressure analytical Dionex EGC before operation 9 15 9 15 1 10 Reconnect the Dionex EGC electrical cable Replacing the CR TC The Dionex CR TC replacement procedure consists of e Removing the old Dionex CR TC see Section 9 14 1 e Installing and hydrating the new Dionex CR TC see Section 9 15 2 e Completing the plumbing for the new Dionex CR TC see Section 9 15 3 See Figure 9 18 for a flow schematic of the EG and Dionex CR TC for capillary IC See Figure 9 22 or Figure 9 23 for a flow schematic for standard pressure or high pressure analytical IC respectively Removing the Old CR TC 1 Turn off the pump flow This turns off the power to the Dionex EGC and the suppressor also 2 Open the front door of the EG 3 Push down on the slide release latch and pull the tray forward until
164. Unscrew the black locking ring on the front of the valve see Figure 9 77 and remove the ring Grasp the front of the valve pod and pull out firmly to remove it from the TC Figure 9 77 Unscrewing the Locking Ring Check that the new pod has the correct number of ports for the injection valve being serviced Align the slots in the new pod with the runner in the valve holder in the TC see Figure 9 78 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 418 Doc 065446 01 11 12 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 78 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Figure 9 78 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 p
165. Warning threshold must be higher 300 Warning threshold must be lower 300 Index 8 Doc 065446 01 11 12 Index X position error 302 You do not have the privilege 302 eWorkflows Chromeleon 7 177 Creating a new sequence 177 External low pressure valves DC 85 External Seal Wash Kit 27 160 442 F Filter end line Bacterial contamination 200 Installation Maintenance 199 Filter inline 37 Fittings DC Replacing 365 Requirements 365 Fittings DP SP Replacing 309 Requirements 309 Fittings EG Replacing 335 Requirements 335 Fittings TC Replacing 413 Requirements 413 Flow restrictions 200 Flow schematics Conductivity detection suppression recycle mode 76 77 High pressure valves AM 99 IC Cube for conductivity detection 62 IC Cube for electrochemical detection 63 Injection valve DC 10 port valve 71 Injection valve DC 4 port valve 69 Injection valve DC 6 port valve 70 Injection valve TC 10 port valve 127 Injection valve TC 6 port valve 126 Low pressure valves AM 100 System configurations 135 146 Front description DC Buttons and LEDs 55 56 Front description DP SP Buttons and LEDs 21 22 Front description EG Buttons and LEDs 39 40 Front description TC LEDs 119 120 Full scale analog output 89 Response range 88 Voltage output ranges 88 Fuses DC 84 Replacement procedure 3
166. able in the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 Information on the column ID chip card is continuously updated as long as the column and the chip card are installed in the TC Column Properties Two types of information can be stored on the column ID chip card e Primary column properties are entered once by the column manufacturer or the user and are never changed during the lifetime of the column The primary properties are the product ID serial number batch lot number date of manufacture and custom information e Secondary column properties are entered by the user and can be changed whenever required by any Chromeleon 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 065446 01 11 12 129 Dionex ICS 5000 Operator s Manual 2 25 Gas and Humidity Sensors The TC contains two sensors that will detect any gas or humidity that may accumulate inside the TC When a certain concentration of gas or humidity is reached while the door is closed the following events occur The corresponding sensor is activated The ALARM LED on the front of the TC lights red and remains red as long as the sensor is exposed to gases or humidity The error is logged in the Chromeleon audit trai
167. abset click the TC tab to display the TC panel see Figure 4 10 Home DP TC Audit Startup Queue Orr F i Status Temperature Control n 120 09 RES ra puo ee TC Temp Door tiesed z psi Pump_1_Pressure Set Temperature 200 C T psi Pump_2_Pressure Ten Cortot On Temperature Ready Delta 1 0 C E ane vm Gas NoLeak e A une Haak Left Valve Right Valve D load Lod g 6 Ta Ri J More Settings Position Load Position Load 50 04 More Options 37 54 Wellness 25 04 Service Column Details i Qualification 12 5 min Relays Inputs ecc i 0 0 2 0 4 0 6 0 8 0 10 1 Date TOSSE pa gt EE E SORGE geen geome 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 Setthe temperature required for the application Doc 065446 01 11 12 173 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 or Chromeleon 6 8 panel tabset verify that the TC temperature is at its set point and is stable 2 Monitor the pump pressure to make sure it is at the expected reading for the installed column and i
168. 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 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 Select the pump name Select the Degasser property and select Off For Chromeleon 6 8 click Execute Oy Ri 0 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 specifications 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 the
169. ached cable e Disconnect are out of the opening cables 6 The cable attached to the leak Lod X E sensor connects to a cable inside the DC Continue pulling the cable until the connectors ge _ _ for the two cables are outside the panel see Figure 9 35 A Figure 9 35 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 Doc 065446 01 11 12 371 Dionex ICS 5000 Operator s Manual 10 Make sure the leak sensor does not touch the bottom of the drip tray 9 22 Rebuilding a High Pressure Injection Valve Thermo Fisher Scientific recommends rebuilding the injection valve annually The Injection Valve Rebuild Kit 4 port valve P N 074698 6 port valve P N 075973 10 port valve P N 079054 contains all required replacement parts To obtain a Valve Rebuild Kit order the appropriate Maintenance Kit e 0 4 uL Internal Loop High Pressure Valve Maintenance Kit P N 075040 e 6 Port High Pressure Valve Maintenance Kit P N 075974 e 10 Port High Pressure Valve Maintenance Kit P N 079053 The injection valve rebuild procedure also applies to high pressure valves installed in an Dionex ICS 5000 Automation Manager NOTE Substitution of non Dionex Thermo Scientific parts may impair valve performance and void the product warranty NOTE Replac
170. 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 065446 01 11 12 111 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 EI Waveform Gold IPAD 2 o M Description Amino Acids Ag AgCl Ref 7 Reference Electrode Mode pH ij 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 carboh
171. al Dionex EGC go on to Section 9 14 5 IC 342 Doc 065446 01 11 12 9 EG Service ES 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 Dionex EGC and CR TC service procedures in a capillary IC system Tubing Assembly Key o 0 25 mm 0 010 in ID black Vent PEEK 86 cm 34 in P N 068658 E 0 062 mm 0 0025 in ID blue IA PEEK 18 cm 7 in P N 072204 0 062 mm 0 0025 in ID blue 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 gt WASTE GAS SEPARATOR EG Degas Regen Out Cartridge blue label inside DC 3 To Inject Valve Figure 9 18 EG Flow Schematic Example for Capillary IC Systems Ber Flushing the Capillary EGC 1 Remove the new Dionex EGC from the shipping container NOTE Save the shipping container it may be required for storage or disposal of the Dionex EGC Doc 065446 01 11 12 343 Dionex ICS 5000 Operator s Manual Verify that the vent fitting on top of the Dionex EGC is tightened Turn the cartridge upside down and place it on the EG drip tray Remove the plugs from the INLET and OUTLET fittings on the eluent generation chamber Locate the 38 cm 15 in piece of 0 025 mm 0 0
172. and B A B e AM low pressure valves A and B open closed e DC low pressure valves A through F on the rear panel open closed 92 Doc 065446 01 11 12 2 DC Description 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 Manager or the Chromeleon 6 8 Server Configuration program You can assign one or more functions to each input NOTE If two instruments or timebases are sharing the DC the TTL input functions are shared between the instruments or timebases For example if TTL input 1 is assigned to control injection valve 1 in the Chromeleon 7 that function is assigned to both instruments You do not need to associate a TTL input with a particular instrument To select TTL input control functions 1 Open the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program 2 Double click the DC icon under the instrument or timebase Doc 065446 01 11 12 93 Dionex ICS 5000 Operator s Manual 3 Select the TTL Inputs tab see Figure 2 39 Dionex DC Detector Chromatography General Detectors High Pressure Valves TTLs Relays AC Thermal Controls Suppressors
173. and will reset 288 Firmware download in progress 289 Gas leak detected 289 Humidity leak detected 289 Illegal parameter 290 Injections limit has been exceeded 298 Injections limit will be exceeded 298 Invalid date time format 290 Invalid enumerated value 290 Next qualification is due 291 Next qualification is overdue 291 Next qualification was due on 291 Next service is due in 291 Next service is overdue 291 No chip card in reader 292 No response from x 292 Nominal temperature must be set 298 Nominal temperature value out of range 298 Operating columns above 293 Oven not fully operable 298 Parameter x value exceeded 293 Primary column ID property 299 Primary property x already assigned 294 Properties cannot be changed 294 295 Raw data file x cannot be created 295 Raw data file x cannot be written 295 Starting data acquisition manually 296 TC firmware download failed 281 TC is not remote 286 The command can format 296 There was already an AcqOff 300 There was already an AcqOn 300 This function cannot be adjusted 301 This operation may affect 301 Two AcqOn commands for channel 300 Unknown error code 301 Unknown format of card data 301 Upper limit must be higher 299 USB LAN communication error 287 Value for parameter is not within 293 Value x replaced by 293
174. ands dialog box Chromeleon 6 8 To troubleshoot Select a valid option from the drop down list box available for this property 290 Doc 065446 01 11 12 8 TC Troubleshooting Next qualification of this module is due in x day s due date is date Or Q 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 Q 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 mon
175. anel of the TC DANGER Doc 065446 01 11 12 419 Dionex ICS 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 79 Use a small screwdriver to remove the fuse cartridge Fuse Cartridge Figure 9 79 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 420 Doc 065446 01 11 12 ICS 5000 DP SP A Specifications DP SP Specifications Dionex ICS 5000 Single Pump 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 41 MPa 0 6000 psi Flow Rate Range Analytical 0 000 10 000 mL min with settable flow increments at 0 001 mL min Capillary 0 001 3 000 mL min with settable flow increments at 0 0001 mL min Flow Rate Precision lt 0 1
176. ange Comment LiOH LIOH 0 1 to 40 mM at 0 1 to 1 0 mL min The eluent flow concentration range 0 1 to XmM at 1 0 to 3 0 mL min for each cartridge is flow 50 of the range for a where X 40 flow single independent cartridge KOH Capillary 0 1 to 100 mM at 0 001 to The eluent MSA Capillary 0 01 mL min concentration range 0 1 to X mM at 0 01 to 0 1mL min for each cartridge is where X 1 flow 50 of the range for an independent cartridge Table 4 3 Eluent Concentration Ranges for Linked Dual Cartridge Configurations Continued Notes for Generating Carbonate Bicarbonate Eluent If a Dionex EGC 300 KCO and a Dionex EPM 300 Electrolytic pH Modifier are installed EGC_1 and EGC_2 respectively 1 Set EGC_1 Target Concentration to the concentration of KCO required for your application 2 Set EGC 2 Target Concentration to the concentration of KHCO required for your application The Dionex K CO cartridge generates the total of the two target concentrations and the Dionex EPM modifies the total to achieve the K C03 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 Dionex K CO cartridge generates 4 50 mM K CO indicated in the Applied Concentration field for the K CO3 EGC The Dionex EPM modifies the 4 50 mM K CO eluent to achieve the required 3 50 mM K CO3 1 00 mM KHCO3 mixture 168 Doc 065446 01 11 12
177. anium see Figure 2 32 Working Electrode Cell Body counter electrode pH Ag AgCl Reference Electrode Titanium Inlet Tubing for analytical IC Figure 2 32 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 resulting 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 Doc 065446 01 11 12 79 Dionex ICS 5000 Operator s Manual 2 15 2 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 disp
178. anual 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 fe Bicss000 Idle i la save studio Print Pup SeInsertRow APAFillDown Lock Y Filtering Grouping f Report Columns g Chromatogram gt Name Type Position Volume ul Instrument Metho Processin Status 1 None dA 1 i Unknown RAT 20 0 ASIZA Product AS124 Idle 2 None A 2 i Unknown RA2 20 0 AS124 Product AS12A Ide 3 None lo 3 i Unknown RAI 20 0 AS124 Product AS124 dle 4 None a4 i Unknown RA4 20 0 AS12A Product AS12A Idle 5 None lo 5 i Unknown RAS 20 0 AS12A Product ASTZA dle 6 None 3 6 i Unknown RBI 20 0 45124 Product AS12A Ide Thiene erre ee DLAT Product ASIZA liano Figure 5 3 New Sequence in Chromeleon 7 Using the Sequence Wizard l 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 then 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 seq
179. application See 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 41 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 Doc 065446 01 11 12 97 Dionex ICS 5000 Operator s Manual The AM is available in the following configurations Components Included Part Number Two 10 port high pressure valves 075950 Two low pressure 3 way valves One 10 port high pressure valve 075951 One low pressure 3 way valve One 6 port high pressure valve 075952 One low pressure 3 way valve AutoPrep configuration 075953 10 port high pressure valve AutoPrep sample loop AutoPrep standard loops AM tray with no valves 079833 Table 2 6 AM Configurations 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 075917 High pressure valve 10 port 075918 Low pressure valve 3 way 061971 Low pressure valve 2 way 079848 RCH 1 Reaction Coil Heater 079849 Temperature stabilizer standard bore 0 25 mm 062561 0 010 in ID Temperature stabilizer microbore 0 125 mm 062562 0 005 in ID Table 2 7
180. arrow bore PEEK inlet tubing for capillary format titanium inlet tubing for analytical format Compatible with 0 2 to 0 6 mm ID columns PEEK inlet 2 to 7 mm ID columns titanium inlet Working Electrodes 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 Full scale of 10 100 or 1000 mV user selectable Cell Volume at Working Electrode lt 0 2 uL Maximum Cell Operating Pressure 0 7 MPa 100 psi System Software Software Chromeleon Chromatography Data System requires Microsoft Windows 7 Windows Vista or Windows XP Doc 065446 01 11 12 A DC Specifications Dionex ICS 5000 Electrochemical Detector Specifications Continued 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 Chromeleon 6 8 only Three dimensional display of the raw integrated amperometry data set with crosshairs
181. arting the Chromeleon 7 Instrument Controller Service 155 4 4 2 Starting the Chromeleon 7 Client 155 4 5 Starting Chromeleon 6 8 157 4 5 1 Starting the Chromeleon 6 8 Server 157 4 5 2 Starting the Chromeleon 6 8 Client 157 DP SP Startup iosre nea rea 159 4 6 Setting Up the Eluent Reservoirs L 00 cece ee eee 159 4 7 Setting Up the Piston Seal Wash System 160 g Startinp the Pump o i ses efor a taser hie Pape da en 163 EG Startup root L a aN 165 4 9 Entering the Eluent Concentration LL 165 4 10 Selecting the Eluent Concentration 2 0 ann 166 DC Startup ii lei 169 4 11 Starting the DCs reale ra 169 4 12 Equilibrating the System and Verifying Operational Readiness 170 TG Start p 255 3 dees nEn EEE eb VEA a 173 4 13 Starting the TE iatale Aia dana ged ace ione 173 Doc 065446 01 11 12 Vv Dionex ICS 5000 Operator s Manual 4 14 Equilibrating the System and Verifying Operational Readiness 174 5 Operation 5 1 Controlling Modules Directly 0 175 5 2 Analyzing Samples 176 5 2 1 Creating a New Sequence in Chromeleon 7 177 5 2 2 Creating a New Sequence in Chromeleon 6 8 178 5 2 3 Starting a Sequence 180 5 3 Loading Samples into the Sample Loop or Concentrator 182 5 3 1 Loading Samples with an Autosampler 182 5 3 2 Loading Samples with a Syringe
182. at which the pressure drops abnormally indicates the point of restriction If the Dionex EGC is the source of the high backpressure replace the outlet frit as instructed in the Dionex EGC manual The manual is provided on the Thermo Scientific Reference Library DVD P N 053891 3 Ifthe restriction has caused such high pressure that the system cannot be operated you must work forward through the system adding parts one at a time until an abnormal pressure increase and hence the restriction is found 9 14 Replacing the EGC Replace the Dionex EGC when the cartridge is expended or when it leaks See Table 2 3 for a list of the Dionex EGC models that can be used with the Dionex ICS 5000 EG Standard pressure analytical IC systems require Dionex EGC 300 cartridges lc Operation with high pressure analytical IC systems typically requires Dionex EGC 500 cartridges NOTE Although it is possible to operate a high pressure analytical system with a Dionex EGC 300 cartridge this will limit the operating pressure to 35 MPa 5000 psi The Dionex EGC replacement procedure consists of e Removing the old Dionex EGC see Section 9 14 1 e Disposing of the old Dionex EGC see Section 9 14 2 e Installing and conditioning a new capillary Dionex EGC see Section 9 14 4 338 Doc 065446 01 11 12 9 EG Service CAUTION MISE EN GARDE VORSICHT Installing and conditioning a new analytical Dionex EGC see Section 9 14 5
183. ate the status of several pump functions see Figure 2 1 and Figure 2 2 FLOW PRIME FLOW PRIME ee eS 0 O CONNECTED ALARM Y PUMP 1 A PUMP 2 Figure 2 1 DP Status Bar FLOW PRIME e e le CONNECTED ALARM V PUMP 1 Figure 2 2 SP Status Bar Doc 065446 01 11 12 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 DP SP 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 DP SP see Section 9 5 The LED indicates whether the pump is being primed The pump is being primed POWER Use this POWER button for routine on off control of the DP SP When the power is on this LED is lighted To turn off the DP SP press and hold this POWER button for 2 seconds Note The main power switch is on the rear panel Does not flash Pump 1 is always installed in the lower half of the DP SP enclosure This button is not present on the SP 22 Doc 065446 01 11 12 2 Description 2 2 DP SP Int
184. ating pressures above 21 MPa 3000 psi 46 Doc 065446 01 11 12 2 EG Description 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 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 Dionex components are provided e Two EGCsorone EGC and one EPM and e Two CR TCs When operating with a Dionex EGC 300 K CO and the Dionex EPM 300 the Dionex EGC is connected to the Dionex EGC power supply for one channel and the Dionex EPM is connected to the Dionex EGC power supply for the second channel Thus the EG can accommodate only one such configuration Doc 065446 01 11 12 47 Dionex ICS 5000 Operator s Manual 2 8 EG Rear Panel Figure 2 13 illustrates the rear panel of the EG Exhaust Fan o 8 6 O O Exhaust Fan Gas Vent Lines USB Receptacle B Connector USB Ports 2 A Connectors Fuse Holder Main Power Switch and Power Receptacle Tubing for Connecting to Suppressors Tubing Chase Drain Port Figure 2 13 EG Rear Panel The exhaust fan cools the interior of the EG and exhausts any oxygen and hydrogen gases
185. ation de danger imm diat qui si elle n est pas vit e entrainera des blessures graves a 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 entra ner 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 ACHTUNG Bedeutet eine m gliche Gef hrdung Mi achtung kann zum Tod oder schwerwiegenden Verletzungen f hren WARNUNG 16 Doc 065446 01 11 12 1 Introduction Bedeutet eine m gliche Gef hrdung MiBachtung kann zu kleineren oder mittelschweren Verletzungen fuhren Wird auch verwendet wenn eine Situation zu schweren Sch den am Ger t f hren kann jedoch VORSICHT keine Verletzungsgefahr besteht Notes Informational messages also appear throughout this manual These are labeled NOTE andare 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 ay Sections preceded with the Capillary IC flag indicate that the
186. ature 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 298 Doc 065446 01 11 12 8 TC Troubleshooting To troubleshoot 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 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 col
187. c 065446 01 11 12 Index 3 Dionex ICS 5000 Operator s Manual Piston seal wash activation 162 Predictive Performance 133 Programs 176 Quantification methods 180 Sequence Wizard 178 179 Sequences creating 178 Server Configuration program 87 414 Temperature compensation CD 73 TTL input assignments 93 Chromeleon 7 10 Analog pressure output 34 Column properties for column ID system 129 Controlling power relays and TTL outputs 92 Direct control commands 175 ePanel Set 10 155 ePanel Set displaying 175 Installation manual 13 Instrument Configuration Manager 87 414 Instrument methods 176 Instrument methods creating 176 Piston seal wash activation 162 Predictive Performance 133 Processing methods 178 Quick Start Guide 13 Sequence Wizard 177 178 Sequences creating 177 Temperature compensation CD 73 TTL input assignments 93 Cinch connector Pin assignments 33 CMMS 74 Column clips Reordering 451 Column ID chip card 122 129 Reordering 451 Slots for installation 122 Column ID system 129 Chip card readers 122 Installing a chip card 415 Selecting a column 414 Selecting column properties 415 Column open circuit 264 Column over safe temperature 264 270 Column properties Primary 129 294 299 Secondary 129 Selecting for column ID system 415 Columns Sizes available 65 Commands AS AP Autosampler control 185 AS DV Autosampler control 185 Creating a progra
188. 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 To troubleshoot 1 Check the buffer selection Doc 065446 01 11 12 267 Dionex ICS 5000 Operator s Manual 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 l 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
189. cal 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 40 Doc 065446 01 11 12 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 0 O Slide Release Latch 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 065446 01 11 12 41 Dionex ICS 5000 Operator s Manual EGC 300 Analytical RFIC Eluent Degasser for Analytical IC only Electrical Cables CR TC Analytical Drip Tray O 0 8 Slide Release Latch Figure 2 10 Example EG Interior Components for an Analytical Standard Pressure IC System System 2 of a Dual Channel EG Shown 42 Doc 065446 01 11 12 2 EG Description EGC 500 Analytical RFIC Eluent Degasser for Analytical IC only Electrical Cables CR TC Analytical Drip Tray O 0 O Slide Release Latch we pub Figure 2 11 Example EG Interior Components for an Analytical High Pressure IC System System 1 Shown Eluent Generator Cartridge EGC Table 2 3
190. cess to additional functions for each module and detailed status and diagnostics functions Figure 1 2 shows the Home panel in Chromeleon 7 and Figure 1 3 shows the Home panel in Chromeleon 6 8 Home Sampler DP EluentGenerator DC CD Left ED Right Audit Startup Queue 1CS 5000 Injection Number Run Time Chromeleon Administrator Sequence Method 1000 p i Pump_1_Pressure 800 pS CD_1 uS CD_I_Totel 6004 2 Pump_2_Pressure ne i ED_I _ sod A ED_1_Total 9 200 Pump Top Woi 2 0100 g 200 0 100 ml min ith o Pian psi J Pump Bottom 600 WB oft Soa 010 tin 0 100 ml min mA 1000 x 3 0 00 1 25 2 50 3 75 5 00 6 25 7 50 2 75 10 00 DP Dips g Q Q 1 emr e 99 gt IC Cube Right 35 00 c 35 00 EGC Left EGC Right U LoadPosition v s a lr CDTot Left Compartment EDTot Right DCAmp 0 00 fr T 15 00 C Injection State Off 3 926 nS re 0 000 Gc 50 Cell Heater 35 00 C ell Heater ra ll s Ast Vial Position RAT Suppressor Left uppressor Right om m of Injection Type PushFull mpm E a 2 Left Valve Right Valve 0 00 mM 0 00 mM Injection Volume 25 0 Vv VV CR TC CRTC io Column a S ot or nil Pei 30 00 C 8 30 00 Gi me gt AS AP DE LoadPasition _ LoadPesition EG ow lt I E Figure 1 2 Chromeleon 7 ePane
191. chip card has Error page 294 not been inserted properly Check the CardState property for all cards and reinsert those indicating BusBlocked Properties cannot be changed if the Error page 294 compartment door is open Properties cannot be changed there is no card Error page 295 in the card reader Raw data file x cannot be created Warning page 295 Raw data file x cannot be created Continuing Warning page 295 with network failure protection Raw data file x cannot be written Warning page 295 Raw data file x cannot be written Continuing Warning page 295 with network failure protection Starting data acquisition manually will overwrite Warning page 296 any data which has been acquired so far TC Firmware download failed Abort page 281 TC is not remote Abort page 286 The command can format only chip cards with Error page 296 an invalid data structure The communication interface is closed Error page 296 Reconnect the instrument The compartment door is open a batch or a Warning page 297 program may need to wait until the door has been closed Please close the door Table 8 4 TC Error Messages Continued 216 Doc 065446 01 11 12 8 Troubleshooting TC Related Audit Trail Error Message Default Severity Level The counter name value x has exceeded its Warning page 297 limit y Module should no longer be used Replace the name
192. cid eluents for isocratic separations on standard bore columns Doc 065446 01 11 12 5 Dionex ICS 5000 Operator s Manual 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 Regulator Accessory and Stand P N AAA 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 a Thermo Scientific Dionex Auto
193. conds and then turn it on again If the error message appears again 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 Checkall 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 If the message appears again the vacuum degassing module should be replaced Contact Technical Support for Dionex products for assistance 232 Doc 065446 01 11 12 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
194. cted EGC 1 The Dionex EGC is on andis 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 Doc 065446 01 11 12 39 Dionex ICS 5000 Operator s Manual 2 7 Button LED If the LED Is On Comment Label CR TC 1 The Dionex 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 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 Interior 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 analyti
195. cterial 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 Dionex 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 Before injection pretreat samples that may contain high concentrations of interfering substances by putting them through Thermo Scientific Dionex OnGuard cartridges Refer to the installation and troubleshooting guide for the OnGuard cartridge for instructions The guide is provided 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
196. ction valve For details refer to the instructions provided with the inline filter 4 7 Setting Up the Piston Seal Wash System Replumbing the Seal Wash System DP only Optional The standard piston seal wash system is designed for use with only one of the two pumps in a DP module When the DP is shipped from the factory 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 160 Doc 065446 01 11 12 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 th
197. ctrolyte 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 Dionex 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 Doc 065446 01 11 12 341 Dionex ICS 5000 Operator s Manual and membranes nonhazardous however check your local state and federal regulatory agency regulations for proper disposal 9 14 3 Storing the Old EGC If the Dionex EGC is not expended follow these steps to prepare the cartridge for storage 1 Plug all fittings Tighten the vent fitting capillary Dionex EGC or high pressure analytical Dionex EGC or cap the vent port standard pressure analytical Dionex 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 Dionex EGC or Section 9 14 5 for an analytical Dionex EGC Bo If you are replacing a capillary Dionex EGC go on to Section 9 14 4 If you are replacing an analytic
198. d during a run To troubleshoot 1 Verify that the door is fully closed 2 Check for and remove any obstruction 3 Ifthe door is fully closed and the error persists contact Technical Support for Dionex products for assistance Doc 065446 01 11 12 273 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 tubing of the same length and internal diameter 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 Ifa 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 Ifthe 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
199. d 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 Waste To Waste Sample Per Carrier Eluent Figure 2 65 TC Injection Valve Flow Schematics 10 Port Valve Example Connections Large Loop to Concentrator e Inthe 10_1 position sample flows from the syringe or autosampler line through the valve and into the sample loop Excess sample flows out to waste Eluent flows from the eluent pump through the valve through the concentrator column and to the separator column If sample was previously loaded onto the concentrator column it is swept to the separator column for analysis Doc 065446 01 11 12 127 Dionex ICS 5000 Operator s Manual e Inthel 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
200. d one internal reference beam Spectral capability from 190 to 900 nm is provided by two light sources a deuterium lamp for ultraviolet detection and a tungsten lamp for visible wavelength operation The four channel detector measures at up to four wavelengths simultaneously The VWD contains a built in holmium oxide filter for wavelength verification To suppress higher order radiation two optical filters can be inserted automatically into the light path Doc 065446 01 11 12 9 Dionex ICS 5000 Operator s Manual Thermo Scientific 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 APCI and electrospray
201. d 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 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 065446 01 11 12 203 Dionex ICS 5000 Operator s Manual 7 12 DC Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The DC preventive maintenance procedure consists of rebuilding each high pressure valve installed in the module The following kits are available e 0 4 uL Internal Loop High Pressure Valve Maintenance Kit P N 075040 e 6 Port High Pressure Valve Maintenance Kit P N 075974 e 10 Port High Pressure Valve Maintenance Kit P N 079053 204 Doc 065446 01 11 12 re 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 a Technical Support Representative for Dionex products 7 13 TC Daily Maintenance e Check the TC components for leaks or spills Wipe up spills Isolate and repair leaks see Section 8 31 Rinse off any dried eluent with ASTM filtered Type I 18 megohm cm deionized water that meets the specifications listed in Section 1 5 e Check the
202. data Optional Displays a waveform plot Doc 065446 01 11 12 115 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 plot For both plot types colors are used to represent the ranges of response values The Iso view is the default view for the 3D raw data This is a top down view of the data imagine you are looking down on the data from above the plot see Figure 2 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 s 1025 10 50 1075 1100 1125 Figure 2 58 3D Amperometry Data in Chromeleon 6 8 Iso View NOTE The 3D data shown in Figure 2 58 and Figure 2 59 was col lected using an analytical waveform see Analytical vs Scanning Waveforms on page 112 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 116 Doc 065446 01 11 12 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 retention time min Lao
203. 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 Doc 065446 01 11 12 153 Dionex ICS 5000 Operator s Manual 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 4 3 4 Filling Sample Containers and Loading the Sample Tray Follow the instructions in the autosampler manual to fill sample vials or well plates and load them into the sample tray or carousel Dionex autosampler manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 Tips for Filling and Loading Dionex AS AP Vials e Fill the vials to the vial shoulder or lower Do not fill to the top e During sampling make sure the needle vent is not im
204. dout 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 meter to check the pH of the buffer e Dry pH Ag AgCl reference electrode l 2 Soak the pH Ag AgcCI reference electrode in a solution containing 1 M KCl and 1 M HCI for 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 AgcCI reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 278 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 a storage cap 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 l 2 Check the electrode by following the instruct
205. ductivity Detection Suppression in Recycle Mode Eluent from the pump flows into the injection valve After sample is loaded into the sample loop and the injection valve is toggled to the Inject position eluent passes through the loop The eluent sample mixture is pumped first through a temperature stabilizer analytical IC only through the guard and separator columns and then through the suppressor From the suppressor the mixture flows through a Dionex CRD if installed to the cell where the analytes are detected A digital signal is sent to Chromeleon 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 76 Doc 065446 01 11 12 2 DC Description chamber Flow is again routed through the Dionex CRD if installed and then to waste Figure 2 31 illustrates the flow path through an EG and a DC fora conductivity detection application using suppression in recycle mode DI WATER IN FROM PUMP EGC COND CELL For anion suppression only CRD Hi CR TC WASTE SUPPRESSOR REGEN IN EG DEGAS 7 SEPARATOR COLUMN GUARD 6 SAMPLE TEMP Eluent Flow VALVE STABILIZER L Regenerant Flow gt Ww 5 c For analytical IC only 4 ELUENT IN WASTE Inject Position Figure 2 31 EG and DC Flow Schematic for Conductivity Detection Suppres
206. e Figure 2 27 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 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 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 polyether ether ketone 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 70 Doc 065446 01 11 12 2 DC Description 2 13 3 10 Port Valve The 10 port valve P N 075918 is an optional valve available for various applications Figure 2 28 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 Dionex Application Note for more information
207. e reference electrode well and tighten it fingertight see Figure 9 63 pH Ag AgCl Reference Electrode O Ring Figure 9 64 pH Ag AgCl reference electrode O Ring Orient the cell assembly with the yoke knob on the left see Figure 9 53 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 Doc 065446 01 11 12 405 Dionex ICS 5000 Operator s Manual 9 28 7 Replacing a 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 65 Unscrew the pH Ag AgCl reference electrode Figure 9 65 Removing the pH Ag AgCI Reference Electrode Cell Configured for Analytical IC Shown 3 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 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 66 pH Ag AgCl Reference Electrode O Ring Figure 9 66 Removing the pH Ag AgC Reference E
208. e Audit Trail Standard feature System Calibration Storage Factory current and previous completely user selectable Customized Reporting Standard feature with unlimited report workbooks GLP Compliance Optional package provides security system modification history and electronic signatures 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 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 Doc 065446 01 11 12 433 Dionex ICS 5000 Operator s Manual 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
209. e Dionex 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 Theanalytical Dionex EGC requires at least 14 MPa 2000 psi of backpressure for optimal removal of electrolysis gas from the 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 Dionex RFIC Eluent Degasser has ruptured Replace the degasser see Section 9 16 Doc 065446 01 11 12 259 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 Dionex 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 tabse
210. e Dionex EGC is disconnected To troubleshoot 1 Make sure the Dionex 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 Dionex EGC control electronics may have malfunctioned NOTE The Dionex ICS 5000 IC system electronics compo nents cannot be serviced by the user 248 Doc 065446 01 11 12 8 EG Troubleshooting EG1 invalid activation date Or EG2 invalid activation date This error occurs if the activation date for the Dionex EGC is nota valid date This may indicate a problem with the memory chip in the Dionex EGC To troubleshoot 1 Make sure the Dionex 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 Dionex ICS 5000 IC system electronics compo nents and instrument control firmware cannot be ser viced by the user Doc 065446 01 11 12 249 Dionex ICS 5000 Operator s Ma
211. e Figure 9 41 and pull the cartridge out of the IC Cube 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 41 Capillary Cartridge Thumbscrews EG Degas Cartridge Shown If you are installing a Dionex suppressor or CRD cartridge hydrate them before use Refer to the instructions in the suppressor or CRD manual Doc 065446 01 11 12 379 Dionex ICS 5000 Operator s Manual 8 The manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 Reconnect the liquid lines that were disconnected in Step 4 9 26 2 Replacing Capillary Columns l 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 42 Disconnect these two lines Figure 9 42 Disconnect Capillary Cartridge Eluent Lines Loosen the two thumbscrews on the column cartridge and pull the cartridge out of the IC Cube 380 Doc 065446 01 11 12 9 DC Service 5 Lift the lid of the column cartridge to open it Figure 9 43 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 O Outlet
212. e Section 9 28 4 If you are using a disposable electrode replace it 226 Doc 065446 01 11 12 8 Troubleshooting rey e 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 Chloride Assymmetry 3 03 Phosphate Assymmetry 48 Nitrite Assymmetry 2 78 3 00 pymmetry 2 68 ps 2 00 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 8 8 Low System Backpressure e Loose fitting Make sure there are no liquid leaks in the flow system Check tubing connections throughout the system including the check valves injection valves and columns and tighten or replace fittings as needed e RFIC Eluent Degasser tubing is ruptured IC If flow from the EG waste line is normal but there is no flow through the columns the tubing assembly inside the Dionex RFIC Eluent Degasser has ruptured Replace the degasser see Section 9 16 Doc 065446 01 11 12 227 Dionex ICS 5000 Operator s Manual e 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 hav
213. e allowable eluent concentration depends on the flow rate and the Dionex EGC type This 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 Dionex CR TC is correctly plugged into the EG Push the Dionex 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 Dionex CR TC may be faulty Replace the Dionex CR TC see Section 9 15 Doc 065446 01 11 12 245 Dionex ICS 5000 Operator s Manual CR TC1 over current Or CR TC2 over current This error occurs when the current applied to the Dionex CR TC exceeds the maximum current allowed The Dionex CR TC current is automatically turned off to prevent damage to the Dionex CR TC This error may also occur if liquid flow to the Dionex CR TC is interrupted To troubleshoot 1 Check the Dionex CR TC cable connection to the electrical bulkhead see Figure 2 10 2 See Section 8 23 to deter
214. e auf der R ckseite des DC 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 38 Save the screws Remove two screws Figure 9 38 DC Rear Panel Removing the I O Option Cover Plate 376 Doc 065446 01 11 12 9 DC Service 5 Slide the new I O option board P N 062201 into the rear panel opening and press firmly to connect the board to the DC motherboard 6 Replace the two screws Figure 9 39 shows the I O option installed E PS ITITIIKKKINI MINI P HMM TITTI n 1 0 Option Figure 9 39 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 33 3 Disconnect the main power cord from both its source and from the DC rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the DC DANGER HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du DC DANGER Doc 065446 01 11 12 377 Dionex ICS 5000 Operator s Manual ACHTUNG HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite des DC The fuse
215. e been eliminated replace the Dionex EGC see Section 9 14 NOTE The EG leak sensor cannot immediately detect leakage from the membrane barrier because these leaks exit the EG through the vent line 8 9 High System Backpressure e Restriction in the system plumbing l Begin pumping eluent through the system including the columns at the flow rate normally used Work backward through the system beginning at the flow cell exit One at a time loosen each fitting and observe the pressure The connection at which the pressure drops abnormally indicates the point of restriction If the Dionex EGC is the source of the high backpressure replace the outlet frit as instructed in the Dionex EGC manual The manual is provided on the Thermo Scientific Reference Library DVD P N 053891 If the restriction has caused such high pressure that the system cannot be operated you must work forward through the system adding parts one at a time until an abnormal pressure increase and hence the restriction is found 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 228 Doc 065446 01 11 12 8 Troubleshooting ED Only Work
216. e column cartridge 13 Secure the inlet and outlet fittings on the guard column if used in the column clips on the lid of the column cartridge 14 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 15 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 49 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 384 Doc 065446 01 11 12 9 DC Service 16 17 18 19 20 21 22 and tubing are installed correctly and secured in the clips o Separator Column Outlet 2 Column Label Hoye A aaa Column Inlet Tubing Figure 9 49 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 Connect the tubing from the Eluent In port of the column cartridge to the Eluent Out port 3 of the injection valve Wait until liquid is flowing out of the Eluent Out port of the column cartridge Reconnect the line to the Eluent Out fitting on the column cartridge that was disconnected in Step 3 see Figure 9 42 Close the DC upper door
217. e of Error page 257 cartridge Pump is disconnected The EG mode is off Warning page 257 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 see the page indicated in the table DC Related Audit Trail Error Message Default Severity Level CD cell option disconnected Abort page 263 CD cell over safe temperature Abort page 264 Column temperature open circuit Abort page 264 Column over safe temperature Abort page 264 Column temperature calibration error Warning page 265 Table 8 3 DC Error Messages Doc 065446 01 11 12 211 Dionex ICS 5000 Operator s Manual DC Related Audit Trail Error Message Default Severity Level Compartment temperature open circuit Abort page 265 Compartment over safe temperature Abort page 265 Compartment temperature calibration error Warning page 265 ED cell current exceeds limits error Warning page 265 ED cell option disconnected Abort page 266 ED cell working electrode disconnected Abort page 267 ED pH offset calibration failed Warning page 267 ED pH slope calibration failed Warning page 268 ED reference electrode disconnected Warning page 268 High pressure valve 1 error Abort page 269 High pressure valve 2 error High pressure valve 3 error High pressure valve 4 error
218. e potential 106 DC Temperature Calibration Kit 67 Declaration of Conformity 19 Degassing eluents 25 Deionized water requirements 20 Detector See Conductivity Detector CD See Electrochemical Detector ED Detector output Low 228 Detector Chromatography Module DC 3 6 Alarm LED is lighted 55 Automation Manager AM 97 Column sizes accommodated 65 Conductivity Detector CD 72 Electrochemical Detector ED 78 Flow schematics 76 77 Front description 55 T O option 86 Maintenance 203 Rebuilding the injection valve 372 Service procedures 365 Spare parts 447 Specifications 429 Status bar buttons and LEDs 55 System configuration 135 Temperature control 66 See also Error messages DC Disposable working electrodes 79 Reordering 449 Drain port TC 125 Drifting baseline 219 Dual Pump DP 3 4 Analog pressure output 33 Digital I O port 32 Fuse replacement 333 Fuse specification 32 Maintenance annual 200 Maintenance daily 199 Maintenance periodic 200 Maintenance weekly 199 Operating humidity 423 Operating temperature 423 Piston replacement procedure 326 Piston seal replacement procedure 319 327 Piston seal wash tubing replacement procedure 329 Pressure limit tripped 228 259 260 Pressure limits for EG 164 Pressure limits selecting 164 Priming procedures 311 314 Priming valve knob seal replacement procedure 332 Doc 065446 01 11 12 Index 5 Dionex I
219. e primary pump head on pump 1 see Figure 4 5 item Connect the inlet line to the primary pump head on pump 2 4 When you finish these connections go to the next section to continue setting up the seal wash system Doc 065446 01 11 12 161 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 2 Place the cap on the reservoir and tighten fingertight 3 Insert the reservoir into the holder on the component panel 4 Check that the tubing is engaged in the peristaltic pump see Figure 4 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 5 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 Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 c Select the pump name 162 Doc 065446 01 11 12 4 DP SP Startup d For Chromeleon 7 click
220. e right remove the tubing and release the lever see Figure 6 1 Doc 065446 01 11 12 187 Dionex ICS 5000 Operator s Manual 188 Doc 065446 01 11 12 ss 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 Dionex CR TC suppressor etc 2 Verify that the current to the Dionex EGC and the suppressor is off IMPORTANT Supplying power to the Dionex EGC when there is no eluent flow can severely damage the cartridge 3 Store the Dionex 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 Inan analytical IC system if the EG has been shut down for more than 3 e to 4 days hydrate the suppressor as instructed in the product manual Suppressor manuals are provided 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 Dionex CR TC suppressor etc Doc 065446 01 11 12 189 Dionex ICS 5000 Operator s Manual 2 3
221. e sensitive to contamination 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 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 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 Dionex ICS Series Variable Wavelength Detector or Dionex ICS Series Photodiode Array Detector 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 AAA 074423 For instr
222. e sure the priming valve is closed see Figure 2 3 To close the valve turn the knob clockwise until closed Tighten no more than fingertight Do not use any tools to tighten the priming valve Overtightening may destroy the cap seal Open or close the priming valve only when the system pressure is down 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 065446 01 11 12 235 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 when 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 instrument method or 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 needed see Section 9 3 Be careful not to overtighten fittings 236 Doc 065446 01 11 12 8 DP SP Troubleshooting The
223. e 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 065446 01 11 12 119 Dionex ICS 5000 Operator s Manual LED Label If the LED Is On If the LED Is Flashing OVEN 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 was 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 62 120 Doc 065446 01 11 12 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 4 Guard Column Slots for Column ID Chip 1 Cards A B C and D 2 Injection Valves O Column Brackets Separator Column O Temperature Stabilizer Figure 2 61 TC Interior View Dual System Configuratio
224. e 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 Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 Doc 065446 01 11 12 301 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 Ifthe 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 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 b
225. e 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 322 Doc 065446 01 11 12 9 DP SP Service 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 l 4 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
226. e when installed with the Dionex EGC 300 K3C03 Requires a carbonate mixer 2 mm P N 063443 4 mm P N 079943 EGC 300 KOH 074532 Generates potassium hydroxide eluent for anion exchange separations EGC 300 LiOH 074534 Generates lithium hydroxide eluent for anion exchange separations EGC 300 MSA 074535 Generates methanesulfonic acid eluent for cation exchange separations EGC 300 NaOH 074533 Generates sodium hydroxide eluent for anion exchange separations Eluent Generator Cartridges for Analytical IC Systems High Pressure EGC 500 KOH 075778 Generates potassium hydroxide eluent for anion exchange separations EGC 500 MSA 075779 Generates methanesulfonic acid eluent for cation exchange separations Table 2 3 Capillary and Analytical Dionex EGCs For more information refer to the Dionex EGC manual The manual is provided on the Thermo Scientific Reference Library DVD P N 053891 44 Doc 065446 01 11 12 2 EG Description Continuously Regenerated Trap Column CR TC The Dionex CR TC is a high pressure electrolytically regenerated trap column The Dionex 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 ofthe Dionex CR TC can be used with the EG Dionex CR TC Version IC System Part Type Number Continuously Regenerated Anion Trap Column Ca
227. eaks 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 079803 to the waste port on the priming valve Open the priming valve turn the knob one half turn 222 Doc 065446 01 11 12 8 Troubleshooting counterclockwise Draw at least 20 mL of the new eluent through the liquid lines before operation e Inoperative eluent proportioning valve gradient pump only The proportioning valve assembly should be replaced Contact Technical Support for Dionex products for assistance 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 GM 4 mixer 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 there is a slimy film on the interior foll
228. eceded 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 AgCl reference electrode needs regenerating or replacing monitor the pH value displayed on the detector panel in Chromeleon see page 150 To have an alarm displayed in the audit trail if the pH exceeds certain values set pH limits in Chromeleon see page 151 Doc 065446 01 11 12 149 Dionex ICS 5000 Operator s Manual To monitor the pH Ag AgCl reference electrode pH 1 Atinstallation 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 Home Sampler DP EluentGenerator DC CD Left ED Right Aud Startup Queue Detector Settings 10005 Le ED Serial Number La EDI nA ED_1_Total Signal 0 000 200 Total Signal 0 000 60075 Mode Ref Electrode pH Rise Time Data Collection Rate 1 00 Hz z Reference Electrode AgCl 3 Waveform 200 Download Waveform Waveform 400 DC Voltage 0 000 V 5 Cell Voltage of v 600 Analog Out 3 a snap gi ascendenti a a aa IA a ttl tata Figure 4 1 Monitoring the pH Ag AgCI Reference Electrode pH 3 Thereafter monit
229. ecifica tions Continued Suppressor Void Volumes Dionex Suppressors 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 uL Anion CES 0 4 mm lt 1 0 pL Cation CES 0 4 mm lt 1 0 uL System Software Software Chromeleon Chromatography Data System requires Microsoft Windows 7 Windows Vista or Windows XP Automated Procedure Wizards Standard feature System Smart Startup and Shutdown Standard feature System Wellness and Predictive Performance Standard feature Application Templates Standard feature Automation Support of Third Party Instruments Fully controls over 300 different instruments including GC HPLC and MS from more than 30 manufacturers Customizable System Control Panels Standard feature Signal Channels Detector signals detector background signals temperatures Data Trending Plots All numerical device parameters plotted System Status Virtual Channels Standard feature Power Failure Protection Standard feature Doc 065446 01 11 12 A DC Specifications Dionex ICS 5000 Detector Chromatography Compartment Specifica tions Continued System Trigger Commands and Conditionals Standard feature Daily Audit Trail Standard feature Sampl
230. edures 413 Shutdown procedure 193 Signal cable 125 451 Specifications 439 Theory of operation 131 Trap column 5 Trap column high pressure 27 Tray autosampler Loading 152 154 Triangular waveform 110 Troubleshooting DC Amperometry cell 275 Error messages DC 263 Liquid leaks DC 274 pH readout always at 7 0 275 pH readout cannot be set to 7 0 276 pH readout nonexistent 277 Reference electrode leaks 278 Reference potential shifts 278 VALVE button not working 275 Troubleshooting DP SP Chromatographic reproducibility 222 Digital I O port not operating 243 Leak alarm 241 Liquid leaks 241 Pump does not start 239 Pump stops unexpectedly 240 Vacuum degas module low vacuum 242 Troubleshooting EG Alarm LED is lighted 257 EG stops operation 260 Leaking fittings 257 Liquid leaks 258 No flow 259 Power LED does not light 258 Troubleshooting system wide 207 High background 229 Low detector output 228 Noisy baseline 219 Retention times too early 224 Retention times too late 224 Tailing peaks 226 Troubleshooting TC Alarm LED is lighted 303 Liquid leaks 304 Temperature does not increase 305 Temperature stabilizer not operating 305 TTL and relay connectors DC 85 86 Installation instructions 87 Index 18 Doc 065446 01 11 12 Index TTL inputs DC 85 Assigning functions 93 Control types 95 Functions available 92 TTL outputs DC 85 Controlling 90 TTL
231. ee Figure 2 20 The valve has a 0 4 uL internal sample loop Figure 2 26 shows flow schematics for the 4 port valve LOAD POSITION INJECT POSITION Internal Internal Sample In Loop di In Loop gt To Column Ww c To Waste P From Pump From Pump Sample Eluent Figure 2 26 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 Doc 065446 01 11 12 69 Dionex ICS 5000 Operator s Manual 2 13 2 6 Port Valve The 6 port valve P N 075917 is the standard injection valve for analytical IC systems It is installed in the lower compartment of the DC see Figure 2 23 Figure 2 27 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 Sampl
232. een granted the appropriate privileges If you attempt to do so the appropriate message shown above is displayed 302 Doc 065446 01 11 12 8 TC Troubleshooting To troubleshoot The Chromeleon administrator is responsible for assigning 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 ALARMLED 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 Ifyou are using Chromeleon 7 Open the Command window press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Humidity leak inside the TC 1 Find and eliminate the leak 2 Ifyou are using Chromeleon 7 Open the Command window press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 3 Ventilate the interior of the TC thoroughly before closing the door and resuming operation e Failure of a mechanical component Ifa VALVE LED is flashing a mechanical component in the TC injection valve has failed 1 Replace the injection val
233. eference Potential Shift on page 278 2 Ifsoaking 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 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 a storage cap filled with saturated KCl solution See Section 4 1 2 for detailed instructions e Contaminated pH Ag AgCl reference electrode Replace the pH Ag AgCl reference electrode see Section 9 28 5 Doc 065446 01 11 12 277 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 AgcCI 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 AgcCI reference electrode with no shift Following the steps below measure the pH Ag AgCl reference electrode potential shift by comparing it t
234. efore initial use Suppressor manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 1 Stop the pump flow Doc 065446 01 11 12 387 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT 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 Afin d viter toute br lure laisser refroidir le DC avant d ouvrir la porte ou d effectuer des op rations de maintenance 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 Open the DC upper door Disconnect the four liquid lines from the suppressor see Figure 9 51 Unplug the suppressor cable from the detector Disconnect lines Thermo CSAS 300 2 mm P N 064557 w m u Figure 9 51 Disconnecting the Suppressor Liquid Lines and Cable Remove the suppressor from the detector by sliding it to the left a few millimeters to detach it from the mounting tabs on the detector Then pull the suppressor toward you Orient the new suppressor with the ELUENT IN and REGEN OUT ports on the bottom see Figure 9 51 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 t
235. ench e 0 2 micron filtered Class 10 isopropyl alcohol IPA e 0 2 micron filtered canned air duster ITW Chemtronics Ultrajet or equivalent 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 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 Doc 065446 01 11 12 315 Dionex ICS 5000 Operator s Manual 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 IMPORTANT Particles of dust dirt etc on the check valves or piston can contaminate the inside of the pump head and result in poor pump performance 7 The check valves are installed in the primary pump head see Figure 9 3 Outlet Check Valve Primary Pump Head 3 Inlet Check Valve Da META Figure 9 3 DP SP Check Valves
236. entative for Dionex products For information about maintenance procedures for the Dionex EGC CR TC trap column or suppressor refer to the appropriate product manual These manuals are provided 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 rene O Check eluent reservoir levels and refill as needed Tay O Check waste containers and empty as needed For detailed daily maintenance instructions for each module see DP SP page 199 EG page 201 DC page 203 TC page 205 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 065446 01 11 12 195 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 tubing connections Be 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 199 EG page 201 DC page 203 TC page 205 7 1 3 Periodic Maintenance O Clean eluent reservoirs when making fresh eluent or as needed see Section 9 4 O Optional Have a Technical
237. er 5 pressure 2 x gt Y emp f Amino Trap or PA20 Guard tabilizer W S Backpressure y i Device From AS AP gt p ml Pe To the CR TC Regen In via the EG rear chase To AS AP Waste lt CC From the degasser Eluent Out Figure 3 11 Analytical IC Single RFIC EG System with ED and VP for Carbohydrate Analysis 146 Doc 065446 01 11 12 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 any 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 Dionex EGC requires at least 14 MPa 2000 IG psi of system backpressure This ensures optimal removal of electrolysis gas from the eluent produced by the cartridge During system equilibration monitor the Current Pressure reading on the Pump panel in Chromeleon The pressure should remain between 14 and 35 MPa 2
238. er 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 of the DC see Figure 2 18 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 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 VORSICHT Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist 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 allow c
239. ering 448 Solvent compatibility 79 Storage 191 Troubleshooting 275 Amperometry detection See Cyclic voltammetry See DC amperometry See Integrated amperometry See Pulsed amperometry Analog output 88 Connection instructions 87 Connectors 85 86 Description 88 Full scale 89 Doc 065446 01 11 12 Index 1 Dionex ICS 5000 Operator s Manual Mark 89 Offset level 89 Polarity 89 Range 88 Recorder calibration 89 Selecting settings 88 Analog pressure output 33 Directing output to different pump 34 Analog to digital converter 88 Analytical IC applications Conductivity detector for 72 CR TC trap column for 45 Eluent generator cartridges for 44 Suppressors for 74 System configurations 135 Annual maintenance DC 197 204 292 450 DP 196 200 443 EG 202 SP 196 200 443 TC 197 206 292 451 Application Wizard 180 Application Wizard Chromeleon 6 8 178 180 Creating a new sequence 180 Applications 135 146 AS AP Autosampler 3 8 Instrument method example 185 Program example 185 Vials filling and loading 154 Well plates filling and loading 154 AS DV Autosampler 3 Instrument method example 185 Program example 185 Vials filling and loading 155 ASRS 300 74 Atlas Electrolytic Suppressor AES 65 Gas separator waste tube 75 Audit trail 22 39 Error messages 207 Icons 207 Automation Manager AM 3 97 Description 7 97 High pressure
240. erior 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 e 8 000000000 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 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 065446 01 11 12 23 Dionex ICS 5000 Operator s Manual 2 2 1 Vacuum Degas Chambers four channels Proportioning Valve Fittings Proportioning Valve Outlet to Primary Pump t Head Static Mixer Pump Outlet to a 5 EG or Injection i Valve if 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 check that the five red Phillips screws installed on the component mounting panel before shipment from the factor
241. es of potential changes is repeated over time By repeatedly pulsing between optimized high 106 Doc 065446 01 11 12 2 DC Description 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 CIRIE a 0 6 Potential ime Seconds E3 Negative Cleaning l E1 E2 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 tl the El potential is applied After a delay the signal is measured by integrating the current for a fixed time Current integrated for a fixed time is charge and the units are coulombs At t2 and t3 positive and negative cleaning pulses are added to the waveform This waveform period repeats until the end of data acquisition or until another waveform is specified Doc 065446 01 11 12 107 Dionex ICS 5000 Operator s Manual Integrated Pulsed Amperometric Detection With integrated pulsed amperometric detection IPAD current is integrated at two o
242. es per DC Temperature Zone 66 Doc 065446 01 11 12 2 DC Description Minimum temperatures are also affected by the ambient humidity If the humidity is high the minimum temperatures achieved for a temperature zone are not as low as those achieved in a low ambient humidity environment NOTE A DC Temperature Calibration Kit P N 063782 is available The kit includes the parts and instructions required to verify the temperature calibration of the DC upper and lower com partments and to recalibrate if required To set the fan speed of the DC upper compartment to high l Open the Chromeleon 7 Instrument Configuration Manager or the Chromeleon 6 8 Server Configuration program Double click the DC icon under the instrument or timebase Click the Thermal Controls tab and then double click Compartment_TC Under Fan click High Speed see Figure 2 25 DC Detector Chromatography ICS 5000 Device Configuration Device Name Compartment_TC Instrument y C Low Speed High Speed V Keep Fan On 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 cere k Cancel ppl Help Figure 2 25 Setting the DC Upper Compartment Fan Speed Doc 065446 01 11 12 67 Dionex ICS 5000 Operator s Manual 2 13 High Pressure Valves Up to four high pressure valves can be installed in the DC T
243. ess the F8 key to open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 Select the pump name Select the AnalogOut property and select PumpTop For Chromeleon 6 8 click Execute USB Connections One USB receptacle B type connector allows a connection from the PC on which Chromeleon is installed 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 Capillary or Analytical 063342 Waste and Drain Lines One waste line is connected to the secondary pump head on each pump and is routed through the tubing chase to the rear of the DP SP 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 34 Doc 065446 01 11 12 2 Description 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 l
244. ex ACES 300 Anion Capillary Electrolytic Suppressor 072053 Dionex CCES 300 Cation Capillary Electrolytic Suppressor 072055 Suppressor bypass cartridge 072054 Dionex CRD 200 Carbonate Removal Device Capillary 072056 Dionex CRD bypass cartridge Doc 065446 01 11 12 447 Dionex ICS 5000 Operator s Manual Part Number Item Conductivity Detector for Capillary IC 072041 Dionex ICS 5000 Conductivity Detector Capillary Conductivity Detector and Accessories for Analytical IC 079829 Dionex ICS 5000 Conductivity Detector Analytical 056116 Dionex AAES Anion Atlas Electrolytic Suppressor 056118 Dionex CAES Cation Atlas Electrolytic Suppressor 064555 Dionex ASRS 300 2 mm Anion Self Regenerating Suppressor 064556 Dionex CSRS 300 4 mm Cation Self Regenerating Suppressor 064557 Dionex 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
245. f To avoid damaging the suppressor and Dionex CR TC always turn them off before conditioning the Dionex EGC The pump flow is on during conditioning however no flow reaches the suppressor or Dionex CR TC 352 Doc 065446 01 11 12 9 EG Service 3 4 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 d Eluent Generator panel Enter 50 mM in the Target Concentration field This turns on the power to the Dionex EGC also e Condition the analytical Dionex EGC for 30 minutes Turn off the Dionex EGC and CR TC power Turn off the pump flow Completing the Analytical EGC Installation IC 1 Twist the ring on the Dionex EGC electrical cable counterclockwise 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 For a standard pressure analytical Dionex EGC Replace the 10 32 plug in the Dionex EGC vent opening For a high pressure analytical Dionex EGC Verify that a fitting is installed in the Dionex EGC vent opening Lift the Dionex 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 Dionex EGC OUTLET port Connect the EGC OUT line to the OUTLET port
246. f 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 Dionex ICS 5000 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 Thermo Scientific Dionex CRD suppressor guard and separator columns and EG degasser The IC Cube is installed in the upper compartment of the DC For a dual system two IC Cubes can be installed Dionex 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 Doc 065446 01 11 12 7 Dionex ICS 5000 Operator s Manual ggg Dione 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 configu
247. f 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 294 Doc 065446 01 11 12 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 cannot 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 065446 01 11 12 295 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 acqu
248. factory the seal wash system is connected to pump 1 the bottom pump If necessary connect 26 Doc 065446 01 11 12 2 Description Analytical 2 2 6 IC Analytical 2 2 7 IC the seal wash system to pump 2 the top pump instead For instructions on how to replumb the system see Section 4 7 NOTE Thermo Fisher Scientific offers an External Seal Wash Kit P N 063518 or a second seal wash system P N 068661 for users who need to operate a piston seal wash system for both pumps in the DP Static Mixer Analytical IC only For an analytical pump a 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 When a GM 4 is installed the DP SP gradient delay volume is 380 uL The gradient delay volume or dwell volume is the volume of liquid in the system between the point where the gradient is formed and the point where it enters the column This includes the mixer transfer tubing and swept volume in the injector or autosampler NOTE Thermo Fisher Scientific offers an External Seal Wash Kit P N 063518 or a second seal wash system P N 068661 for users who need to operate a piston seal wash system for both pumps in the DP High Pressure Trap Column Analytical IC only For an analytical pump a high pressure trap colu
249. for a summary of the procedure described in detail in this section 4 Disconnect the pump output line from the injection valve 5 Disconnect the line from the suppressor ELUENT OUT port to the cell inlet and connect the pump output line directly to the cell inlet 6 Verify that backpressure at the pump is at least 7 MPa 1000 psi at 0 01 mL min for a capillary pump or 1 00 mL min for an analytical pump 7 Set the cell heater to 35 C Allow the cell to reach this temperature when it does the LED stops blinking 8 Begin pumping 1 0 mM KCI through the cell at 0 01 mL min for a capillary pump or 1 0 mL min for an analytical pump 9 Wait until the total conductivity reading stabilizes 15 to 30 minutes 10 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 11 To record the new calibration value in the audit trail click Log 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 uS cm stop the pump 13 Reconnect the 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 how to prepare a new suppressor b
250. fthe new column configuration is the same as the previous one connect the precision cut tubing that you removed in Step 8 to the new columns If you are changing the column configuration see the following figures for the precision cut tubing required for your configuration 250 mm Separator 2 TN Column x 65 mm 2 5 in 0 Precision Cut Tubing O P N 072188 A 50 mm Guard a Column 115 mm 4 5 in 1 O Precision Cut Tubing P N 072189 Figure 9 46 Tubing Connections for 250 mm Separator Column and 50 mm Guard Column 150 mm Separator Column XI 75 mm 3 in 2 4 2 Precision Cut Tubing P N 074603 35 mm Guard Column Q 115 mm 4 5 in Precision Cut Tubing P N 072189 Figure 9 47 Tubing Connections for 150 mm Separator Column and 35 mm Guard Column Doc 065446 01 11 12 383 Dionex ICS 5000 Operator s Manual Separator Column A 2 210 mm 8 3 in 2 Precision Cut Tubing P N 072187 1 Use with any _ s length separator column Figure 9 48 Tubing Connections for Separator Column Only 11 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 45 12 Coil the separator column tubing inside the cartridge as shown in Figure 9 43 or Figure 9 44 Secure the column and the inlet fitting in the clips on th
251. g 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 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 VORSICHT If you select a low flow rate that allows the system pressure to drop below 14 MPa 2000 psi and you do not turn off the EG the EG will continue to generate eluent at the concentration set for the last step of the last Chromeleon 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 Dionex EGC For a complete list of operating precautions for Dionex EGCs and CR TC trap column
252. g capillary columns 380 385 Suppressors for 74 System configurations 135 Tube fitting installation 307 Tubing and fittings DC 365 Carbohydrate analysis 146 Carbonate mixer 46 Carbonate bicarbonate eluent 44 46 168 CCES 300 Capillary 61 74 CD cell disconnected error 263 CD cell over safe temperature 264 CE mark 19 cETLus mark 19 Check valve cartridges Replacement procedure 315 Chromatogram Amperometry data 115 Dips instead of peaks 89 Pulsed amperometry example 113 Water dip in 154 Chromeleon 7 10 Application Wizard 178 180 Audit trail 22 39 207 Audit trail error messages 207 Connected LED 55 Controlling external valves 85 Controlling high pressure valves 101 Controlling low pressure valves 101 Controlling switched AC sockets 84 Home panel 11 Predictive Performance 133 Starting 155 157 Troubleshooting communication problems 261 USB connections DC 84 USB connections DP SP 34 USB connections EG 48 USB connections TC 125 User s guide 13 Virtual Column Separation Simulator 176 180 Waveform Editor 112 Waveforms pre programmed 112 See also Chromeleon 6 8 See also Chromeleon 7 Chromeleon 6 8 10 Analog pressure output 34 Application Wizard 178 180 Column properties for column ID system 129 Controlling power relays and TTL outputs 92 Direct control commands 175 Installation manual 13 Panel tabset 11 157 175 Panel tabset displaying 175 Do
253. g runners 374 Doc 065446 01 11 12 9 DC Service 8 10 11 12 13 Also verify that the two splines on the pod align with the matching splines inside the valve holder see Figure 9 37 If necessary twist the end of the pod to adjust the position of the splines Valve Pod Valve Holder Figure 9 37 High Pressure Valve Pod and Pod Holder Push the pod into the holder until it clicks into place Replace the black locking ring Reconnect all liquid lines to the valve Turn on the power to the DC Turn on the pump flow Check for leaks from the valve Tighten fittings as required For tightening requirements for the 10 32 fitting bolt P N 074449 and 10 32 double cone ferrule P N 074373 see Section 9 2 Close the door Doc 065446 01 11 12 375 Dionex ICS 5000 Operator s Manual 9 24 DANGER DANGER ACHTUNG Installing or Replacing an I O Option Board l 4 Press the POWER button on the front of the DC for 2 seconds to turn off the power Turn off the main power switch on the DC rear panel see Figure 2 33 Disconnect the main power cord from both its source and from the DC rear panel HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the DC HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du DC HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchs
254. gh 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 Doc 065446 01 11 12 237 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 qualified personnel can change this parameter For assistance contact Technical Support for Dionex products Upper pressure limit exceeded This error occurs if the upper pressure limit specified in the Chromeleon 7 instrument method or Chromeleon 6 8 program is exceeded The running batch is aborted default and this message appears To troubleshoot 1 Inspect the tubing for blockage or crimping and replace it 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 Onthe Chromeleon 7
255. gh 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 valve 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 Chromeleon by clicking Connected on the Pump panel 318 Doc 065446 01 11 12 9 DP SP Service 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 e Removing the pump head and piston Section 9 7 1 e Cleaning the piston Section 9 7 2 e Removing the main piston seal Section 9 7 3 e Removing the piston seal wash seal Section 9 7 4 e Install
256. gste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist VORSICHT Tubing Chase The tubing chase routes tubing from the front of the EG through the interior of the module and to the rear panel Suppressor Vent and Drain Lines e The lines exiting the tubing chase white tubing are for connecting the REGEN IN port on the Dionex RFIC Eluent Degasser or Dionex EPM 300 Electrolytic pH Modifier to the REGEN OUT port on the suppressor e The gas vent lines clear tubing discharge the electrolysis gas H or O2 that is vented from the Dionex EGC electrolyte reservoir and the Dionex RFIC Eluent Degasser Doc 065446 01 11 12 49 Dionex ICS 5000 Operator s Manual e The drain port removes any liquid that collects in the drip tray in the bottom of the EG A clear 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 Dionex EGC Direct current is applied t
257. h 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 Seal and Seal Insertion Tool c Insert this end of the tool partway into the seal wash body Make sure the tool is centered and does not rock back and forth Then press firmly on the tool and the seal wash body until they snap together d Remove the seal insertion tool from the seal wash body 324 Doc 065446 01 11 12 9 DP SP Service 4 e The seal wash seal is now partially installed To complete the seal installation place the retainer in the seal wash body and use the large flat blade screwdriver to tighten the retainer f Place the new O ring P N 040695 on the seal wash body NOTE When replacing a piston seal always replace the O ring also This will prevent leaks g Place the new backup ring capillary pump P N 074371 analytical pump P N 074370 on the seal wash body Rinse the new main piston seal capillary pump P N 075493 analytical pump P N 075768 with isoprop
258. h your other hand wind the tubing around the rotor d Release the lever Figure 9 10 PharMed Tubing Tygon 2075 Tubing Secondary Head Piston Seal Wash Tubing Connections e Pull on 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 Turn on the pump flow Doc 065446 01 11 12 331 Dionex ICS 5000 Operator s Manual 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 l 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 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 com
259. he 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 H e 1 H3 Where the hydrogen is supplied by the following process Pd 2 Hy Pd H 4 gt Pd H ads abs 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 hydrogen 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 PAH 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 PAH 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
260. he Chromeleon 7 Instrument Controller Service right click the Chromeleon tray icon Xx which is crossed out in red on the Windows taskbar and click Start Chromeleon Instrument Controller The icon changes to gold is to indicate that the Instrument Controller Service is starting When the Instrument Controller Service is running idle the icon changes to gray Ey If the Chromeleon tray icon is not on the Windows 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 In addition a Doc 065446 01 11 12 155 Dionex ICS 5000 Operator s Manual limited number of device functions can be controlled directly from this panel and the audit trail can be accessed from here Home Sampler DP EluentGenerator DC CD Left ED Right Audit Startup
261. he following valve models are available 4 port P N 074525 6 port P N 075917 and 10 port P N 075918 7 In a capillary IC system one 4 port high pressure valve is installed in each IC Cube This valve is 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 lc 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 68 Doc 065446 01 11 12 2 DC Description 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 s
262. he suppressor to verify that it is securely fastened 388 Doc 065446 01 11 12 9 DC Service 8 9 10 11 Reconnect the four liquid lines to the new suppressor Plug in the suppressor cable Close the DC door Turn on the DC power and restart the pump flow 9 27 3 Replacing a CD l 2 ENI 4 IC di Stop 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 tubing from the CD CELL IN and CELL OUT ports see Figure 9 52 Disconnect tubing Release Lever Figure 9 52 Disconnecting the CD Liquid Lines Capillary CD shown For an analytical CD remove the suppressor from the detector For instructions see Section 9 27 2 Press the release lever located below the detector see Figure 9 52 The detector pops out slightly from the DC compartment Grasp the top of the detector and pull outward to remove the detector from the compartment Do not pull from the CELL IN and CELL OUT fittings Note the electrical plug on the back of the detector and the receptacle on the inside of the DC Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure Reconnect the cell inlet and outlet lines Doc 065446 01 11 12 389 Dionex ICS 5000 Operator s Manual 9 Reinstall the suppressor see Section 9 27 2 10 Turn on the DC power and restart the pump
263. hen the temperature of the DC lower compartment is higher than the maximum allowed This error may occur if the Dionex ICS 5000 IC system is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot See 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 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 065446 01 11 12 265 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
264. hip 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 Consumables documentation For complete information about Dionex columns suppressors eluent generator cartridges etc refer to the appropriate Doc 065446 01 11 12 13 Dionex ICS 5000 Operator s Manual product manual These manuals are provided on the Thermo Scientific Reference Library DVD 1 3 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 5000 system Introduction a i includes a brief description ofthe 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 p y Description 3 components and important operating features includes an introduction to Chromeleon
265. hoot 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 program does not include a command that ends data acquisition To troubleshoot The AcqOn command must be paired with an AcqOff command Enter the Acqoff command at the appropriate point in the instrument method or program AII samples scheduled for run on timebases x need to specify the same value for property nominal Temperature or A All samples scheduled for run on timebases x need to specify the same value for property TempCtrl or Doc 065446 01 11 12 279 Dionex ICS 5000 Operator s Manual All samples scheduled for run on timebases x need to specify the same value for property y When a TC is shared by two instruments in Chromeleon 7 or timebases in Chromeleon 6 8 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 dur
266. ine Maintenance 201 7 6 EG Daily Maintenance 201 7 7 EG Weekly Maintenance 0 cece cece ees 201 7 8 EG Annual Maintenance 00 eee ee eee 202 DC Routine Maintenance 004 203 7 9 DC Daily Maintenance 203 Doc 065446 01 11 12 vii Dionex ICS 5000 Operator s Manual 7 10 DC Weekly Maintenance LL 203 7 11 DC Periodic Maintenance eee eee eee 203 7 12 DC Annual Maintenance 0 0 0 2 eee eee 204 TC Routine Maintenance 205 7 13 TC Daily Maintenance 205 7 14 TC Weekly Maintenance 0 205 7 15 TC Periodic Maintenance 205 7 16 TC Annual Maintenance 0 0 cee eee ee eee 206 8 Troubleshooting 8 1 Audit Trail Error Messages 207 8 1 1 DP SP Error Messages cece eee eens 208 8 1 2 EG Error Messages 0 cece eee eens 209 8 1 3 DC Error Messages 211 8 1 4 TC Error Messages 0 c cece eee ees 213 8 2 Noisy Baseline acct lia Used aid ab eS av da Salar RA dane 218 8 3 Poor Retention Time Reproducibility 222 8 4 Peak Retention Times Are Too Early 000000000 ee 224 8 5 Peak Retention Times Are Too Late 0 00000 eee ee 224 8 60 INO Peaks silla ice ale iena 225 87 Tallin Peaks ol ae e 226 8 8 Low System Backpressure c eee eee eens 227 8 9 High System Backpressure
267. ines to be submerged in waste liquid 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 vide hors ligne d luants Le r servoir n a pas t congu cette fin MISE EN GARDE Verwenden Sie keine Plastikbehalter zum Offline Vakkum Entgasen von Eluenten Die Behalter sind daf r nicht ausgelegt VORSICHT 2 5 1 EO Optional The 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 Doc 065446 01 11 12 35 Dionex ICS 5000 Operator s Manual CAUTION MISE EN GARDE VORSICHT Scientific recommends pressurizing reservoirs with helium or nitrogen under the following circumstances When using eluents that ar
268. information in the section applies to capillary IC systems only Sections preceded with the Analytical IC flag indicate that the information in ie 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 MI D Primary protective conductor terminal Secondary protective conductor terminal Power supply is on O Power supply is off Doc 065446 01 11 12 17 Dionex ICS 5000 Operator s Manual AN Indicates a potential hazard Refer to this operator s manual for an explanation of the hazard and how to proceed 18 Doc 065446 01 11 12 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 Product 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 conformit
269. ing 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 find 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 1 Run the Chromeleon IQ to diagnose the problem Select Tools gt Instrument Qualification in Chromeleon 7 or Qualification gt Chromeleon 6 8 IQ in Chromeleon 6 8 2 When you eliminate the source of the error rerun the Setup program 280 Doc 065446 01 11 12 8 TC Troubleshooting 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 as well as a Timebase Class 1 license This error occurs if you attempt to start data acquisition when these requirements are not met To troubleshoot Contact Thermo Fisher Scientific to obtain the appropriate software
270. ing electrode fouled l 2 If a disposable working electrode is being used replace the electrode 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 278 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 AgCI reference electrode see Section 9 28 5 Analog Output Option Analog output range set too high Select a more sensitive analog output range 8 11 High Background Dionex CR TC is contaminated Clean the trap column as instructed in the Dionex CR TC manual The manual is provided 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 detecto
271. ing new seals Section 9 7 5 e 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 in Figure 9 6 and Figure 9 7 Before beginning locate the following items in your pump ship kit e 3 0 mm hex key P N 062338 e 10 32 fitting plugs P N 042772 e 10 cc syringe P N 079803 e 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 Doc 065446 01 11 12 319 Dionex ICS 5000 Operator s Manual 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 l 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 Whe
272. ing the high pressure valve pod is an alternative to rebuilding the valve Replacing the pod is easier and faster than rebuilding the valve For instructions see Section 9 23 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 372 Doc 065446 01 11 12 9 DC Service Open the DC door 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 Reconnect all liquid lines to the injection valve Turn on the power to the DC Turn on the pump flow Check for leaks from the valve Tighten fittings as required For tightening requirements for the 10 32 fitting bolt P N 074449 and 10 32 double cone ferrule P N 074373 see Section 9 2 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 4 port P N 074699 6 port P
273. intenance annual DC 204 DP 200 O EG 202 mie Offset percentage analog out 89 SP 200 ee TC 206 Offsetting background conductivity 171 SA i Open circuit 271 Maintenance daily DC 203 205 oe or DP SP 199 ais EG 201 Operation 176 TC 205 Analyzing samples 176 Mai i mer Creating a sequence Chromeleon 6 8 aintenance periodic 178 DP SP 2 mee DO Creating a sequence Chromeleon 7 177 oie Direct control of modules 175 Maintenance weekly m DC 203 Filling vials 152 154 Filling well plates 152 DP SP 199 EG 201 Instrument method example 184 Loading samples 182 Index 12 Doc 065446 01 11 12 Index Program example 184 Sample preparation 152 Starting a sequence 180 181 Organic solvent 80 Oven TC 120 See also Temperature control TC Oven LED DC LED is flashing 55 LED is lighted 55 Oven LED TC LED is flashing 120 304 LED is lighted 120 P PAD See Pulsed amperometry Palladium hydrogen PdH reference electrode 82 Replacement procedure 407 Panel tabset 11 Displaying 175 Home panel 11 155 157 How to display 163 169 173 259 260 Peak height Reproducibility 72 Peaks Fronting 122 Reversed 89 Tailing 122 226 Periodic maintenance DC 203 DP SP 200 TC 205 pH gradient 80 pH half cell 80 pH limits 151 pH modifier 46 pH reading Adjusting potentials for 81 Always 7 0 275 Cannot be set to 7 0 276 Effect on potentials 80 Mo
274. 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 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 1 SR2 or later or Chromeleon 6 8 Chromatography Data System release 6 8 SR12 or later Chromeleon 7 and Chromeleon 6 8 provide complete instrument control data acquisition and data management NOTE All references in Chromeleon to Dionex ICS 5000 systems apply equally to Dionex ICS 5000 systems Optionally the Dionex ICS 5000 system can be controlled by a PC configured with Thermo Scientific Dionex 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 10 Doc 065446 01 11 12 1 Introduction 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 ac
275. ions in Section 8 28 6 Regenerate the electrode by soaking in a solution containing 1 M KC1 and 1 M HCI for 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 AgcCI reference electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 278 276 Doc 065446 01 11 12 8 DC Troubleshooting 3 Ifsoaking 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 e PdH reference electrode selected Select the AgCl reference electrode mode on the Chromeleon 7 ED ePanel or in the instrument method or the Chromeleon 6 8 EC Detector Control panel or in the program e Disconnected reference electrode Verify that the reference electrode cable is securely connected see Figure 8 8 e Uncalibrated pH Ag AgCl reference electrode Calibrate the pH Ag AgCl reference electrode see Section 9 28 6 Dry pH Ag AgCl reference electrode 1 Soak the pH Ag AgCl reference electrode in a solution containing 1 M KCl and 1 M HCI for 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 R
276. iquid Doc 065446 01 11 12 85 Dionex ICS 5000 Operator s Manual 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 34 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 output 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
277. is detected 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 o Abort A message is displayed in the audit trail and the running batch is aborted Doc 065446 01 11 12 207 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 see the page indicated in the table DP SP Related Audit Trail Error Message Default Severity Level exceeded the safety limit A program with this name already exists Abort page 231 Abnormal drive current for x x seconds Warning page 231 Camshaft index too early Abort page 232 Camshaft index too late Abort page 23
278. isition 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 to the power supply 3 Ifyou cannot identify the cause of the error contact Technical Support for Dionex products for assistance 296 Doc 065446 01 11 12 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
279. it reaches the stop 4 Pull the Dionex CR TC off the ball studs on the component mounting panel 5 Disconnect the liquid lines from the four ports on the Dionex CR TC 6 Twist the ring on the Dionex 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 7 Remove the Dionex CR TC from the EG 354 Doc 065446 01 11 12 9 EG Service 9 15 2 Installing and Flushing the New CR TC 1 Remove the plugs from the ports on the new Dionex CR TC Bey 2 Ifyouare installing a Dionex 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 Dionex CR TC see Figure 9 27 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 IC Cube Ship Kit P N 072003 c Connect one end of this line to the Dionex EGC INLET port 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 Doc 065446 01 11 12 355 Dionex ICS 5000 Operator s Manual d Connect the EGC OUT line to the Dionex CR TC ELUENT IN port and connect the waste line to the Dionex CR TC REGEN OUT port EGC Capillary CR TC Flushing Capillary Pump at 0 02 mL min for 15 min EGC LA 0 062 mm
280. itors the date on which service was last performed and displays an appropriate message shown above at the following times when the due date for the next service is approaching and when the due date is overdue The Service WarningPeriod property determines the number of days before the due date that the warning is first displayed Doc 065446 01 11 12 291 Dionex ICS 5000 Operator s Manual To troubleshoot Contact Technical Support for Dionex products for information about performing annual preventive maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The DC TC preventive maintenance procedure consists of rebuilding each high pressure valve installed in the module The following kits are available e 0 4 uL Internal Loop High Pressure Valve Maintenance Kit P N 075040 e 6 Port High Pressure Valve Maintenance Kit P N 075974 e 10 Port High Pressure Valve Maintenance Kit P N 079053 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 con
281. l A beep sounds What to do when an alarm occurs Find and eliminate the leak If you are using Chromeleon 7 Open the Command window press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button Ventilate the interior of the TC thoroughly before closing the door and resuming operation Adjusting the Sensor Sensitivity Follow the steps below to change the sensitivity setting of the gas or humidity sensor or to turn off a sensor l 2 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset Press the F8 key to open the Command window Chromeleon 7 or the Commands dialog box Chromeleon 6 8 Select the TC If you are using Chromeleon 7 Click the Parameters tab page for the TC and click the GasLeakSensor or HumidityLeakSensor parameter Select the new sensitivity setting or select Off to disable the sensor If you are using Chromeleon 6 8 Click the plus sign beside TC to display 130 Doc 065446 01 11 12 2 TC Description 2 26 the items underneath Under TC_Temp select the GasLeakSensor or HumidityLeakSensor parameter Select the new sensitivity setting or select Off to disable the sensor and click Execute TC Theory of Operation The fundamental requirement for a thermal compartment intended for chromatography applications is the ability to maintain the pre
282. l Set Home Panel Shown Doc 065446 01 11 12 11 Dionex ICS 5000 Operator s Manual Figure 1 3 Chromeleon 6 8 Panel Tabset Dionex ICS 5000 Home Panel Shown 12 Doc 065446 01 11 12 1 Introduction 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 Dionex ICS 5000 lon Chromatography 065446 Yes No System Operator s Manual Installing the Dionex ICS 5000 Ion 065447 Yes Yes Chromatography System Dionex AS AP Autosampler Operator s 065361 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 071679 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 s
283. le System 1 Deionized Deionized Water Water D Oc UE To waste From suppressor 1 Regen Out via the DC rear chase q S gt DC front view EG left side view System 1 RFIC Eluent Degasser Cell In Cell Out Cell In Cell Out Regen Out Eluent Out Regen Out Eluent Out q o e oso Eluent Eluent Out Y Y A In To Waste Out afl A To the CR TC 1 Regen In via the EG rear chase From AS AP CI To AS AP Waste a j 4 To waste T System 1 System 2 From suppressor 2 Regen Out via the DC rear chase EG System 2 right side view y EGC RFIC high pressure Eluent Degasser Eluent Eluent Out v Vio A In aseyo DI au eN uj UaBey Z L HO UL OL Waste Regen To inject valve ut Eluent ZERO In Out CR TC To waste ili ess Figure 3 6 Analytical IC Dual RFIC EG System CD CD Doc 065446 01 11 12 141 Dionex ICS 5000 Operator s Manual Pump front view To pump 2 inlet via the pump rear chase To pump 1 inlet via the pump rear chase System 2 10 8 __ fay See g y To waste pump not to scale i Piston o A a HI E jc 3 System 1 tes ol og Deionized huen Water A _ 8 i D Foro To waste gt From suppressor 1 Regen Out via the DC rear chase cli From the ED cell out via the DC rear chas From pump 2 DC
284. le 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 a timebase Chromeleon 6 8 Doc 065446 01 11 12 261 Dionex ICS 5000 Operator s Manual 262 Doc 065446 01 11 12 a DC 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 Check the detector connection An electronics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the upper part of the detector see Figure 8 3 to make sure 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 Dionex ICS 5000 IC system electronics compo nents cannot be serviced by the user Push here to ensure the ____ detector s electrical connection is secure Thermo CSAS 3OO Hren w Figure 8 3 Conductivity Detector Connection Doc 065446 01 11 12 263 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 Dionex ICS 5000 IC system is operating in an
285. lectrode O Ring 5 Slide the new O ring P N 014067 onto the electrode 406 Doc 065446 01 11 12 9 DC Service 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 53 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 you observe 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 Tweezers 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 Doc 065446 01 11 12 407 Dionex ICS 5000 Operator s Manual
286. led in the upper compartment of the DC see Figure 2 23 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 including pulsed amperometric detection PAD and integrated pulsed amperometric detection IPAD see Section 2 19 2 e Cyclic voltammetry see Section 2 19 3 NOTE Cyclic voltammetry is supported in Chromeleon 6 8 but not Chromeleon 7 Electrochemical Detector Cell The ED cell is a miniature flow through amperometric detection cell that includes three different electrodes a titanium cell body the counter electrode a working electrode and either a combination pH Ag AgCl reference electrode see Figure 2 32 or a PdH reference electrode 78 Doc 065446 01 11 12 2 DC Description 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 polytetrafluoroethylene silver platinum and carbon The ED cell can be used in both capillary IC and 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 tit
287. leon 6 8 panel tabset While being primed pump starts briefly and an alarm sounds If the high pressure limit was tripped 1 Check that the priming valve on the secondary pump head is opened see Figure 2 3 To open the valve turn the knob one half turn counterclockwise 2 Check fittings for overtightening Check tubing for crimping and replace it as needed see Section 9 3 Be careful not to overtighten fittings Doc 065446 01 11 12 239 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 see the troubleshooting steps listed for the particular message 8 14 DP SP Stops Unexpectedly 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 See the troubleshooting steps on page 235 for this audit trail message Pressure fallen below lower li
288. 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 065446 01 11 12 205 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 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 defecti
289. ll Disposable Working Electrode Gasket 393 9 28 3 Replacing an ED Cell Conventional Working Electrode Gasket 393 9 28 4 Polishing an ED Cell Conventional Working Electrode 396 9 28 5 Replacing a pH Ag AgCl Reference Electrode 399 9 28 6 Calibrating a pH Ag AgCl Reference Electrode 401 9 28 7 Replacing a pH Ag AgCl Reference Electrode O Ring 406 9 28 8 Replacing a PdH Reference Electrode 407 9 28 9 Replacing an ED Detector 411 TG Servi oel an ii Riga gi 413 9 29 Replacing Tubing and Fittings LL 413 9 30 Setting Up the Column ID System 414 9 31 Rebuilding an Injection Valve 416 9 32 Replacing an Injection Valve Pod 417 9 33 Changing the Main Power Fuses 0000 c eee eee ees 419 A Specifications DP SP Specifications a 421 EG Specelfications i illuela lea uri 425 DC Specifications 429 Doc 065446 01 11 12 xiii Dionex ICS 5000 Operator s Manual TC Specifications pelata pieni sila 439 B Reordering Information DP SP Reordering Information 441 EG Reordering Information 445 DC Reordering Information 447 TC Reordering Information 451 xiv Doc 065446 01 11 12 1 Introduction 1 1 Dionex ICS 5000 System Overview Dionex ICS 5000 Dual Pump O pp Dionex I
290. lled 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 10 Reinstall the working electrode block and the yoke knob and block Fingertighten the yoke knob by turning it a full 360 degrees Doc 065446 01 11 12 395 Dionex ICS 5000 Operator s Manual 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 period 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
291. ltage 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 Dionex EGC power and the cell voltage 9 28 9 Replacing an ED Detector CAUTION l 2 Turn off the pump flow 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 Doc 065446 01 11 12 411 Dionex ICS 5000 Operator s Manual 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 and disconnect the cell inlet and outlet lines 4 Disconnect the reference electrode cable and the cell cable 5 Grasp the cell body and pull straight out to remove the cell from the detector 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 P
292. ly 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 November 2012 initial release of instrument Software version Chromeleon 7 1 SR2 or later or Chromeleon 6 8 SR12 or later For Research Use Only Not for use in diagnostic procedures Contents 1 Introduction 1 1 Dionex ICS 5000 System Overview 0 00 1 1 1 1 Dionex ICS 5000 System Components 3 1 1 2 Dionex ICS 5000 System Control 10 1 2 Dionex ICS 5000 System Documentation 13 1 3 Dionex ICS 5000 System Operator s Manual 14 14 Safety and Regulatory Information 15 1 4 1 Safety Messages and Notes 00 02 e eee eee 15 1 4 2 Safety Symbols LL 17 1 4 3 Declaration of Conformity 0 0 00 eee ee eee 19 1 5 Deionized Water Requirements for IC 20 2 Description DP SP Description cece eee 21 2 1 DP SPFrontFeatures dotiert ni EEEren Nis 21 2 2 DP SP Interior Components LL 23 22 1 Pump Heads
293. m 176 Creating an instrument method 176 Inject sample 184 Load sample 184 Compartment open circuit 265 Compartment over safe temperature 265 Concentrator column 71 127 Condensation 203 Conductivity Detector CD 3 Air bubble removal 390 Analytical IC system version 72 Capillary IC system version 72 Cell calibration 386 Cell description 72 Cell temperature control 72 Description 7 72 Effect of temperature on conductivity 72 Leaking 274 Replacement procedure 389 Specifications 434 Temperature compensation 73 Configuration drawings 135 146 Connected LED DC LED is lighted 55 Connected LED DP SP LED is lighted 22 Connected LED EG LED is lighted 39 119 Connected LED TC LED is lighted 119 Counter electrode 78 79 Index 4 Doc 065446 01 11 12 Index CRD bypass cartridge for IC Cube 60 CRD cartridge for IC Cube 60 CR TC trap column 5 45 Contamination 229 Hydration procedure 357 Replacement procedure 354 360 CSRS 300 74 Cyclic voltammetry 109 110 Data collection rate 109 Sweep rate 110 Triangular waveform example 110 Waveforms 109 111 D Daily maintenance DC 203 DP SP 199 EG 201 TC 205 Data Displaying 3D amperometry data 114 Reprocessing amperometry data 113 Data collection rate Cyclic voltammetry 109 Electrochemical detector 114 Integrated amperometry 111 Data compression Cyclic voltammetry 109 DC amperometry 106 Entering th
294. mbination of these The SP contains one of the following pump types 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 isocratic analytical IC pumps or one isocratic capillary IC pump and one gradient analytical IC pump 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 Analytical IC pumps operate at flow rates ranging from 0 00 to 10 0 mL min and operating pressures up to 41 MPa 6000 psi 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 lt A high precision programmable current source power supply Doc 065446 01 11 12 1 Introduction For each channel the following options must be ordered separately for installation inside the EG A disposable eluent generator cartridge Thermo Scientific Dionex EGC Each cartridge contains the electrolyte concentrate solution appropriate for the eluent being generated
295. mersed in liquid e For 10 mL vials only If necessary raise the needle height inside the vial to position the vent above the liquid Set the needle height in a Chromeleon 7 instrument method or a Chromeleon 6 8 program e Install a cap on each vial Make sure the septum is pushed fully into the cap and the cap is securely tightened Tips for Filling and Loading Dionex AS AP Well Plates e Put on powder free latex gloves before handling well plates and covers to minimize sample contamination e Rinse well plates and covers thoroughly with deionized water before use to remove any contaminants e Air dry well plates completely to prevent any changes in sample concentration If necessary use 690 kPa 100 psi nitrogen gas to assist in drying 154 Doc 065446 01 11 12 4 Startup 4 4 4 4 1 4 4 2 e In general pipet the amount of sample to be drawn plus 70 uL Refer to the autosampler manual for details about the sample volumes drawn for each type of injection Tips for Filling and Loading Dionex AS DV Vials e Fill the vials until the level in the vial reaches the top of the vial tray e Install a cap on each vial Use the cap insertion tool P N 037987 to prevent contamination and ensure the cap is inserted to the proper depth Starting Chromeleon 7 NOTE All references in Chromeleon to Dionex ICS 5000 systems apply equally to Dionex ICS 5000 systems Starting the Chromeleon 7 Instrument Controller Service To start t
296. mine why liquid flow stopped 3 Ifthe error message appears again contact Technical Support for Dionex products for assistance The Dionex CR TC control electronics may have malfunctioned NOTE The Dionex ICS 5000 IC system electronics compo nents 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 Dionex CR TC when the Dionex EGC is turned off The Dionex CR TC current is automatically turned off to prevent damage to the Dionex CR TC To troubleshoot Verify that the pump flow and the Dionex EGC are on before turning on the Dionex CR TC 246 Doc 065446 01 11 12 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 Dionex EGC current and Dionex CR TC are on The Dionex CR TC current is automatically turned off to prevent damage to the Dionex 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 if you try to turn on the Dionex CR TC when a live EG is linked to a virtual pump 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
297. mit High pressure limit was tripped See the troubleshooting steps on page 237 for this audit trail message The system pressure exceeded the safety limit Electrical connections incorrectly installed The electrical cables may not be properly installed For assistance contact Technical Support for Dionex products NOTE The Dionex ICS 5000 IC system electronics compo nents cannot be serviced by the user 240 Doc 065446 01 11 12 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 Chromeleon audit trail e Defective piston seal Check the pump heads for leaks If there is any leakage tighten the fitting connections just enough to stop the leak Dry the components If the pump head continues to leak replace the piston seal see Section 9 7 e Leaking check valve If the leaking check valve is securely tightened but allows leaks despite this the valve is defective Replace both check valve cartridges see Section 9 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
298. mits defined for the Warning page 285 column Current temperature is out of limits defined for Warning page 285 the column Data buffer overrun Abort page 285 Device control feature is not available Please Abort page 286 check key code and CM Features see About Chromeleon in the client s Help menu Device is not remote Abort page 286 Device not found on the USB Abort page 287 Either the current date is later than the Warning page 287 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 287 Error during storing of the card data to the chip Error page 288 card Table 8 4 TC Error Messages Continued 214 Doc 065446 01 11 12 8 Troubleshooting TC Related Audit Trail Error Message Default Severity Level Error finishing download Abort page 281 Error programming flash memory Abort page 288 Executing this command will reset associated Warning page 288 counter values stored in the module Firmware download failed Abort page 289 Firmware download in progress Please wait Error page 289 Gas leak detected Error page 289 Humidity leak detected Error page 289 Illegal parameter Abort page 290 Invalid date time format Either use DD MMM Error page 290 YYYY or current Nyear s Nmonth s
299. mn can be installed after the secondary pump head in place of the static mixer see Section 2 2 6 Several Thermo Scientific high pressure trap columns are available for use with the Dionex ICS 5000 system see Table 2 1 Doc 065446 01 11 12 27 Dionex ICS 5000 Operator s Manual For details about a column refer to the column manual Column manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 High Pressure Trap Column Part Number Dionex MFC 500 079017 Dionex ATC 500 2 mm 079018 Dionex CTC 500 2 mm 079019 Dionex ATC 500 4 mm 075976 Dionex CTC 500 4 mm 075977 Dionex ATC HC 500 075978 Dionex ATC HC 500 Borate 075979 Table 2 1 Thermo Scientific Dionex High Pressure Trap Eg 2 2 8 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 28 Doc 065446 01 11 12 2 Description 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 R 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 o
300. module et facilement accessible MISE EN GARDE Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher da sich die Steckdose nahe am Ger t befindet und leicht zuganglich ist VORSICHT Digital I O Connectors The two 6 pin mini DIN connectors can be used to exchange digital signals with any external device capable of being controlled through a relay or TTL input The two connectors are identical in function Relay_Com Relay_N O Digital Input Digital_GND Not Used Not Used N O Normally open contact Figure 2 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 124 Doc 065446 01 11 12 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 see Table 2 8 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 10
301. move any precipitate with water and a lint free tissue and then install a new gasket see Section 9 28 3 Turn the yoke knob see Figure 9 54 a full 360 degrees to completely engage the knob 230 Doc 065446 01 11 12 ICS 5000 Je DP SP Troubleshooting 8 12 Troubleshooting DP SP Error Messages If any of the following alarm conditions occurs a message is displayed in the Chromeleon 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 it as needed see Section 9 3 Be careful not to overtighten fittings If the message appears again contact Technical Support for Dionex products for assistance Doc 065446 01 11 12 231 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 se
302. mp 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 Doc 065446 01 11 12 333 Dionex ICS 5000 Operator s Manual DANGER DANGER ACHTUNG 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 main power cord from both its source and from the rear panel of the pump HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the pump HAUTE TENSION D branchez le cordon d alimentation principal de sa source et du panneau arri re du pump HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der R ckseite der Pumpe 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 fro
303. n 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 detector of each type For details about the CD see Section 2 14 For details about the ED see Section 2 15 64 Doc 065446 01 11 12 2 DC Description Suppressors for conductivity detection are also installed in the upper compartment The following types of Thermo Scientific suppressors can be used e Dionex SRS 300 Self Regenerating Suppressor 2 and 4 mm e Dionex AES Atlas Electrolytic Suppressor e Dionex 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 24 Handle for pulling tray forward Figure 2 24 DC Lower Compartment Tray Handle Doc 065446 01 11 12 65 Dio
304. n 4 9 for a list of valid concentration ranges for the cartridges and then edit the Chromeleon 7 instrument method or Chromeleon 6 8 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 Peak Retention Times Are Too Late Eluent concentration setting is too low The correct eluent concentration setting depends on several factors the flow rate Dionex EGC type etc See Section 4 9 for a list of valid concentration ranges for the cartridges and then edit the Chromeleon 7 instrument method or Chromeleon 6 8 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 224 Doc 065446 01 11 12 8 Troubleshooting 8 6 No Peaks EG power is not turned on 1 Check that the POWER button on the front of the EG is turned on 2 Check that the EG main power switch on the rear panel is turned on 3 Check that the main power cord is plugged into both the EG rear panel connector and the power source Check that the wall outlet has power Injection valve is not actuating or the sample loop is plugged 1 Test the valve by manually swi
305. n 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 three columns with an inner diameter of 1 to 9 mm and a maximum length of 30 cm 11 8 in Columns are attached to the brackets with special column clips P N 064786 set of six clips Doc 065446 01 11 12 121 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
306. n Valve Figure 2 20 IC Cube Features fe Dionex CRD Cartridge or CRD Bypass Cartridge The Dionex CRD 200 Capillary cartridge P N 072054 contains a Dionex CRD 200 Carbonate Removal Device Capillary The Dionex CRD 200 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 Dionex CRD 200 Capillary is optimized for operation at the flow rate range typically used with capillary columns The Dionex 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 60 Doc 065446 01 11 12 2 DC Description Installation of a Dionex CRD 200 Capillary is optional However if one is not used a Dionex CRD bypass cartridge P N 072056 must be installed The bypass cartridge contains the plumbing connections necessary for eluent and waste flow through the system as Suppressor Cartridge or Suppressor Bypass Cartridge Capillary suppressor cartridges are available in two versions Thermo Scientific Dionex ACES 300 Anion Capillary Electrolytic Suppressor cartridge P N 072052 and Thermo Scientific Dionex 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 su
307. n 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 AgCI reference electrode typically lasts from 3 months to 1 year depending on use NOTE Toregenerate a pH Ag AgCl reference electrode soak it in a solution of 1 M KCl and 1 M HCl Items Needed e pH Ag AgCI 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 Doc 065446 01 11 12 399 Dionex ICS 5000 Operator s Manual 2 Unscrew the pH Ag AgCl reference electrode and remove it from the cell body see Figure 9 57 Unscrew the pH Ag AgCl reference electrode Figure 9 57 Removing the pH Ag AgCI Reference Electrode Cell Configured for Analytical IC Shown 3 Unscrew the storage cap from the new pH Ag AgcCI reference electrode see Figure 9 58 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 damaging the electrode See Section 6 4 for storage instructions Save the storage cap Figure 9 58 pH Ag AgCI Reference Electrode in Storage Cap 4 To remove any precipitated salt rinse
308. n ranges 165 167 Eluent generator cartridges 5 Fuse cartridge 49 Fuses 49 Gas vent line 49 Leak sensor 47 256 Liquid flow path 50 53 Liquid leaks 257 259 Main power switch 49 Maintenance 201 Operating precautions 147 Power LED does not light 258 Pump pressure limits 260 Rear panel description 48 49 Selecting the eluent concentration 165 Shutdown procedures 189 Spare parts 445 Specifications 425 Status bar buttons and LEDs 39 System configuration 135 USB connections 48 Waste lines 49 50 See also Error messages EG Eluent generator cartridges 5 43 Backpressure requirement 46 147 148 259 260 Conditioning procedure 190 Index 6 Doc 065446 01 11 12 Index Electrical connections 47 Frit outlet 228 338 Leaks 228 257 259 Replacement procedure 338 354 Selecting the eluent concentration 165 Start up procedures 190 Storage long term 190 Storage short term 189 Eluent Organizer EO 3 6 35 Eluent proportioning valves 25 Eluent reservoirs See Reservoirs eluent Eluent filtering 37 Eluents Aqueous 200 Degassing 25 Filtering 159 Flushing lines after eluent change 222 Monitoring pH 80 Outgassing 390 End line filter See Filter end line EO Regulator Kit 36 ePanel Set 10 155 Displaying 175 Home panel 11 EPM 300 Electrolytic pH Modifier 43 44 46 47 361 Function 44 46 Troubleshooting 257 Equilibration system 170 174
309. n 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 to pull the panel forward until it reaches the stop 320 Doc 065446 01 11 12 9 DP SP Service 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 see 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 075767 Analytical Piston O Ring Primary Pump Head P N 068646 Capillary P N 040695 P N 074447 Capillary P N 079857 Analytical Capillary and Analy
310. nce Motor position error The motor is overloaded This error occurs if the pump motor is overloaded To troubleshoot 1 Oneor 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 see page 238 for additional troubleshooting steps 234 Doc 065446 01 11 12 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 l 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 as instructed in Section 4 6 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 Mak
311. nd 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 aay 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 Type I 18 megohm cm filtered and deionized water 6 Dry the reservoir with clean particulate free air 9 5 Priming the DP SP Prime the pump if the eluent has been changed the eluent line is new empty or the eluent line contains air This section describes two different priming procedures 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 079803 can be used with either priming procedure Thermo Fisher Scientific recommends using a syringe only if eluent lines are 100 empty or if the pump is dry Doc 065446 01 11 12 311 Dionex ICS 5000 Operator s Manual 9 5 1 Priming with the PUMP PRIME Button 1 On the
312. nd 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 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 2 Press the POWER button on the front of the DC to turn off the DC CAUTION MISE EN GARDE 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 370 Doc 065446 01 11 12 9 DC Service 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 VORSICHT 3 Open the DC lower door 4 Loosen the screw on the front of the leak sensor P N 062437 see Figure 9 34 Note The screw remains attached to the sensor eak Sensor i Loosen this screw Figure 9 34 Leak Sensor 5 Start pulling the leak sensor out er of the component panel i Gad continue pulling until both the ry sensor and the att
313. necting tubing to a port make sure the 10 32 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 Figure 9 1 shows the correct and incorrect placement of the ferrule and fitting bolt on the tubing Correct Incorrect 2 mm Figure 9 1 Correct and Incorrect Ferrule and Fitting Bolt Placement for Tubing Connections High Pressure Fitting and Ferrule Shown Doc 065446 01 11 12 307 Dionex ICS 5000 Operator s Manual 9 2 Follow the steps below to install tube fittings l 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 Insert the tubing into the port until it stops While maintaining pressure on the tubing to keep it in place in the port tighten the fitting bolt fingertight Follow the instructions in Section 9 2 to tighten the fitting Tightening Guidelines for High Pressure Fittings Follow these guidelines when tightening a high pressure 10 32 fitting bolt P N 074449 and high pressure 10 32 double cone ferrule P N 074373 1 Use your fingers to tighten the fitting bolt as tight as you can Then use a wrench to tighten the fitting an additional three quarter turn 270 degrees If leaks occur replace the fitting bolt ferrule and tubing 308
314. nex CR TC e Dionex RFIC Eluent Degasser to injection valve e Dionex RFIC Eluent Degasser to eluent reservoir 1 58 mm 0 062 in ID Colorless 047203 Dionex EGC gas vent line polyurethane tubing and Dionex RFIC Eluent Degasser vent line 10 mm 0 39 in ID Colorless 055075 Drip tray drain hose polyethylene tubing 1 8 in fitting bolt Tan 052267 Suppressor REGEN OUT port 1 8 in ferrule Yellow 048949 and eluent reservoirs Table 9 4 Tubing and Fittings for an Analytical IC EG Channel NEMI Notes for analytical IC channels IC e For tightening requirements for the 10 32 fitting bolt P N 074449 and 10 32 double cone 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 that 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 for details Doc 065446 01 11 12 337 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
315. nex 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 current applied to the Dionex EGC exceeds the maximum current allowed The Dionex 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 Dionex EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 See Section 8 23 to determine why there is no flow 3 Ifthe error message appears again contact Technical Support for Dionex products for assistance The cartridge control electronics may have malfunctioned NOTE The Dionex ICS 5000 IC system electronics components cannot be serviced by the user Doc 065446 01 11 12 251 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 Dionex EGC can support To troubleshoot Replace the Dionex EGC see Section 9 14 EG1 over voltage Or EG2 over voltage This error occurs when the current applied to the Dionex EGC exceeds the maximum current allowed The
316. nex ICS 5000 Ion Chromatography System Installation Instructions Document No 065447 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 065446 01 11 12 305 Dionex ICS 5000 Operator s Manual 306 Doc 065446 01 11 12 9 e Service This chapter describes Dionex ICS 5000 IC 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 Scientific office Before replacing any part see the troubleshooting information in Chapter 8 to correctly identify the cause of the problem Substituting non Dionex Thermo Scientific parts may impair a module s IMPORTANTI performance thereby voiding the product warranty Refer to the 9 1 warranty statement in the Dionex Terms and Conditions for more information Connecting Tubing High pressure 10 32 fitting bolts P N 074449 and high pressure 10 32 double cone ferrules P N 074373 are used for most ICS 5000 tubing connections even in low pressure systems When con
317. nex ICS 5000 Operator s Manual 2 12 DC Temperature Control Zones The following temperature control zones are possible with the DC depending on the options installed e DC upper compartment e DC lower compartment e Heated conductivity cell e IC Cube capillary column heater e 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 4 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 67 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 4 Achieved Temperatur
318. nitoring 81 Nonexistent 277 pH Ag AgCl reference electrode 78 80 Long term storage 191 O ring replacement procedure 406 Replacement procedure 399 See also Reference electrode Photodiode Array Detector 3 9 Regulator Bracket Kit 36 Piston seal wash solution 26 187 Piston seal wash system 26 160 Activating 162 Dual pump seal wash option 27 160 442 Replumbing the DP connections 160 Setup 162 Piston seals Replacement procedure 319 Pistons Replacement procedure 326 Platinum working electrodes 79 Plot I t 115 Plumbing Replacing DC tubing and fittings 365 Replacing DP SP tubing and fittings 309 Replacing EG tubing and fittings 335 Replacing TC tubing and fittings 413 Plumbing configuration drawings 135 146 Polarity Analog output 89 Polishing kit ED 396 Polishing procedure 396 Reordering 449 Post column reagent addition 64 97 145 Potassium carbonate eluent 44 46 Potassium hydroxide eluent 44 Potential shifting 80 278 Power cord 363 376 377 419 Power LED DC 56 Power LED DP SP 22 Power LED EG 40 Power LED TC 120 Power output DC Doc 065446 01 11 12 Index 13 Dionex ICS 5000 Operator s Manual T O option 85 86 90 Power receptacle DC 84 DP SP 31 EG 49 TC 123 Power switch rear panel DC 84 DP SP 31 EG 49 TC 123 Pre concentration 64 97 Predictive Performance 133 Pressure limit settings 164 Pressure limits tripped 228 Pressure tran
319. nly 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 then to the remainder of the chromatography system Doc 065446 01 11 12 29 Dionex ICS 5000 Operator s Manual 2 3 2 Gradient Pump Flow Schematic Figure 2 6 illustrates the liquid flow path through a gradient pump OUTLET CHECK VALVE ELUENT ELUENT ELUENT ELUENT A B C 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 Eluent 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 pu
320. 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 304 Doc 065446 01 11 12 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 ventilation slots are not obstructed in any way Allow at least 6 cm 2 4 in behind the TC for ventilation Ambient temperature is too high Reduce the ambient temperature for example ventilate the lab in which the TC is installed 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 Dio
321. nt Organizer Detector Chromatography Compartment Dionex ICS 5000 Detector Chromatography Module IC Cube inside DC Dionex ICS 5000 IC Cube Detector inside DC Dionex ICS 5000 Conductivity Detector Dionex ICS 5000 Electrochemical Detector Accessory inside DC Dionex ICS 5000 Automation Manager Detector outside DC Thermo Scientific Dionex ICS Series Photodiode Array Detector D Thermo Scientific Dionex ICS Series Variable Wavelength Detector D Thermal Compartment Dionex ICS 5000 Thermal Compartment D Autosampler Thermo Scientific Dionex ICS Series AS AP Autosampler Thermo Scientific Dionex AS DV Autosampler D Mass Spectrometer Thermo Scientific MSQ Plus D D Oo Doc 065446 01 11 12 Dionex ICS 5000 Operator s Manual Analytical IC 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 co
322. nt 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 334 Doc 065446 01 11 12 oa EG Service 9 12 Replacing Tubing and Fittings bo 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 Dionex CR TC ELUENT OUT precision cut to EG degas ELUENT IN 0 062 mm 0 0025 in ID PEEK 61 cm 24 in Tubing assembly Blue 072204 Dionex CR TC ELUENT IN to precision cut Dionex EGC 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 Dionex CR TC REGEN IN PEEK 64 cm 25 in Tubing assembly Clear 072225 Dionex CR TC REGEN OUT 1 58 mm 0 062 in ID to waste ETFE ethylene tetrafluoroethylene 2 1m 7 ft 10 mm 0 39 in ID Colorless 055075 Drip tray drain hose polyethylene Table 9 3 Tubing and Fittings for a Capillary IC EG Channel Doc 065446 01 11 12 335 Dionex ICS 5000 Operator s Manual Tubing Fitting Size Color P N Use to connect and Type High pressure 10 32 Blue 074449 Use high pressure fittings for fitting bolt all other tubing connections including Pump outlet to Dionex EGC IN e Dionex EGC OUT to Dionex CR TC ELUENT IN
323. ntive Maintenance Kit 075039 DP SP Capillary Annual Preventive Maintenance Kit Doc 065446 01 11 12 443 Dionex ICS 5000 Operator s Manual 444 Doc 065446 01 11 12 so EG Reordering Information Part Number Item Dionex Consumables for Capillary EG 072076 EGC KOH Capillary 072077 EGC MSA Capillary 072078 CR ATC Capillary 072079 CR CTC Capillary Dionex Consumables for Analytical EG Standard Pressure Systems 074536 EGC 300 K2C03 074532 EGC 300 KOH 074534 EGC 300 LiOH 074535 EGC 300 MSA 074533 EGC 300 NaOH 075550 CR ATC 500 075551 CR CTC 500 080135 EPM 300 Electrolytic pH Modifier 079943 EGC CO3 Mixer 4 mm 063443 EGC CO Mixer 2 mm Dionex Consumables for Analytical EG High Pressure Systems 075778 EGC 500 KOH 075779 EGC 500 MSA 075550 CR ATC 500 075551 CR CTC 500 Precision Cut Tubing for Capillary EG 072203 0 062 mm 0 0025 in ID PEEK 61 cm 24 in Dionex CR TC ELUENT OUT to EG Degas ELUENT IN 072204 0 062 mm 0 0025 in ID PEEK 18 cm 7 in Dionex CR TC ELUENT IN to Dionex EGC OUT Backpressure Coils AAA 053762 Backpressure coil 2 0 mL min 500 psi 4 mm Doc 065446 01 11 12 445 Dionex ICS 5000 Operator s Manual Part Number Item AAA 053763 Backpressure coil 2 0 mL min 1000 psi 4 mm 053764 Backpressure coil 0 5 mL min 5
324. nual 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 See Appendix A for flow rate 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 Dionex EGC type and cartridge configuration For details see Section 4 9 EGI1 invalid ion count or EG2 invalid ion count This error occurs if the ion count reported by the Dionex EGC is invalid This may indicate a problem with the memory chip in the Dionex EGC To troubleshoot 1 Make sure the Dionex 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 250 Doc 065446 01 11 12 8 EG Troubleshooting EG1 invalid serial number OF EG2 inval