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Thermo Scientific Dionex ICS-5000, Operator'S Manual

The Thermo Scientific Dionex ICS-5000 Operator's Manual is an essential resource for users of this advanced analytical instrument. Obtain in-depth knowledge on operating procedures, troubleshooting, and maintenance. Experience seamless performance with this high-quality manual, available for free download from our website, ensuring optimal utilization of the product.

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8 • Troubleshooting

Doc. 065342-06 12/11

217

3 seconds. Repeat two or three times. If the baseline does not improve, 
check the other causes of baseline instability described in this section. 

NOTE

To prevent air from becoming trapped in the cell in the future, 
increase the backpressure on the cell by connecting backpres-
sure tubing to the cell outlet. The backpressure limit for the 
ED cell is 690 kPa (100 psi). Do not exceed this limit.

•

(DC Amperometry and Integrated Amperometry modes) Frequent, 
random spikes in the baseline

The pH-Ag/AgCl reference electrode diaphragm is plugged. First, try 

regenerating the pH-Ag/AgCl reference electrode frit by soaking the 
electrode in a solution of 1 M KCl plus 1 M HCl. If this does not 
eliminate the spiking, replace the electrode (P/N 061879).

•

(DC Amperometry and Integrated Amperometry modes) Regular 
baseline oscillation on high-sensitivity ranges

Reconnect the short length of titanium tubing to the cell inlet (see 

Figure 2-30

).

•

(DC Amperometry and Integrated Amperometry modes) Dirty or 
pitted conventional (nondisposable) working electrode

Polish the working electrode (see 

Section 9.28.4

). If you are using a 

disposable electrode, replace it.

•

(Integrated Amperometry mode) Regular baseline oscillations

1. Check the pump pressure plot to verify that the pump is working 

properly.

2. Air bubbles may be trapped inside the cell. While wearing gloves and 

eye protection, generate a slight temporary backpressure by putting 
your finger over the end of the cell outlet tubing for 2 to 3 seconds. 

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.

Summary of Contents for Dionex ICS-5000

Page 1: ...Dionex ICS 5000 Ion Chromatography System Operator s Manual Document No 065342 Revision 06 December 2011 ...

Page 2: ...c 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...

Page 3: ... s Manual 15 1 4 Safety and Regulatory Information 16 1 4 1 Safety Messages and Notes 16 1 4 2 Safety Symbols 18 1 4 3 Declaration of Conformity 19 1 5 Deionized Water Requirements for IC 20 2 Description DP SP Description 21 2 1 DP SP Front Features 21 2 2 DP SP Interior Components 23 2 2 1 Pump Heads 24 2 2 2 Pressure Transducer 25 2 2 3 Proportioning Valves Gradient pump only 25 2 2 4 Vacuum De...

Page 4: ...EO Optional 34 2 5 2 Pressurizing Eluent Reservoirs 34 2 5 3 Filtering Eluent 36 EG Description 37 2 6 EG Front Features 37 2 7 EG Interior Components 38 2 8 EG Rear Panel 45 2 9 EG Flow Schematics 47 DC Description 51 2 10 DC Front Features 51 2 11 DC Interior Components 53 2 11 1 DC Interior Components for Capillary IC 54 2 11 2 IC Cube for Capillary IC 55 2 11 3 DC Interior Components for Analy...

Page 5: ...5 3 Palladium Hydrogen PdH Reference Electrode 79 2 16 DC Rear Panel 80 2 17 I O Option 83 2 17 1 I O Option Connections 84 2 17 2 Analog Outputs 85 2 17 3 Power Relay and TTL Outputs 87 2 17 4 TTL Inputs 89 2 18 Automation Manager 94 2 18 1 AM High Pressure Switching Valves 96 2 18 2 AM Low Pressure Valves 97 2 18 3 AM High and Low Pressure Valve Control 98 2 18 4 RCH 1 Reaction Coil Heater 101 2...

Page 6: ... 23 1 Injection Valve Operation 122 2 23 2 Injection Valve Plumbing 124 2 24 Column Identification ID System 125 2 25 Gas and Humidity Sensors 126 2 26 TC Theory of Operation 127 2 26 1 Predictive Performance 128 3 Configurations 3 1 Overview 129 4 Startup 4 1 Operating Precautions 141 4 1 1 EG Operating Precautions 141 4 1 2 ED Cell Operating Precautions 143 4 2 System Startup Checklist 146 4 3 P...

Page 7: ...Starting the Chromeleon 6 8 Server 150 4 5 2 Starting the Chromeleon 6 8 Client 151 DP SP Startup 153 4 6 Setting Up the Eluent Reservoirs 153 4 7 Setting Up the Piston Seal Wash System 154 4 8 Starting the Pump 157 EG Startup 161 4 9 Entering the Eluent Concentration 161 4 10 Selecting an Eluent Concentration 162 DC Startup 165 4 11 Starting the DC 165 4 12 Equilibrating the System and Verifying ...

Page 8: ...r Concentrator 178 5 3 1 Loading Samples with an Autosampler 178 5 3 2 Loading Samples with a Syringe 178 5 3 3 Loading Samples with a Vacuum Syringe Pull Method 179 5 4 Autosampler Commands for Loading and Injecting Samples 180 6 Shutdown DP SP Shutdown 183 EG Shutdown 185 6 1 Short term Shutdown 185 6 2 Long term Shutdown 185 DC Shutdown 187 6 3 Consumables Storage 187 6 4 ED Cell Storage 187 6 ...

Page 9: ...ance 191 7 1 3 Periodic Maintenance 192 7 1 4 Annual Maintenance 192 DP SP Routine Maintenance 195 7 2 DP SP Daily Maintenance 195 7 3 DP SP Weekly Maintenance 195 7 4 DP SP Periodic Maintenance 196 7 5 DP SP Annual Maintenance 196 EG Routine Maintenance 197 7 6 EG Daily Maintenance 197 7 7 EG Weekly Maintenance 197 7 8 EG Annual Maintenance 197 DC Routine Maintenance 199 7 9 DC Daily Maintenance ...

Page 10: ...8 Troubleshooting 8 1 Audit Trail Error Messages 203 8 1 1 DP SP Error Messages 204 8 1 2 EG Error Messages 205 8 1 3 DC Error Messages 207 8 1 4 TC Error Messages 209 8 2 Noisy Baseline 214 8 3 Poor Retention Time Reproducibility 218 8 4 Peak Retention Times Are Too Early 220 8 5 Peak Retention Times Are Too Late 220 8 6 No Peaks 220 8 7 Tailing Peaks 222 8 8 Low System Backpressure 223 8 9 High ...

Page 11: ...1 8 19 Troubleshooting EG Error Messages 241 8 20 EG ALARM LED Is Lighted 253 8 21 EG POWER LED Fails to Light 254 8 22 Liquid Leaks in the EG 254 8 23 No Flow 255 8 24 EG Stops Operation 256 DC Troubleshooting 259 8 25 Troubleshooting DC Error Messages 259 8 26 Liquid Leaks from DC Components 270 8 27 VALVE Button Not Working 271 8 28 ED Cell Troubleshooting 271 8 28 1 ED Cell pH Readout Always 7...

Page 12: ...re Stabilizer Not Operating Properly 301 9 Service 9 1 Connecting Capillary Tubing 303 9 2 Tightening Guidelines for High Pressure Fittings 305 DP SP Service 306 9 3 Replacing Tubing and Fittings 306 9 4 Cleaning Eluent Reservoirs 308 9 5 Priming the DP SP 308 9 5 1 Priming with the PUMP PRIME Button 309 9 5 2 Priming from the Chromeleon Panel 310 9 6 Replacing the Check Valves 312 9 6 1 Removing ...

Page 13: ...ing the DP SP Priming Valve Knob Seal 329 9 11 Changing the DP SP Main Power Fuses 330 EG Service 333 9 12 Replacing Tubing and Fittings 333 9 12 1 Tubing and Fittings for Capillary IC EG Channels 333 9 12 2 Tubing and Fittings for Analytical IC EG Channels 335 9 13 Isolating a Restriction in the Liquid Lines 336 9 14 Replacing the EGC 336 9 14 1 Removing the Old EGC 337 9 14 2 Disposing of the Ol...

Page 14: ...9 20 Connecting a Sample Loading Port to the Injection Valve 363 9 21 Replacing the Leak Sensor 364 9 22 Rebuilding a High Pressure Injection Valve 366 9 23 Replacing a High Pressure Injection Valve Pod 367 9 24 Installing or Replacing an I O Option Board 369 9 25 Changing the DC Main Power Fuses 371 9 26 IC Cube Service Procedures 372 9 26 1 Replacing an IC Cube Cartridge 372 9 26 2 Replacing Cap...

Page 15: ... 9 28 6 Calibrating the pH Ag AgCl Reference Electrode 394 9 28 7 Replacing the pH Ag AgCl Reference Electrode O Ring 399 9 28 8 Replacing a PdH Reference Electrode 400 9 28 9 Replacing an ED Detector 404 TC Service 407 9 29 Replacing Tubing and Fittings 407 9 30 Setting Up the Column ID System 408 9 31 Rebuilding an Injection Valve 410 9 32 Replacing an Injection Valve Pod 411 9 33 Changing the M...

Page 16: ...onex ICS 5000 Operator s Manual xiv Doc 065342 06 12 11 B Reordering Information DP SP Reordering Information 435 EG Reordering Information 439 DC Reordering Information 441 TC Reordering Information 445 ...

Page 17: ...ression 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 Figure 1 1 Dual Dionex ICS 5000 System with RFIC EG Dionex ICS 5000 Detector Chromatography M...

Page 18: ...ypically from 0 2 to 0 5 mL min Standard bore IC applications use 4 mm diameter columns with flow rates typically from 1 0 to 2 0 mL min A dual Dionex ICS 5000 system can be configured with any combination of the above application types for example one capillary IC channel and one microbore IC channel or two capillary IC channels or one microbore IC channel and one standard bore IC channel 1 1 1 D...

Page 19: ...one of the following pump types Isocratic capillary IC pump Isocratic analytical IC pump 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 Detector inside DC Dionex ICS 5000 Conductivity Detec...

Page 20: ...Pa 5000 psi without RFIC and up to 21 MPa 3000 psi with RFIC Before operating at pressures above these limits verify that you have the appropriate pump HPC is stamped on the secondary pump heads of the older lower pressure rated capillary IC pumps HPC 2 is stamped on the secondary pump heads of the newer higher pressure rated capillary IC pumps A Capillary Pump High Pressure Upgrade Kit P N 075994...

Page 21: ...riate for the eluent being generated A Continuously Regenerated Trap Column CR TC to remove any extraneous contaminants from the deionized water source The CR TC is electrolytically regenerated which allows it to operate for extended periods without chemical regeneration A high pressure gas removal device that removes electrolysis gases created during eluent generation Two versions of EGC and CR T...

Page 22: ...ailable 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 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...

Page 23: ...upper compartment of the DC For a dual system two CDs can be installed Dionex ICS 5000 Electrochemical Detector ED The ED is a modular detector and a modular cell The ED supports multiple waveforms multiple integration times and post analysis data manipulation With Chromeleon 6 8 the ED is also capable of providing 3D amperometry data The ED cell can be configured with gold silver platinum carbon ...

Page 24: ... electrochemical detection The TC is available in four configurations With one 2 position 6 port high pressure injection valve With two 2 position 6 port high pressure injection valves With one 2 position 6 port high pressure injection valve and one 2 position 10 port high pressure injection valve With no injection valves An optional temperature stabilizer standard bore P N 064548 microbore P N 06...

Page 25: ...ICS 5000 holds 50 vials either 0 5 mL or 5 0 mL or a combination of the two sizes Vials can be sampled in any order and multiple samples can be taken from each vial The Dionex AS DV remembers the vial size and volume delivered for each vial position allowing multiple samples to be taken from a vial non sequentially Dionex AS Autosampler AS The AS is a powerful full featured autosampler that precis...

Page 26: ... 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 det...

Page 27: ...igured with Chromeleon Xpress Chromeleon Xpress provides real time control and monitoring of Dionex chromatography instruments but does not include data management capabilities In Chromeleon 7 an ePanel Set provides centralized system control You can use the ePanel Set to view system status information and issue commands for controlling each module In Chromeleon 6 8 these functions are available o...

Page 28: ...ex ICS 5000 Operator s Manual 12 Doc 065342 06 12 11 the Home panel in Chromeleon 7 and Figure 1 3 shows the Home panel in Chromeleon 6 8 Figure 1 2 Chromeleon 7 ePanel Set Dionex ICS 5000 Home Panel Shown ...

Page 29: ...1 Introduction Doc 065342 06 12 11 13 Figure 1 3 Chromeleon 6 8 Panel Tabset Dionex ICS 5000 Home Panel Shown ...

Page 30: ...on instructions is provided in the software ship kit Source Part Number PDF File Printed Manual Thermo Scientific Dionex ICS 5000 Ion Chromatography System Operator s Manual 065342 Yes No Installing the Thermo Scientific Dionex ICS 5000 Ion Chromatography System 065343 Yes Yes Dionex AS Autosampler Operator s Manual 065051 Yes No Dionex ICS Series Photodiode Array Detector Operator s Manual 065147...

Page 31: ...der for assistance Chapter 1 Introduction An overview of the Dionex ICS 5000 system includes a brief description of the Dionex ICS 5000 modules the software required for Dionex ICS 5000 operation and the Dionex ICS 5000 user manuals Chapter 2 Description Detailed descriptions of Dionex ICS 5000 system components and important operating features includes an introduction to Chromeleon software Chapt...

Page 32: ...Fisher Scientific office 1 4 1 Safety Messages and Notes This manual contains warnings and precautionary statements that can prevent personal injury and or damage to the Dionex ICS 5000 system when properly followed Safety messages appear in bold type and are accompanied by icons as shown below Chapter 8 Troubleshooting List of Chromeleon Audit Trail error messages and a list of minor problems tha...

Page 33: ...graves à mortelles Signale une situation de danger potentiel qui si elle n est pas évitée pourrait entraîner des blessures graves à mortelles Signale une situation de danger potentiel qui si elle n est pas évitée pourrait entraîner des blessures mineures à modérées Également utilisé pour signaler une situation ou une pratique qui pourrait gravement endommager l instrument mais qui n entraînera pas...

Page 34: ...IC systems only Sections preceded with the Analytical IC flag indicate that the information in 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 Capillary IC Alternating current...

Page 35: ...Doc 065342 06 12 11 19 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 ...

Page 36: ...ionized water that meets the specifications listed in Table 1 1 Contaminant Specification Ions Resistivity 18 0 megohm cm Organics TOC 10 ppb Iron Transition Metals 1 ppb Pyrogens 0 03 Eu mL Particulates 0 2 µm 1 units mL Colloids Silica 10 ppb Bacteria 1 cfu mL Iron transition metal content not specified for ASTM Type I Water Table 1 1 ASTM Filtered Type I Deionized Water Specifications for Ion C...

Page 37: ...ex ICS 5000 Single Pump SP includes buttons for controlling certain pump functions as well as LEDs light emitting diodes that indicate the status of several pump functions see Figure 2 1 and Figure 2 2 ICS 5000 DP SP Figure 2 1 DP Status Bar Figure 2 2 SP Status Bar ALARM PUMP 1 PUMP 2 CONNECTED FLOW PRIME FLOW PRIME ALARM CONNECTED PUMP 1 FLOW PRIME ...

Page 38: ...FLOW button to start and stop the pump flow The LED indicates when the flow is on Does not flash PUMP 1 PRIME PUMP 2 PRIME Use the PRIME button to prime the pump see Section 9 5 The LED indicates whether the pump is being primed The pump is being primed POWER 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 ...

Page 39: ...e unique to a gradient analytical pump Figure 2 3 Example DP Interior Components Pump 1 Analytical Gradient Pump Pump 2 Capillary Isocratic Pump Status Bar Priming Valve Vacuum Degas Chamber one channel Piston Seal Wash Reservoir Eluent Supply On Off Valve isocratic pumps only Tubing Chase 2 Primary Pump Head Secondary Pump Head Handle 2 Peristaltic Pump for seal wash system 1 3 2 4 7 8 9 9 10 12 ...

Page 40: ...ary head are connected in series Eluent passes through both pump heads in succession The primary pump head delivers eluent at the selected flow rate while simultaneously filling the secondary pump head The latter serves as a reservoir and delivers eluent while the primary head carries out the refill stroke The characteristic feature of the patented isokinetic pre compression phase is the programme...

Page 41: ...plications 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 2 2 4 Vacuum Degassing Module The DP SP vacuum degassing module provides continuous online eluent degassing Eluent quality significantly affects DP SP performance and vacuu...

Page 42: ...n the Commands dialog box 3 Select the pump name 4 Select the Degasser property and select Off 5 For Chromeleon 6 8 click Execute 6 To turn on the degasser again select On 2 2 5 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...

Page 43: ...t proportioned eluents are mixed thoroughly In the isocratic pump the mixer is optional but can function as a pulse damper The DP SP gradient delay volume is 600 L when a GM 3 is installed and 380 L when a GM 4 is installed The gradient delay volume or dwell volume is the volume of liquid in the system between the point where the gradient is formed and the point where it enters the column This inc...

Page 44: ...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 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 Figure 2 5 Isocratic Pump Flo...

Page 45: ...he 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 Flow exits the secondary pump head continues through the static mixer and is then directed to the eluent generator if installed or injection valve and then to the remainder of the chromatography system Figure ...

Page 46: ...Receptacle The rear panel power switch is the main power switch for the DP SP Turn on the main power switch before initial operation and leave it on unless instructed to turn it off for example before performing a service procedure Figure 2 7 DP SP Rear Panel 1 2 3 5 6 7 8 4 Tubing Chase 2 USB Receptacle B Connectors Main Power Switch Fuse Holder and Power Receptacle Drain Port USB Ports 3 A Conne...

Page 47: ...main disconnect device Make sure the socket outlet is located near the DC and is easily accessible Le cordon d alimentation principal est utilisé comme dispositif principal de débranchement Veillez à ce que la prise de base soit située installée près du module et facilement accessible Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher daß sich die Steckdose nahe am G...

Page 48: ...ound 10 Gnd Ground Ground 11 Gnd Ground Ground 12 Gnd Ground Ground 13 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 17 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 T...

Page 49: ...rovided in the pump ship kit Waste and Drain Lines One waste line is connected to the secondary pump head on each pump and is routed through the tubing chace to the rear of the DP SP The drain port removes any liquid that collects in the drip tray in the bottom of the DP SP A clear corrugated drain hose P N 055075 is connected to this port during installation Place the free ends of the waste lines...

Page 50: ...ed with four 2 liter reservoirs P N 072058 2 5 2 Pressurizing Eluent Reservoirs All eluent reservoirs available for use with the DP SP can be pressurized Although the DP SP does not require pressurized reservoirs Thermo Fisher Scientific recommends pressurizing reservoirs with helium or nitrogen under the following circumstances When using eluents that are sensitive to contamination Do not use the...

Page 51: ...PDA Regulator Bracket Kit P N 074424 is required The kit includes the EO Regulator Kit described above as well as a right angle regulator bracket and mounting hardware After attaching the bracket to the TC or detector you will mount the gas regulator assembly on the bracket If more reservoirs are required order a second regulator P N 074423 For instructions on installing the regulator kits refer t...

Page 52: ...ir s eluent line End line filters are provided in the pump ship kit A Dionex High Pressure Inline Filter P N 044105 can be used to remove particulates down to 0 45 micron from eluent Connect the inline filter between the pump outlet and the eluent inlet port on the injection valve For details see the instructions provided with the inline filter ...

Page 53: ...instrument or a Chromeleon 6 8 timebase ALARM An EG related problem has occurred for example the eluent generator cartridge EGC was disconnected Check the Chromeleon Audit Trail for the cause EGC 1 EGC 2 The EGC is on and is generating eluent EGC 1 is always installed in the left section of the component compartment EGC 2 if present is installed in the right section of the compartment CR TC 1 CR T...

Page 54: ...2 of a dual channel EG Each section holds the components for either a capillary IC or an analytical IC system A dual channel EG can hold components for two capillary IC systems two analytical IC systems or one system of each type Figure 2 9 shows the component panel for a capillary IC system Figure 2 10 shows the component panel for an analytical IC system POWER Use this POWER button for routine o...

Page 55: ...and pull the tray forward until it reaches the stop Figure 2 9 Example EG Interior Components for a Capillary IC System System 1 Shown CR TC Capillary Leak Sensor EGC Capillary Slide Release Latch 1 3 4 5 6 4 2 1 3 5 Note For a capillary IC system the eluent degasser is installed in the IC Cube Drip Tray 6 Chase for Electrical Cables 2 ...

Page 56: ...Figure 2 10 Example EG Interior Components for an Analytical IC System System 2 of a Dual Channel EG Shown EGC III Analytical CR TC Analytical RFIC Eluent Degasser for Analytical IC only Drip Tray Electrical Cables Slide Release Latch 1 2 3 4 5 5 4 1 2 3 6 6 ...

Page 57: ...IC Systems EGC KOH Capillary 072076 Generates potassium hydroxide eluent for anion exchange separations EGC MSA Capillary 072077 Generates methanesulfonic acid eluent for cation exchange separations Eluent Generator Cartridges and Accessories for Analytical IC Systems EGC III K2CO3 074536 Generates potassium carbonate eluent for anion exchange separations EPM III Electrolytic pH Modifier 080135 Pr...

Page 58: ...ry DVD P N 053891 NOTE Do not install a CR TC in the same channel as an EGC K2CO3 or an EPM III Electrolytic pH Modifier NOTE The Thermo Scientific Dionex IonPac ATC HC Trap Col umn P N 059604 or Thermo Scientific Dionex IonPac CTC 1 Trap Column P N 040192 may be used with the EG However both Dionex IonPac trap columns require off line chemical regeneration Contact Thermo Fisher Scientific for mor...

Page 59: ...refer to Section 9 17 EPM III Electrolytic pH Modifier and Carbonate Mixer The EGC III K2CO3 can be used with an EPM III Electrolytic pH Modifier P N 080135 and a carbonate mixer P N 061686 4 mm P N 063443 2 mm to produce a carbonate bicarbonate mixture for use with anion exchange separations on carbonate based Dionex IonPac columns After the cartridge generates potassium carbonate eluent the EPM ...

Page 60: ...are two sets of electrical connectors one per channel Connections for the following components are provided Two EGCs or one EGC and one EPM and Two CR TCs When operating with an EGC III K2CO3 and the EPM III the EGC is connected to the EGC power supply for one channel and the EPM is connected to the EGC power supply for the second channel Thus the EG can accommodate only one such configuration ...

Page 61: ...onnections One USB receptacle B type connector allows a connection from the PC on which Chromeleon is installed Two USB Universal Serial Bus ports A type connectors are provided for connections to other Dionex ICS 5000 modules Figure 2 12 EG Rear Panel Exhaust Fan Gas Vent Lines Fuse Holder Main Power Switch and Power Receptacle Drain Port USB Receptacle B Connector USB Ports 2 A Connectors Tubing...

Page 62: ...bing 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 The lines exiting the tubing chase white tubing are for connecting the REGEN IN port on the RFIC Eluent Degasser or EPM III Electrolytic pH Modifier to the REGEN OUT port on the suppressor The gas vent line clear tubing discharges the electroly...

Page 63: ...ows through the backpressure coil if installed through the injection valve to the separator column and finally to the detector cell The detector cell effluent is directed through the suppressor regenerant chamber to the degasser regenerant tubing through the CR TC regenerant chamber and finally to waste The flow paths for a capillary IC and an analytical IC system are the same However in a capilla...

Page 64: ...PER EGC IN To CR TC Regen Out blue label To CR TC Eluent In red label ELUENT OUT REGEN IN To EG Degas Regen Out blue label To CR TC Regen In orange label Vent WASTE GAS SEPARATOR To CR TC Eluent Out yellow label To EG Degas Eluent In red label EG Degas Cartridge inside DC ELUENT IN REGEN OUT ELUENT OUT To Inject Valve EGC Capillary ...

Page 65: ...eference Library DVD P N 053891 Figure 2 14 EG Flow Schematic Example for Analytical IC Eluent Out EGC VENT To Waste EGC IN EGC OUT EGC Inlet Outlet TO INJ VALVE P TO PUMP WASTE GAS SEPARATOR Coupler TO SRS AES REGEN OUT Eluent In CR TC Coupler ELUENT OUT REGEN IN TO CR TC REGEN OUT blue label To CR TC Eluent In red label To CR TC Eluent Out yellow label To CR TC Regen In orange label RFIC Eluent ...

Page 66: ...Dionex ICS 5000 Operator s Manual 50 Doc 065342 06 12 11 ...

Page 67: ...6 8 timebase Does not flash ALARM The leak sensor is wet or there was a valve or suppressor error Check the Chromeleon Audit Trail for the cause Does not flash SUPPRESSOR 1 SUPPRESSOR 2 The suppressor is on and current is being applied Does not flash OVEN UPPER The upper compartment is at its set temperature The upper compartment is transitioning to the set temperature The compartment is not ready...

Page 68: ...o injection valves installed inside the DC A syringe can then be used to manually load sample through the ports For automated sample VALVE 1 LOAD VALVE 2 LOAD VALVE 1 INJECT VALVE 2 INJECT 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 Valve error See Section 8 25 for troubleshooti...

Page 69: ...n the lower door The upper and lower compartments are isolated from each other in separate temperature zones There is no common air flow between the two compartments For details about DC temperature control see Section 2 12 The compartments can accommodate the components necessary for up to two IC systems The following configurations are possible Single system one capillary IC or one analytical IC...

Page 70: ... The DC upper compartment consists of two sections The top section houses one or two Dionex IC Cubes IC Cube For details about the IC Cube see Section 2 11 2 The tray slides forward for easy access to components 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 abou...

Page 71: ...stalled NOTE When an IC Cube is installed a Dionex ICS 5000 Automa tion Manager cannot be included in the DC Each IC Cube includes an injection valve a column heater and four component cartridges that slide into the housing Each cartridge holds a capillary IC component and includes the plumbing required to connect the component to other IC Cube and system components Figure 2 17 Example DC Interior...

Page 72: ...removes the carbonate peak contributed by the sample in hydroxide eluent chemistries Removal occurs immediately after suppression of the eluent before the sample reaches the detector The CRD 200 Capillary is optimized for operation at the flow rate range typically used with capillary columns The CRD and tubing connections inside the cartridge are not accessible Tubing exits the front of the cartri...

Page 73: ...ressor The suppressor and tubing connections inside the cartridge are not accessible Tubing exits the front of the cartridge to allow connection to other capillary IC components When the cartridge is installed in the IC Cube pins on the rear of the cartridge connect the suppressor to its power source For details about the suppressors refer to the suppressor manuals The manuals are on the Thermo Sc...

Page 74: ...e columns and column plumbing The capillary columns are ordered separately For information about how to replace columns and column tubing see Section 9 26 2 EG Degas Cartridge The EG degas capillary cartridge contains a tubing assembly that purges the electrolysis gas from eluent that has been generated by an EG After passing through the degas tubing the eluent is directed to the injection valve a...

Page 75: ...uding the flow through components installed inside the IC Cube cartridges see Section 2 14 3 Figure 2 19 IC Cube Eluent and Regenerant Flow Schematic for Conductivity Detection Capillary IC From CR TC Eluent Out Port To CR TC Regen In Port CRD 200 EG DEGAS From Autosampler To Waste ELUENT IN ELUENT IN ELUENT OUT ELUENT OUT REGEN IN CES 300 ELUENT IN ELUENT OUT ELUENT IN REGEN OUT ELUENT OUT SAMPLE...

Page 76: ... configured for electrochemical detection Figure 2 20 IC Cube Eluent and Regenerant Flow Schematic for Electrochemical Detection PdH Electrode Shown CRD BYPASS EG DEGAS REGEN IN SUPPRESSOR BYPASS ELUENT IN ELUENT OUT ELUENT IN REGEN OUT ELUENT OUT SAMPLE IN SAMPLE OUT ELUENT IN ELUENT OUT IN OUT EC CELL From Autosampler To Waste From CR TC Eluent Out Port To CR TC Regen In Port 1 2 3 5 6 4 7 8 9 9...

Page 77: ...M contains various components required for performing matrix elimination large volume pre concentration post column reagent addition and other functions See Section 2 18 for details about the AM 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 Sect...

Page 78: ...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 ...

Page 79: ...o temperature controlled devices CD cell IC Cube heater or RCH 1 are on Minimum temperature ambient 22 C If a temperature controlled device is set to 60 C or above Minimum temperature ambient 17 C Note The achieved temperature can be reduced another few degrees by setting the DC upper compartment fan speed to high see page 64 Maximum temperature ambient 20 C Lower compartment 10 to 70 C Minimum te...

Page 80: ...udes the parts and instructions required to verify the temperature calibration of the DC upper and lower com partments and to recalibrate if required To set the fan speed of the DC upper compartment to high 1 Open the Chromeleon 7 Instrument Configuration program or Chromeleon 6 8 Server Configuration program 2 Double click the DC icon under the instrument or timebase 3 Click the Thermal Controls ...

Page 81: ... auxiliary valves In an analytical IC system one 6 port high pressure valve is installed in the 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...

Page 82: ...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 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 ...

Page 83: ...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 L PEEK sample loop P N 042949 is installed between ports L 1 and L 4 Thermo Fisher Scientific offers sample loops in various size...

Page 84: ...n Figure 2 26 the flow occurs as follows In the Load position sample flows from the syringe or autosampler line through the valve and into the sample loop Excess sample flows out to waste Eluent flows from the eluent pump through the valve through the concentrator column and to the separator column If sample was previously loaded onto the concentrator column it is swept to the separator column for...

Page 85: ...running analytical standard bore or microbore flow rates The features and functions of the two CD versions are the same However because the cell volumes of the two are different the versions are not interchangeable The CD version must match the system type capillary IC or analytical IC If the CD version and system type are mismatched chromatograms will be affected for example broad peaks or lowere...

Page 86: ...ature compensation helps minimize changes in the baseline or in peak heights if the operating temperature is different from the temperature at which the cell was calibrated The default temperature compensation is 1 7 per C This can be reset to between 0 and 3 0 per C depending on the eluent If you notice that the baseline shifts up when the temperature increases the compensation factor is too low ...

Page 87: ...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 The analytical suppressor is installed on clips on the lower area of the analytical CD see Figure 2 27 The suppressor cable plugs into the connector next to the detector CD Type Availa...

Page 88: ...efer to Thermo Scientific Dionex ICS 5000 Ion Chromatography System Installation Instructions Document No 065343 2 14 3 System Flow Schematics for Conductivity Detection Figure 2 28 illustrates the flow path through a DC for a conductivity detection application using suppression in recycle mode For information about other suppression modes refer to the suppressor manuals The manuals are on the The...

Page 89: ...s through a 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 Figure 2 28 DC Flow Schematic for Conductivity Detection Suppression in Recycle Mode ELUENT IN TEMP STABILIZER CELL COND SUPPRESSOR PUMP or ELUENT GE...

Page 90: ... through the EG degas tubing and then 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 Figure 2 29 EG and DC Flow Schematic for Conductivity Detection Suppression in Recycle Mode 9 10 1 2 3 4 5 6 7 8 9 ELUENT IN CELL COND SUPPRESSOR GUARD SEPARATOR COLUMN VALVE 1 2 3 4 5 6 WASTE SAMPLE L P ...

Page 91: ... output if installed The detector is installed in the upper compartment of the DC see Figure 2 21 The cell mounts on the front of the detector The detector electronics are not accessible to the user The ED can perform the following electrochemical detection modes DC amperometry see Section 2 19 1 Integrated amperometry includes pulsed amperometric detection PAD and integrated pulsed amperometric d...

Page 92: ...ctrode 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 polye...

Page 93: ...ode containing a glass membrane pH half cell and a Ag AgCl half cell The combination pH electrode monitors eluent pH The Ag AgCl half cell is typically used as the cell reference electrode To minimize changes in the baseline the combination pH Ag AgCl electrode can be used as the reference electrode during a pH gradient pH Dependence The potentials at which many redox reactions take place on metal...

Page 94: ...u to determine when the pH Ag AgCl reference electrode needs regenerating or replacing thus improving the reproducibility of your analyses For instructions on how to monitor the pH readout see Section 4 1 2 NOTE Monitor the pH when the pH Ag AgCl reference electrode is used in the Ag mode as well as in the pH mode Do not allow the pH Ag AgCl reference electrode to dry out Make sure that eluent is ...

Page 95: ...ion 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 ion...

Page 96: ...strates the rear panel of the DC 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 Figure 2 31 DC Rear Panel Tubing Chase 2 Analog Output and TTL Relay Connectors optional USB Receptacle B Connector External Low Pressure Valve Connectors Switched AC Sockets Fuse Holder Main Power Switch and Power R...

Page 97: ...o turn off the DC press and hold the POWER button for 2 seconds The power cord plugs into the IEC 320 three prong receptacle USB Connections The USB Universal Serial Bus receptacle B type connector allows connection to the PC on which Chromeleon software is installed The two USB ports A type connectors allows connection to other USB devices in the system for example the pump and eluent generator A...

Page 98: ...O option P N 062201 is installed the following connections are provided Two analog outputs one for each detector One 5V power output Two relay outputs Two TTL outputs Eight programmable TTL inputs See Section 2 17 for details about the I O option Drain Port The drain port removes any liquid that collects in the drip tray in the bottom of the DC A clear corrugated drain hose P N 055075 is connected...

Page 99: ...1 83 2 17 I O Option When the I O option P N 062201 is installed two 12 pin connector strips are on the DC rear panel Figure 2 32 describes the functions assigned to each connector pin Figure 2 32 Optional Rear Panel I O Connector Strips ...

Page 100: ...e ground pin 3 Plug the connector into the appropriate 12 pin connector on the DC rear panel 4 Connect the wires from the DC connector plug to the appropriate connector pins on the other modules Additional connector plugs are provided with other Dionex modules NOTE Check the polarity of each connection Connect signal wires to signal pins and ground wires to ground pins 5 If you connected a TTL inp...

Page 101: ...rred settings on the detector panel on the Chromeleon 7 ePanel Set see Figure 2 34 or Chromeleon 6 8 panel tabset Analog Output Setting Values Description Full scale voltage 0 01 0 10 or 1 00 V Sets the voltage output of a full scale detector response The voltage to use depends on the recording device to which the analog output is connected For example if the analog output is connected to a device...

Page 102: ...the full scale analog output An offset allows a recording device to plot the signal if it becomes negative The offset level does not affect the magnitude of the output signal Polarity Positive Negative Use this setting to set the polarity of the analog output signal to either positive the default or negative In applications in which the analyte output is lower than the background signal the polari...

Page 103: ...connection can be either normally open N O or normally closed N C see Figure 2 35 Choose N O or N C based on what you want the state of the connected device to be when the DC power is turned off A normally open relay is open when the relay is switched off and closed when the relay is turned on A normally closed relay is closed when the relay is off and is open when the relay is on Figure 2 34 Cond...

Page 104: ...ion for the external device for connection instructions Figure 2 35 Relay Output Configuration RELAY OUTPUT CONFIGURATION The relays are capable of switching 2 A at 24 VDC For a normally open connection connect a COM pin and an N O pin For a normally closed connection connect a COM pin and an N C pin NOTES N O COM N C Rear Panel Pins Relay Output on DC Electronics Non Energized Relay N O COM N C E...

Page 105: ... 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 Injection valves left and right load inject AM high pressure valves A and B A B AM low pressure valves A and B open closed DC low pressure valves A through F on the rear panel open closed Figure ...

Page 106: ...omeleon 6 8 Server Configuration program You can assign one or more functions to each input NOTE If two timebases are sharing the DC the TTL input functions are shared between the timebases For example if TTL input 1 is assigned to control injection valve 1 that function is assigned to both timebases You do not need to associate a TTL input with a particular timebase To select TTL input control fu...

Page 107: ...cription Doc 065342 06 12 11 91 3 Select the TTL Inputs tab see Figure 2 37 4 Select the name of the input and press the F2 key or double click the name Figure 2 37 DC Server Configuration Properties TTL Inputs ...

Page 108: ...ected functions 6 By default several functions are selected Scroll down the list and disable all unwanted functions TTL Input Control Types The DC TTL inputs respond to four types of signals to accommodate different controlling devices The default control type Normal Edge is compatible with the output signals provided by Dionex modules If the device connected to the DC does not send a normal edge ...

Page 109: ...s it For the detector mark and offset functions the falling edge turns on the function and the rising edge has no effect Inverted Edge The inverted edge mode works identically to the normal edge mode except that the positive and negative edges are reversed in function Normal Pulse In normal pulse operation the negative falling edge of the TTL signal is the active edge and the positive rising edge ...

Page 110: ... pump injection valve reagent reservoirs etc depend on the application Refer to Chapter 3 for the configuration schematic for your application NOTE Because the AM requires the full width of the DC upper com partment an IC Cube cannot be installed in the DC when an AM is installed e AM is available in the following configura tions Figure 2 39 Dionex ICS 5000 Automation Manager Components Included P...

Page 111: ...loop AutoPrep standard loops 066343 AM tray with no valves 061734 AM Component Part Number High pressure valve 6 port 061961 High pressure valve 10 port 061962 Low pressure valve 3 way 061971 Low pressure valve 2 way 061745 RCH 1 Reaction Coil Heater 061746 Temperature stabilizer standard bore 0 25 mm 0 010 in ID 062561 Temperature stabilizer microbore 0 125 mm 0 005 in ID 062562 Figure 2 41 AM Co...

Page 112: ...liquid flow path through the valve ports at each valve position Valve port connections to chromatography components vary depending on the application Refer to Chapter 3 for the configuration schematic for your application Valves are controlled by Chromeleon see Section 2 18 3 Figure 2 42 High Pressure Switching Valve Flow Schematics 6 Port Valve Figure 2 43 High Pressure Switching Valve Flow Schem...

Page 113: ...e port connections to chromatography components vary depending on the application Refer to Chapter 3 for the system flow schematic for your application Valves are controlled by Chromeleon see Section 2 18 3 Figure 2 44 Three Way Low Pressure Valve Flow Schematics COM 0 1 N O N C OFF POSITION COM 0 1 N O N C ON POSITION N C normally closed N O normally open COM common flow Note When the valve is of...

Page 114: ...ed to control the high and low pressure valves For automated control commands for valve control can be included in a Chromeleon 7 instrument method or a Chromeleon 6 8 program To add AM valve control commands to a Chromeleon 7 instrument method use the Script Editor see Figure 2 45 Figure 2 45 Chromeleon 7 Script Editor ...

Page 115: ... 12 11 99 To add AM valve control commands to a Chromeleon 6 8 program use the Relay and State Devices Options page in the Program Wizard see Figure 2 46 Figure 2 46 Chromeleon 6 8 Program Wizard Relay and State Devices Options Page ...

Page 116: ... Manual 100 Doc 065342 06 12 11 For manual control of AM valves execute commands from the DC ePanel in Chromeleon 7 see Figure 2 47 or the DC Control panel in Chromeleon 6 8 Figure 2 47 Valve Control on DC ePanel in Chromeleon 7 ...

Page 117: ...ge of from 5 C above the temperature of the upper compartment up to 80 C For automated control of the heater commands can be included in a Chromeleon 7 instrument method see Figure 2 48 or Chromeleon 6 8 program For direct control of the heater use the controls on the DC ePanel in Chromeleon 7 or the Control panel in Chromeleon 6 8 Figure 2 48 Instrument Wizard DC Options Page in Chromeleon 7 ...

Page 118: ...mperometric detection IPAD see Section 2 19 2 Cyclic voltammetry see Section 2 19 3 2 19 1 DC Amperometric Detection In DC amperometry a constant potential is applied to the working electrode The potential can be entered into a Chromeleon 7 instrument method see Figure 2 49 or Chromeleon 6 8 program The applied voltage can be changed up to 10 times during the run The actual number of potential cha...

Page 119: ...tween optimized high positive and negative potentials the electrode surface is continually regenerated Current is measured by integration during a portion of the repeating potential vs time waveform See Section 2 19 4 for more information about waveforms Pulsed Amperometric Detection In pulsed amperometric detection PAD current is integrated at a single constant potential see Figure 2 50 The poten...

Page 120: ...orm shown in Figure 2 51 the current is integrated both while the potential is swept across the metal oxide formation wave and also during the reverse sweep across the oxide reduction wave This technique minimizes baseline shift and the peak dips that can occur when an eluting analyte s effect on oxide suppression is greater than the detector response from the analyte As with pulsed amperometric d...

Page 121: ...at the end of the scan is the same as at the beginning This results in a triangular waveform see Section 2 19 4 In the cyclic voltammetry mode the detector measures the current at a rate of 1 kHz i e 1000 raw data points per second are collected The data is compressed before storage to 20 Hz 2 19 4 Waveforms A waveform is a series of steps defined as points on a plot of potential vs time Waveforms...

Page 122: ...om 0 80 to 0 60 V and then from 0 60 to 0 80 V The total time for one waveform period is 28 s This provides a sweep rate of 0 1 V s as shown in the equation below Figure 2 52 Example Cyclic Voltammetry Waveforms Seconds 0 60 Volts 0 40 0 20 0 20 0 40 0 60 0 80 0 00 5 00 10 00 15 00 20 00 25 00 30 00 28 0 0 80 14 0 0 60 0 00 0 80 0 00 2 V CV Cycle Time Sweep Rate 2 1 4 V 28s 0 1 V s ...

Page 123: ...m period is 2 0 s However for 2D data because only one data point is generated per waveform period the effective maximum length of a waveform period depends on the data collection rate the rate at which Chromeleon collects digital data points from the detector The relationship is as follows Multiple waveforms can be defined for a single run provided they all have the same cycle duration Up to 15 w...

Page 124: ...age in the Instrument Method Wizard Chromeleon 7 or Program Wizard Chromeleon 6 8 Analytical vs Scanning Waveforms The pre programmed analytical waveforms supplied with Chromeleon are designed for quantitative analysis of specific compounds alcohols amino acids carbohydrates etc With analytical waveforms integration occurs either while a single constant potential is being applied over time see the...

Page 125: ... unknown peaks or to determine whether a substance is coeluting with another 2 19 5 Storing and Reprocessing Amperometry Data Chromeleon provides storage of 2D and 3D pulsed amperometry and integrated amperometry data For 2D data Chromeleon stores the detector s response at each waveform period s integration interval One integrated data point per waveform period is stored This allows you to produc...

Page 126: ...ion intervals are collected Displaying and Reprocessing 3D Data This section describes how to display and reprocess 3D amperometry data using Chromeleon 6 8 If you are using Chromeleon 7 the features described here are available by displaying the data in a contour plot For details refer to the Chromeleon 7 Help In Chromeleon 6 8 you can display and reprocess 3D amperometry data in the 3D Amperomet...

Page 127: ...3D Amperometry View Window in Chromeleon 6 8 Sample injection data Displays information about the sample Chromatogram plot Displays a chromatogram of data selected from the selected integration interval in the 3D amperometry data plot 3D amperometry data plot Displays the raw 3D amperometry data Waveform I t plot Displays an I t plot current vs waveform time of selected data and optionally a wavef...

Page 128: ...eform period ms The z axis which is represented by different colors in the plot is the response nA NOTE The 3D data shown in Figures 2 58 and 2 59 were collected using an analytical waveform see Analytical vs Scanning Waveforms on page 108 To switch to the 3D plot view right click on the Iso plot select Decoration and click the Iso 3D Plot tab The 3D view projects the response values in the third ...

Page 129: ... line Chromeleon can calculate a baseline I t plot for each data point of a peak Each I t plot measured at a given retention time can be corrected by subtracting the calculated baseline I t plot from the 3D amperometry data By definition if baseline correction is enabled 3D amperometry data is zero unless a peak is present Figure 2 59 3D Amperometry Data in Chromeleon 6 8 3D View retention time mi...

Page 130: ...Dionex ICS 5000 Operator s Manual 114 Doc 065342 06 12 11 ...

Page 131: ...lashing CONNECTED The TC is connected to a Chromeleon 7 instrument or a Chromeleon 6 8 timebase Does not flash ALARM A sensor detected the presence of a gas or humidity leak inside the TC or a valve or oven error was detected Check the Chromeleon Audit Trail for the cause Does not flash VALVE 1 LOAD VALVE 2 LOAD VALVE 1 INJECT VALVE 2 INJECT Indicates whether the injection valve is in the Load or ...

Page 132: ...ady for operation If the LED is flashing and the ALARM LED is lighted an oven error has been detected See Section 8 30 for troubleshooting POWER When the power is on this LED 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 Does not flash LED Label If the LED I...

Page 133: ...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 Figure 2 61 TC Interior Vie...

Page 134: ... 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 shipp...

Page 135: ... 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 Figure 2 62 TC Rear Panel USB Receptacle B Connector Main Power Switch Fuse Holder and ...

Page 136: ...if principal de débranchement Veillez à ce que la prise de base soit située installée près du module et facilement accessible Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung Stellen Sie sicher daß sich die Steckdose nahe am Gerät befindet und leicht zugänglich ist Figure 2 63 Digital I O Connector Connection Description Digital Input Digital_GND 0 to 5 V Relay_Com Relay_N O Switchin...

Page 137: ...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 Pin Signal Name Signal Level Core Color Core Label 1 Not occupied Pink Analog High 2...

Page 138: ...he pump through the valve and to the column bypassing the sample loop Sample flows from the syringe TC Description Part Number TC with no injection valves 074108 TC with one 2 position 6 port high pressure injection valve 074109 TC with two 2 position 6 port high pressure injection valves 074112 TC with one 2 position 6 port high pressure injection valve and one 2 position 10 port high pressure in...

Page 139: ...cted for an application that uses a concentrator column In the 10_1 position sample flows from the syringe or autosampler line through the valve and into the sample loop Excess sample flows out to waste Eluent flows from the eluent pump through the valve through the concentrator column and to the separator column If sample was previously loaded onto the concentrator column it is swept to the separ...

Page 140: ...the 6 port valve The injection valve is plumbed at the factory with all tubing and fittings for connection to the pump sample loading port column and waste A 25 L 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 L loop can be replaced with a loop that has a different sample injection volu...

Page 141: ...nformation 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 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 num...

Page 142: ...the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation Adjusting the Sensor Sensitivity Follow these steps to change the sensitivity setting of the gas or humidity sensor or to turn off a sensor 1 Open the Chro...

Page 143: ...gn of the TC reduces the time required to equilibrate the temperature between the column and the eluent Peltier elements in the TC heat up and cool down the columns They also help to bring the air and all of the installed components including the injection valves to the selected temperature If necessary a temperature stabilizer standard bore P N 064548 microbore P N 064650 can be installed in the ...

Page 144: ...on Monitoring of the injection valve usage Reminders for service and qualification periods including display of warning messages when limits are approaching or overdue Predictive Performance commands and parameters are available in the Chromeleon Commands dialog box Control Range Achieved Temperatures Based on Ambient 5 to 85 C Minimum temperature 18 C below ambient Maximum temperature 70 C above ...

Page 145: ...ge 132 Analytical IC Single System without EG CD page 133 Analytical IC Single RFIC EG System CD page 134 Analytical IC Dual RFIC EG System CD CD page 135 Analytical IC Dual RFIC EG System CD ED page 136 Analytical IC Single RFIC EG System with Matrix Elimination Using a DP and a 6 Port Valve page 137 Analytical IC Single RFIC EG System with Matrix Elimination Using an SP and a 10 Port Valve page ...

Page 146: ... ELUENT OUT ELUENT IN REGEN OUT ELUENT OUT SAMPLE IN SAMPLE OUT ELUENT IN ELUENT OUT Conductivity Detector Capillary CELL IN CELL OUT CRD 200 EG DEGAS ELUENT IN ELUENT IN ELUENT OUT ELUENT OUT REGEN IN CES 300 ELUENT IN ELUENT OUT ELUENT IN REGEN OUT ELUENT OUT SAMPLE IN SAMPLE OUT ELUENT IN ELUENT OUT Conductivity Detector Capillary CELL IN CELL OUT From IC Cube 1 EG Degas Regen Out To IC Cube 1 ...

Page 147: ...ide view EG left side view To waste System 1 System 2 System 1 System 2 Eluent In Eluent Out Regen In Regen Out EGC capillary pump not to scale CRD 200 EG DEGAS ELUENT IN ELUENT IN ELUENT OUT ELUENT OUT REGEN IN CES 300 ELUENT IN ELUENT OUT ELUENT IN REGEN OUT ELUENT OUT SAMPLE IN SAMPLE OUT ELUENT IN ELUENT OUT Conductivity Detector Capillary CELL IN CELL OUT From IC Cube 1 EG Degas Regen Out To ...

Page 148: ... IN ELUENT OUT Conductivity Detector Capillary CELL IN CELL OUT Piston Seal Wash Seal Wash Pump Eluent In Eluent Out Regen In Regen Out EGC capillary From autosampler To waste System 1 System 2 To EGC 2 In Separator Temp Stabilizer 1 L L S W P C 2 3 4 5 6 To waste Guard From autosampler Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Backpressure Device From the suppressor Regen Out via t...

Page 149: ... EG CD To the pump inlet via the pump rear chase DC front view Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Separator Temp Stabilizer 1 L L S W P C 2 3 4 5 6 To AS Waste Guard From AS Pump front view Pump inlet On Off Valve Seal Wash Pump To waste Piston Seal Wash Mixer Eluent ...

Page 150: ...pressor Regen Out via the DC rear chase Pump inlet On Off Valve Seal Wash Pump To waste Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Separator Temp Stabilizer 1 L L S W P C 2 3 4 5 6 To AS Waste Guard From AS Mixer Backpressure Device Piston Seal Wash pump not to scale To the degasser Regen In via the EG rear chase CR TC Eluent Out Eluent In Regen Out Regen In Eluent In Eluent Out Rege...

Page 151: ... Out via the DC rear chase A B C D A B C D A B C D A B C D To waste To waste Seal Wash Pump Temp Stabilizer To AS Waste Separator 2 Separator 1 Guard 2 Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Temp Stabilizer Eluent Out Eluent Out Mixer Mixer To AS Waste From AS Guard 1 From AS Backpressure Device Backpressure Device Piston S...

Page 152: ...ut System 1 System 2 To inject valve 1 port P 2 Temp Stabilizer To AS Waste From AS To AS Waste Temp Stabilizer Separator 2 Separator 1 Guard 2 Guard 1 Deionized Water Mixer Mixer Backpressure Device Eluent Piston Seal Wash pump not to scale To the degasser 1 Regen In via the EG rear chase EGC In Out Eluent Out CR TC ELUENT OUT REGEN IN Regen Out Eluent In Regen In Eluent In Eluent Out Regen In Re...

Page 153: ...mp Mixer Mixer EG left side view DC front view To Waste From the suppressor Regen Out via the DC rear chase Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Separator Temp Stabilizer 1 L L S W P C 2 3 4 5 6 To AS Waste Guard Large Loop carrier Pump 1 Pump 2 To AS Waste To inject valve sample port 1 2 3 4 5 6 From AS Backpressure Device Piston Seal Wash pump not to scale To the degasser Reg...

Page 154: ... rear chase 10 2 4 6 8 1 3 5 7 9 From AS To AS Waste Guard Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Separator Injection Valve Connections Key 3 Carrier pump in To waste 2 1 To waste 10 8 Concentrator 7 4 Sample in 9 5 Eluent in 6 To column Pump front view Pump inlet On Off Valve A B C D A B C D To waste To waste Seal Wash Pump Mixer Mixer Pump 1 Pump 2 Backpressure Device Piston Se...

Page 155: ...S Waste From AS Eluent In Regen In Regen Out Eluent Out Cell In Cell Out Separator Guard Deionized Water Regen Reagent Deionized Water Pump front view Pump inlet On Off Valve A B C D A B C D To waste To waste Seal Wash Pump Mixer Pump 1 Pump 2 Mixer To 3 way valve 1 COM Port via the DC rear chase From the suppressor Regen Out via the DC rear chase Backpressure Device Piston Seal Wash pump not to s...

Page 156: ...Seal Wash Pump To waste Temp Stabilizer 1 L L S W P C 2 3 4 5 6 To AS Waste From the degasser Eluent Out From AS Mixer Backpressure Device Piston Seal Wash pump not to scale To the CR TC Regen In via the EG rear chase CR TC Eluent Out Eluent In Regen Out Regen In Eluent In Eluent Out EGC In Out A B C D A B C D Deionized Water Regen In Regen Out CarboPac PA20 Amino Trap or PA20 Guard To the VP From...

Page 157: ...n the Thermo Scientific Reference Library DVD P N 053891 4 1 Operating Precautions 4 1 1 EG Operating Precautions In an analytical IC system the EGC requires at least 14 MPa 2000 psi of 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 pr...

Page 158: ...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 NE FERMEZ PAS LE CONTENEUR DE GAZ RÉSIDUEL Le Dionex ICS 5000 Eluent Generator EG le Atlas Electrolytic Suppressor et le Self Regenerating Suppressor SRS travaillent avec un proces d électrolyse qui produit des petites quantités de gaz d oxygène ou d hydrogène Afin ...

Page 159: ... in use The gold spring loaded pogo contact must also remain clean and dry If a salt bridge forms it can cause an electrical short between the working electrode contact and the cell body If the conventional nondisposable working electrode becomes discolored or if you notice a degradation in performance baseline noise tailing peaks etc polish the electrode as instructed in Section 9 28 4 Over the l...

Page 160: ...te the pH value displayed on the Chromeleon panel see Figure 4 1 3 Thereafter monitor the pH value to determine whether there is a shift in the pH A shift in the pH reading for the same eluent composition indicates a change in the Ag AgCl reference potential If the pH value shifts by 0 5 pH unit from the value first observed check the pH Ag AgCl reference electrode see Section 8 28 6 Figure 4 1 Mo...

Page 161: ...r pH limits in the Chromeleon 7 Instrument Method Wizard see Figure 4 2 or Chromeleon 6 8 Program Wizard The Audit Trail displays an alarm if the limits are exceeded NOTE To disable the alarm set the upper limit to 14 and the lower limit to 0 Figure 4 2 Setting pH Limits in Chromeleon 7 ...

Page 162: ... the piston seal wash system see page 154 Start the pump see page 157 Set the pressure limits see page 158 If an EG is installed start the EG and set the eluent concentration see page 161 Start the DC see page 165 or TC see page 169 Equilibrate the system and verify operational readiness DC see page 166 TC see page 170 NOTE You can use the Smart Startup feature in Chromeleon to auto mate system st...

Page 163: ...rations to change over time Refrigerating the samples at 4 C 39 F will reduce but not eliminate bacterial growth Analyze samples containing nitrite or sulfite as soon as possible Nitrite oxidizes to nitrate and sulfite to sulfate thus increasing the measured concentrations of these ions in the sample In general samples that do not contain nitrite or sulfite can be refrigerated for at least one wee...

Page 164: ...r example many water samples concentrations are so low that dilution is not necessary To dilute the sample use eluent or ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 When using carbonate eluents diluting with eluent minimizes the effect of the water dip at the beginning of the chromatogram If you dilute the sample with eluent also use el...

Page 165: ...s to gold to indicate that the Instrument Controller Service is starting When the Instrument Controller Service is running idle the icon changes to gray If the Chromeleon Tray Icon is not on the taskbar click Start All Programs Chromeleon 7 Services Manager to open the Services Manager and click Start Instrument Controller 4 4 2 Starting the Chromeleon 7 Client 1 To start the Chromeleon 7 client c...

Page 166: ...Chromeleon 6 8 Server right click the Chromeleon Server Monitor icon which is crossed out in red on the Windows taskbar and click Start Server The icon changes to gold to indicate that the Chromeleon Server is starting When the Chromeleon Server is running idle the icon changes to gray If the Server Monitor icon is not on the Windows taskbar click Start All Programs Chromeleon Server Monitor to op...

Page 167: ... tabset click View Default Panel Tabset or click the 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 number of device functions can be controlled directly from this panel You can also access the Audit Trail from here Figure 4 4 Example Chromeleon 6 8 Panel Tabset ...

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Page 169: ...s 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 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 en...

Page 170: ...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 Thermo Fisher Scientific the seal wash system is connected to pump 1 the bottom pump If you want to connect the seal wash system to pump 2 the top pump follow the instructions in this section NOTE For users who ne...

Page 171: ...eads on pump 1 see Figure 4 5 item Connect this tubing to the pump heads on pump 2 3 Disconnect the seal wash reservoir inlet line from the primary pump head on pump 1 see Figure 4 5 item Connect the inlet line to the primary pump head on pump 2 4 When you finish these connections go to the next section to continue setting up the seal wash system Figure 4 5 Piston Seal Wash Connections to Pump 1 1...

Page 172: ...g 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 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 Commands dialog ...

Page 173: ...eeding The eluent has been changed The eluent line is new empty The eluent line contains air 3 On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab to display the Pump panel see Figure 4 7 4 Enter the Flow rate required for your application This starts the pump flow also Figure 4 7 Setting the Pump Flow Rate and Pressure Limits Chromeleon 7 Version Shown Enter a new...

Page 174: ...illary and analytical pumps Pump Configuration Default Low Pressure Limit Default High Pressure Limit Capillary pump not linked to an EGC 0 41 MPa 6000 psi a a Capillary IC pumps shipped before February 17 2011 were rated for lower operating pressures than the pumps currently being shipped Refer to the im portant note on the next page for details Capillary pump linked to an EGC 1 4 MPa 200 psi 35 ...

Page 175: ... is stamped on the secondary pump heads of the newer higher pressure rated capillary IC pumps A Capillary Pump High Pressure Upgrade Kit P N 075994 is available for converting a lower pressure rated capillary IC pump to a higher pressure rated pump IMPORTANT If your system includes a capillary pump linked to an EGC check the label on the EG degas capillary cartridge in the IC Cube and verify that ...

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Page 177: ...p in selecting an eluent concentration see Section 4 10 If the pump flow is on entering a new Target Concentration value automatically turns on the power to the EGC also 4 If the pump flow is off first turn on the flow and then click the switch under EG1 Control or EG2 Control This turns on the power to the EGC at the selected Target Concentration value 5 If the CR TC switch is off click the switc...

Page 178: ...y DVD P N 053891 EGC Eluent Concentration Range KOH Capillary 0 1 to 200 mM at 0 001 to 0 010 mL min flow 0 1 to X mM at 0 010 to 0 030 mL min where X 2 flow MSA Capillary 0 1 to 200 mM at 0 001 to 0 010 mL min flow 0 1 to X mM at 0 010 to 0 030 mL min where X 2 flow K2CO3 0 1 to 15 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 2 0 mL min flow where X 15 flow KOH 0 1 to 100 mM at 0 1 to 1 0 m...

Page 179: ...t exceed the specified range The EPM concentration must not exceed 10 mM See the notes below for additional information KOH KOH KOH MSA KOH NaOH MSA MSA MSA NaOH NaOH NaOH 0 1 to 50 mM at 0 1 to 1 0 mL min flow 0 1 to X mM at 1 0 to 3 0 mL min flow where X 50 flow The eluent concentration range for each cartridge is 50 of the range for an independent cartridge LiOH LiOH 0 1 to 40 mM at 0 1 to 1 0 ...

Page 180: ...et Concentration to the concentration of KHCO3 required The K2CO3 cartridge generates the total of the two target concentrations and the EPM modifies the total to achieve the K2CO3 KHCO3 eluent mixture that you require For example For a 3 50 mM K2CO3 1 00 mM KHCO3 eluent set EGC_1 to 3 50 mM and EGC_2 to 1 00 mM The K2CO3 cartridge generates 4 50 mM K2CO3 indicated in the Applied Concentration fie...

Page 181: ...the DC panel see Figure 4 9 3 For each of the following temperature control devices installed in the DC Compartment Column Reaction Coil IC Cube enter the preferred Set temperature This turns on the device also If the preferred temperature is already selected but the device is off click the corresponding switch to turn on the device ICS 5000 DC Figure 4 9 DC Control Panel Chromeleon 7 Version Show...

Page 182: ...anel Set or Chromeleon 6 8 panel tabset verify that each device listed below if installed in your system is turned on and the selected setting for the device flow rate eluent concentration temperature and so on is correct for your application Pump EGC CR TC EPM Suppressor Temperature control devices DC compartment DC column compartment IC Cube CD cell heater reaction coil heater 2 Click Monitor Ba...

Page 183: ... baseline is drifting or is excessively noisy there are large fluctuations in readings 6 Monitor the DP SP pressure and make sure it is at the expected reading for the installed column and it is stable 7 Verify that all installed temperature control devices are at their set points and are stable The system is now ready for operation Because capillary IC systems use low flow rates and consume very ...

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Page 185: ...omeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the TC tab to display the TC panel see Figure 4 10 3 Click the Oven switch Chromeleon 7 or the Oven on button Chromeleon 6 8 to turn on the oven 4 Set the temperature required for the application ICS 5000 TC Figure 4 10 TC Panel Chromeleon 7 Version Shown ...

Page 186: ...libration 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 make sure it is at the expected reading for the installed column and is stable 3 Verify that the detector baseline is at the expected reading for your application and is stable The system is n...

Page 187: ...meleon 7 connects to the instrument and displays the ePanel Set To display the Chromeleon 6 8 panel tabset 1 Click View Default Panel Tabset or click the toolbar button 2 Select the Chromeleon server and click OK 3 If more than one timebase is configured on the server Chromeleon 6 8 displays a panel tabset for each timebase Click the Expand Timebase View button for the timebase that you want to co...

Page 188: ...lled an instrument method in Chromeleon 7 or a program in Chromeleon 6 8 The chromatographic data acquired for each injection Figure 5 1 Sample Analysis Overview 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 Templates for displaying chromatographic data on the screen and for printing reports...

Page 189: ...ur laboratory eWorkflows are the preferred method for creating a new sequence If eWorkflows are not available use the Sequence Wizard Using eWorkflows 1 On the Console click the eWorkflows category bar see Figure 5 2 In the Navigation Pane click the eWorkflow name 2 In the work area click the instrument name and then click Launch 3 The eWorkflow Wizard opens Complete the steps in the wizard For de...

Page 190: ... 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 3 After you finish the wizard the new sequence is displayed in the Console Data view see Figure 5 3 5 2 2 Creating a New Sequence in Chromeleon 6 8 In Chromeleon 6 8 two wizards are available to help you crea...

Page 191: ...program and quantitation method to use For help at any time click the Help button on the Sequence Wizard page NOTE If preferred you can create the sequence first and then specify the program and quantitation method later You can also edit other details of the sequence for example add or remove samples after you finish the wizard 3 After you finish the Sequence Wizard the new sequence is displayed ...

Page 192: ...he in a new sequence via Sequence Wizard option 4 Click Next to go to the Sequence Wizard 5 Complete the steps in the Sequence Wizard specifying the number of samples and standards that you want For help at any time click the Help button on the Sequence Wizard page After you finish the Sequence Wizard a sequence is created and displayed in the Chromeleon 6 8 Browser A program and quantification me...

Page 193: ...ly running another sequence the sequence is started 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 Figure 5 6 Running Sequence in Chromeleon 7 Figure 5 7 Starting a Sequence in Chromeleon 6 8 ...

Page 194: ...rmo Scientific Reference Library DVD P N 053891 3 Create a sequence in Chromeleon that specifies the vials from which to take sample injections and the order in which the injections should be run 4 Specify a Chromeleon 7 instrument method or Chromeleon 6 8 program that includes the appropriate load and inject commands for the autosampler See the examples in Section 5 4 5 3 2 Loading Samples with a...

Page 195: ...injection valve to the Inject position 5 3 3 Loading Samples with a Vacuum Syringe Pull Method 1 Verify that a luer adapter fitting is installed on the sample loading port on the front of the DC and that tubing is connecting the sample loading port and the injection valve If this is not the case refer to Section 9 20 for connection instructions 2 Disconnect the waste line from the injection valve ...

Page 196: ...e performed are added automatically An Inject command to switch the injection valve to the Inject position is always included The Inject command occurs at time 0 00 This is when the sample enters the high pressure side of the system and defines the beginning of a chromatogram Wait commands to pause the instrument method or program while the autosampler is performing the injection are also included...

Page 197: ...utosampler Figure 5 10 shows the basic Chromeleon commands for controlling sample injection with a Dionex AS DV Autosampler Figure 5 9 Commands for Loading and Injecting a Sample with a Dionex AS AP Chromeleon 7 Script Editor Shown Figure 5 10 Commands for Loading and Injecting Sample with a Dionex AS DV Chromeleon 7 Script Editor Shown ...

Page 198: ...le injection with a Dionex AS Autosampler 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 Figure 5 11 Commands for Loading and Injecting a Sample with a Dionex AS Chromeleon 7 Script Editor Shown ...

Page 199: ...oir with wash solution see Section 2 2 5 Rinse out buffers This will reduce the time required for column equilibration when you resume operation 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 Before shipping the pump Empty the seal wash reservoir Disconnect the tubing from the peristal...

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Page 201: ...leon 6 8 panel tabset For EG startup information see Section 4 9 2 In an analytical IC system if the EG has been shut down for more than 3 to 4 days hydrate the suppressor as instructed in the product manual Suppressor manuals are included on the 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 mo...

Page 202: ...page 343 or Conditioning the Analytical EGC on page 348 3 Hydrate the CR TC see Installing and Flushing the New CR TC on page 350 4 Hydrate the suppressor as instructed in the product manual Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 5 Let the system equilibrate before collecting data Before shipping the EG 1 Follow the instructions in Section 9 14 1 ...

Page 203: ...luent 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 KCl and 1 M HCl 6 4 2 Long term Storage of the pH Ag AgCl Reference Electrode If the cell will not be used for 2 days or more remove the pH Ag AgCl reference electrode and store it in a solution of saturated KCl ...

Page 204: ...ionex ICS 5000 Operator s Manual 188 Doc 065342 06 12 11 5 Make sure there is no air bubble in the cap Add more KCl solution if needed Figure 6 2 pH Ag AgCl Reference Electrode in Storage Cap Storage Cap ...

Page 205: ...manuals for the individual products for instructions These manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 6 6 Short term Shutdown Before a TC shutdown of less than one week no special procedure is required 6 7 Long term Shutdown Before interrupting TC operation for more than one week or before shipping the TC rinse the fluid connections with deionized water ICS 5000...

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Page 207: ...cientific Reference Library DVD P N 053891 7 1 System Maintenance Checklists 7 1 1 Daily Maintenance Check for leaks Wipe up liquid spills Check eluent reservoirs for microbial growth clean reservoirs and replace eluent as needed Check eluent reservoir levels and refill as needed Check waste containers and empty as needed For detailed daily maintenance instructions for each module see 7 1 2 Weekly...

Page 208: ... Thermo Fisher Scientific perform the performance qualification PQ procedure for IC systems For detailed periodic maintenance instructions for each module see NOTE There are no periodic maintenance instructions for the EG 7 1 4 Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance on each module annually Preventive Maintenance Kits contain all the required parts ...

Page 209: ...9 DC TC Preventive Maintenance Kits 0 4 L Internal Loop High Pressure Valve Preventive Maintenance Kit P N 075040 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 10 Port High Pressure Valve Preventive Maintenance Kit P N 075042 NOTE There is no Preventive Maintenance Kit for the EG ...

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Page 211: ...emain 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...

Page 212: ...tions Check the tubing connected to the peristaltic pump If the tubing is blocked or crimped replace it see Section 9 9 Check the liquid level in each eluent reservoir and refill as required 7 4 DP SP Periodic Maintenance Make fresh eluent as needed Replace piston seals every 6 to 12 months see Section 9 7 Clean eluent reservoirs every 3 months with methanol or isopropyl alcohol as instructed in S...

Page 213: ... water Rinse the EG drip tray with deionized water to prevent formation of salt crystals and dry the drip tray thoroughly Rinse and dry the leak sensor also if the sensor is not dry it will remain activated and continue to report a leak to the Audit Trail Check the waste container and empty as needed 7 7 EG Weekly Maintenance Check all lines for crimping Move or reroute pinched lines and replace d...

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Page 215: ... empty as needed NOTE If you are using an electrochemical detector also see the spe cial maintenance considerations that are described in Section 4 1 2 7 10 DC Weekly Maintenance Check liquid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines Check for excess condensation inside the DC Condensation may build up when the DC is operated in a highly humid environment...

Page 216: ...entific recommends performing preventive maintenance annually The following kits are available 0 4 L Internal Loop High Pressure Valve Preventive Maintenance Kit P N 075040 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 10 Port High Pressure Valve Preventive Maintenance Kit P N 075042 ...

Page 217: ...aste container and empty as needed 7 14 TC Weekly Maintenance Check liquid lines for crimping or discoloration Relocate any pinched lines Replace damaged lines 7 15 TC Periodic Maintenance 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 ICS 5000 TC ...

Page 218: ...of damage A defective seal impairs the performance of the instrument If the seal is defective contact Technical Support for Dionex products 7 16 TC Annual Maintenance Thermo Fisher Scientific recommends performing preventive maintenance annually The following kits are available 6 Port High Pressure Valve Preventive Maintenance Kit P N 075041 10 Port High Pressure Valve Preventive Maintenance Kit P...

Page 219: ... personnel 8 1 Audit Trail Error Messages The instrument control firmware installed in each Dionex ICS 5000 module periodically checks the status of certain parameters If a problem is 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 ...

Page 220: ...ge 228 Degasser malfunction Warning page 228 Excessive drive current Camshaft x x Abort page 229 Invalid flow value Abort page 229 Leak detected Flow stopped Abort page 229 Left hand pump block carryover pressure is too high Abort page 230 Motor malfunction Abort page 230 Motor position error The motor is overloaded Abort page 230 Pressure fallen below lower limit Abort page 231 Relay 4 is configu...

Page 221: ...lt Severity Level See Concentration out of range The maximum value at time 1 is 2 Error page 241 Concentration out of range The maximum value is 1 Error page 241 CR TC1 open circuit CR TC2 open circuit Abort page 241 CR TC1 over current CR TC2 over current Abort page 242 CR TC1 stopped because EGC1 OFF CR TC2 stopped because EGC2 OFF Abort page 242 CR TC1 stopped due to zero flow CR TC2 stopped du...

Page 222: ...e concentration Abort page 246 EG1 invalid ion count EG2 invalid ion count Abort page 246 EG1 invalid serial number EG2 invalid serial number Abort page 247 EG1 over current EG2 over current Abort page 247 EG1 over power EG2 over power Abort page 248 EG1 over voltage EG2 over voltage Abort page 248 EG1 wrong cartridge error EG2 wrong cartridge error Abort page 249 The EG mode is off due to pump pr...

Page 223: ...llary EGC Abort page 251 EGC is either not installed or invalid cartridge number Please install an analytical EGC Abort page 251 EGC is either not installed or invalid cartridge number Please install an EGC Abort page 252 Leak sensor wet Warning page 252 pH modifier must be used with a different type of cartridge Error page 252 Pump is disconnected The EG mode is off Warning page 253 EG Related Au...

Page 224: ...arning page 264 High pressure valve 1 error High pressure valve 2 error High pressure valve 3 error High pressure valve 4 error Abort page 265 IC Cube 1 heater over safe temperature IC Cube 2 heater over safe temperature Error page 266 Lower door opened Warning page 267 Lower leak sensor wet Warning page 267 Reaction coil open circuit Abort page 267 Reaction coil over safe temperature Abort page 2...

Page 225: ...rty TempCtrl Error page 275 All samples scheduled for run on timebases x need to specify the same value for property y Error page 276 Can t execute Disconnect command during data acquisition Warning page 276 Can t execute Standby command during data acquisition Warning page 276 Can t find download image TC3000 HEX Abort page 276 Can t start acquisition at negative retention times Error page 277 Ca...

Page 226: ...imits defined for the column Warning page 280 Current pressure is out of limits defined for the column Warning page 281 Current temperature is out of limits defined for the column Warning page 281 Data buffer overrun Abort page 281 Device control feature is not available Please check key code and CM Features see About Chromeleon in the client s Help menu Abort page 282 Device is not remote Abort p...

Page 227: ...e 286 Next qualification of this module is due in x day s due date is date Warning page 286 Next qualification of this module is overdue due date was date Warning page 287 Next qualification of this module is overdue due date was date Module may no longer be used Error page 287 Next qualification of this module was due on date Allowing x more grace day s Warning page 287 Next service of this modul...

Page 228: ...reader Error page 291 Raw data file x cannot be created Warning page 291 Raw data file x cannot be created Continuing with network failure protection Warning page 291 Raw data file x cannot be written Warning page 291 Raw data file x cannot be written Continuing with network failure protection Warning page 291 Starting data acquisition manually will overwrite any data which has been acquired so fa...

Page 229: ...s of Standby Ready Door and CardState Error page 294 The primary column ID property x will be changed The property can t be changed in the future Warning page 295 The upper limit must be higher than the lower limit Error page 295 The Warning threshold must be higher than the Limit threshold Error page 296 The Warning threshold must be lower than the Limit threshold Error page 296 There was already...

Page 230: ...new stock solution Two AcqOn commands for the same channel The second chromatogram will overwrite the first Error page 296 Unknown error code Warning page 297 Unknown format of the card data Error page 297 USB LAN communication error Please check communication cable and instrument s power Abort page 283 Value for name parameter is not within valid range Value passed x will be substituted by y Warn...

Page 231: ...ystem backpressure is below 14 MPa 2000 psi The optimal system backpressure is 16 MPa 2300 psi in an analytical IC system with an EG installed Low system backpressure may cause high baseline noise as the eluent concentration increases in the gradient To correct this install a backpressure coil in the EG after the RFIC Eluent Degasser see Section 9 17 Flow system leak ahead of cell Check all fittin...

Page 232: ...ressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Temperature compensation setting not optimized Optimize the selected setting see Section 2 14 Trapped gases in cell Release any trapped gases in the cell by loosening the lines to and from the cell and then retightening them Also loosen and retighten the fittings to and from the suppressor eluent ports Inadequate...

Page 233: ... electrode P N 061879 DC Amperometry and Integrated Amperometry modes Regular baseline oscillation on high sensitivity ranges Reconnect the short length of titanium tubing to the cell inlet see Figure 2 30 DC Amperometry and Integrated Amperometry modes Dirty or pitted conventional nondisposable working electrode Polish the working electrode see Section 9 28 4 If you are using a disposable electro...

Page 234: ...ston seals Replace the piston seal on any head with a leak see Section 9 7 2 Check for leaks throughout the remainder of the system including the check valves injection valve and columns Tighten or replace fittings as needed DP SP not primed Prime the pump see Section 9 5 Liquid lines incompletely flushed after an eluent change Attach a 10 cc syringe P N 054578 to the waste port on the priming val...

Page 235: ...tions listed in Section 1 5 3 Replace all end line filters P N 045987 See Section 4 6 for instructions 4 Prepare new stock solution 5 Prepare fresh eluent To ensure eluent purity prepare all eluents with electrochemical grade chemicals and ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 Problem unrelated to the pump 1 The eluent concentrati...

Page 236: ... Support for Dionex products for assistance 8 5 Peak Retention Times Are Too Late Eluent concentration setting is too low The correct eluent concentration setting depends on several factors the flow rate EGC type etc Refer to Section 4 9 for a list of valid concentration ranges for the cartridges and then edit the program as required DP SP flow rate is too high Decrease the DP SP flow rate Inopera...

Page 237: ...nics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the detector to make certain the connector is securely connected see Figure 8 1 ED Verify that the signal cables from the cell are connected to the detector block In addition an electronics connector on the back of the detector plugs into a receptacle on the detector compartment Push on the detec...

Page 238: ...lectrode Clean the working electrode with water and dry with pressurized air or nitrogen Polish the working electrode see Section 9 28 4 If you are using a disposable electrode replace it Capillary tubing fittings incorrectly installed Incorrectly installed fittings on capillary tubing can increase void volumes causing chromatograms with tailing peaks see Figure 8 2 To correctly install fittings o...

Page 239: ...ee 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 Restriction in the system plumbing 1 Begin pumping eluent through the system including the columns at the flow rate normally used 2 Work backward through the system beginning at the flow cell exit One at a time loosen...

Page 240: ...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 3 Check the value of the reference potential shift see Using a Digital Voltmeter to Determine Reference Potential Shift on page 274 If the value fluctuates by more...

Page 241: ...ot suppressed by suppressor Verify that the suppressor is turned on and the current is set to the correct value Refer to the suppressor manual for additional troubleshooting guidance Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 Regenerant fails to suppress background Use a higher regenerant flow rate Refer to the suppressor manual for the suggested rege...

Page 242: ... or nitrogen Remove any precipitate on the counter electrode by cleaning the spot directly opposite the working electrode with a lint free tissue DC Amperometry and Integrated Amperometry modes Leak between gasket and electrode or between gasket and cell body Remove any precipitate with water and a lint free tissue and then install a new gasket see Section 9 28 3 Turn the yoke knob see Figure 9 53...

Page 243: ...ent 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 r...

Page 244: ...chanism To troubleshoot Turn off the DP SP power for 30 seconds and then turn it on again If the error message appears again contact Technical Support for Dionex products for assistance Degasser malfunction The vacuum degassing module monitors the vacuum system continuously If a problem is detected this error occurs To troubleshoot 1 Check all tubing connections to the vacuum degassing module for ...

Page 245: ... needed see Section 9 3 Be careful not to overtighten fittings Invalid flow value This error occurs if you enter an invalid value for the DP SP flow rate in Chromeleon To troubleshoot Select a flow rate within the DP SP flow rate range For the flow rate range for each type of DP SP refer to Section 1 5 Leak detected This error occurs if the DP SP leak sensor detects a liquid leak inside the enclos...

Page 246: ...s 2 Inspect the outlet check valve for blockage Replace the check valve cartridge if needed see Section 9 6 Motor malfunction This error occurs if an internal error in the pump drive mechanism occurs To troubleshoot Turn off the DP SP power for 30 seconds and then turn on the power again If the error message appears again contact Technical Support for Dionex products for assistance Motor position ...

Page 247: ...end line filter P N 045987 See Section 4 6 for instructions Verify that the end of each filter extends to the bottom of the reservoir and is submerged in eluent Prime the pump see Section 9 5 3 Eluents may be insufficiently degassed Check the vacuum degassing module 4 Check all tubing connections for leaks tighten loose fitting connections Be careful not to overtighten fittings 5 Make sure the pri...

Page 248: ...pler sample injection To troubleshoot Define the relay as a standard relay or specify a different relay for use in the program The maximum purge pressure was exceeded If the DP SP pressure exceeds 5 MPa 725 psi during priming this error occurs and the priming process is aborted To troubleshoot 1 Verify that the priming valve is open To open the valve turn the knob one half turn counterclockwise 2 ...

Page 249: ...OWER button on the front of the DP SP to turn on the pump c On the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset set the Flow rate to 0 01 mL min for a capillary IC system or 1 0 mL min for an analytical IC system and record the backpressure d Disconnect all components after the injection valve e One at a time reconnect each component of the flow path If reconnecting a component causes an...

Page 250: ...program is exceeded The running batch is aborted default and this message appears To troubleshoot 1 Inspect the tubing for blockage or crimping replace as needed see Section 9 3 Be careful not to overtighten fittings 2 To determine the source of the high backpressure isolate segments of the flow path a Remove the pump outlet tubing at the injection valve b Press the POWER button on the front of th...

Page 251: ...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 Chr...

Page 252: ...strument method the Chromeleon 6 8 program or other remote signal source If you do not want the pump to stop take the appropriate preventive action edit the instrument method the program or the settings of the other remote signal source Low pressure limit was tripped Refer to the troubleshooting steps for the Audit Trail message Pressure fallen below lower limit on page 231 High pressure limit was...

Page 253: ... 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 If the check valve continues to leak tighten it an...

Page 254: ... the normal operating backpressure for the currently configured system including the column tubing may be plugged or overtightened Refer to the troubleshooting steps for the Audit Trail message The system pressure exceeded the safety limit on page 233 8 16 Vacuum Degassing Module Low Vacuum Leak in the vacuum degassing module Check all tubing connections for leakage tighten loose fitting connectio...

Page 255: ...rify that the correct signal type is selected 2 A programming error occurred in the device sending the signal Refer to the user s manual for the device for troubleshooting assistance TTL Relay output related error 1 A programming error occurred in the device sending the signal Refer to the user s manual for the device for troubleshooting assistance 2 The device being triggered may require a TTL no...

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Page 257: ...ated 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 C...

Page 258: ... to Section 8 23 to determine why liquid flow stopped 3 If the error message appears again contact Technical Support for Dionex products for assistance The CR TC control electronics may have malfunctioned NOTE The Thermo Scientific Dionex ICS 5000 Ion Chromatogra phy System electronics components cannot be serviced by the user CR TC1 stopped because EGC1 OFF or CR TC2 stopped because EGC1 OFF This...

Page 259: ... pump and you try to turn on the CR TC The mode is automatically turned off to ensure that the EG does not operate when there is no flow CR TC mode will be turned off for invalid flow Flow range for analytical EGC 0 100 3 000 mL min capillary EGC 0 001 0 100 mL min This error occurs when the flow to the CR TC is out of range or there is no pumped linked to the EGC To troubleshoot 1 Set the flow ra...

Page 260: ...heck the EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the correct pump is linked to the EGC EG1 cartridge disconnected or EG2 cartridge disconnected This error occurs if Chromeleon sends a command to set an EG parameter when the EGC is disconnected To troubleshoot 1 Make sure the EGC cable is secure...

Page 261: ...ed 2 If the 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 assista...

Page 262: ...o troubleshoot Set the flow rate to a value within the allowed range The allowable eluent concentration for a particular application depends on several factors the flow rate suppressor type EGC type and cartridge configuration For details refer to Section 4 9 EG1 invalid ion count or EG2 invalid ion count This error occurs if the ion count reported by the EGC is invalid This may indicate a problem...

Page 263: ...or occurs when the current applied to the EGC exceeds the maximum current allowed The EGC current is automatically turned off to prevent damage to the cartridge This error may also occur if the liquid flow to the cartridge is interrupted To troubleshoot 1 Make sure the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened 2 Refer to Section 8 23 to determine w...

Page 264: ... applied to the EGC exceeds the maximum current allowed The EGC current is automatically turned off to prevent damage to the cartridge This error may also occur if the liquid flow to the cartridge is interrupted To troubleshoot 1 Refer to Section 8 23 to determine why there is no flow 2 If the error message appears again contact Technical Support for Dionex products for assistance The EGC control ...

Page 265: ...atically turned off to prevent damage to the EG To troubleshoot Check the troubleshooting information for the pump in Section 8 14 and Section 8 15 The EG mode is off for a virtual pump This error occurs when a live EG is linked to a virtual pump and you try to turn on the EGC To prevent damage to the EGC the mode is automatically turned off to ensure that the EG does not operate when there is no ...

Page 266: ... EGC configuration properties in the Chromeleon 7 Instrument Controller Service or the Chromeleon 6 8 Server Configuration program to verify that the pump and EGC are linked EGC 1 is not linked to a compatible pump or EGC 2 is not linked to a compatible pump This error occurs if the type of pump linked to the EGC does not match the EGC type A capillary EGC can only be used with a capillary pump an...

Page 267: ...ease install a capillary EGC This error occurs if no EGC cartridge is connected to the EG or an analytical EGC is connected to a capillary IC system To troubleshoot 1 Verify that a capillary EGC is installed 2 Verify that the EGC cable is securely plugged into the EG see Figure 2 10 and the locking ring is tightened EGC is either not installed or invalid cartridge number Please install an analytic...

Page 268: ...tray in the bottom of the EG To troubleshoot 1 Locate the source of the leak by visually inspecting the tubing fittings and components in the EG 2 Tighten fittings or replace tubing and fittings as required see Section 9 12 Refer to Section 8 22 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray and leak sensor thoroughly to prevent the leak sensor fro...

Page 269: ...2 Blocked or improperly installed waste line Check the EG waste lines to be sure they are not crimped or otherwise blocked Make sure the lines are not elevated at any point after they exit the EG EGC leaks Replace the EGC see Section 9 14 RFIC Eluent Degasser leaks Replace the RFIC Eluent Degasser see Section 9 16 EGC electrical connection is open 1 Tug gently on the EGC electrical cable the locki...

Page 270: ...wer 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 Leaking fitting Locate the source of the leak Tighten or replace liquid line connections as needed see Section 9 12 Blocked or improperly installed waste lin...

Page 271: ...he Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset is between the high and low limits displayed on the panel For details see Section 4 8 NOTE The analytical EGC requires at least 14 MPa 2000 psi of backpressure for optimal removal of electrolysis gas from the eluent produced by the car tridge A system backpressure of 16 MPa 2300 psi is ideal Analytical IC only RFIC Eluent Degasser tubin...

Page 272: ...sure for optimal removal of electrolysis gas from the eluent produced by the cartridge A system backpressure of 16 MPa 2300 psi is ideal DP SP flow rate is too low or too high For a capillary IC system select a flow rate between 0 001 and 0 100 mL min For an analytical IC system select a flow rate between 0 100 and 3 000 mL min Electrical error detected ALARM LED is lighted To prevent damage to th...

Page 273: ... the power source Check that the wall outlet has power 4 Check the USB connections The EG should be connected to the DP SP or other Dionex ICS 5000 module via a USB cable P N 960777 In addition one module in the system must be connected to the PC on which Chromeleon is installed 5 Check that the EG is configured in Chromeleon and is assigned to an instrument Chromeleon 7 or timebase Chromeleon 6 8...

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Page 275: ...receptacle on the detector compartment Push on the upper part of the detector see Figure 8 3 to make certain the connector is securely connected 2 If the error persists there may be a problem in the detector electronics Contact Technical Support for Dionex products for assistance NOTE The Thermo Scientific Dionex ICS 5000 Ion Chroma tography System electronics components cannot be serviced by the ...

Page 276: ...han the CD cell setpoint 3 Check the suppressor current setting Running the suppressor at a higher current than is recommended for the application can cause heat up of the CD cell Column temperature open circuit This error may indicate a problem in the detector electronics Contact Technical Support for Dionex products for assistance Column over safe temperature This error occurs when the temperatu...

Page 277: ...mum allowed This error may occur if the Thermo Scientific Dionex ICS 5000 Ion Chromatography System is operating in an environment in which the temperature is greater than 40 C 104 F To troubleshoot Refer to Appendix A for environmental specifications Compartment temperature calibration error To troubleshoot Repeat the calibration procedure following the instructions provided in the DC Temperature...

Page 278: ...correct electrode material waveform potentials and reference mode are selected for the application being run 5 Restart the flow and select DC amperometry mode Apply cell potential in steps increasing toward the detection potential the potential of the integration period in integrated amperometric detection If the current becomes excessive again try a new working electrode or another cell if availa...

Page 279: ...orking electrode is disconnected from the cell electronics To troubleshoot Check the cable connection Verify that the signal cable from the working electrode is connected to the detector block see Figure 8 4 ED pH offset calibration failed This error occurs when the pH reading differs by more than 1 0 pH unit from 7 0 which is the value specified for offset calibration This can be caused by too la...

Page 280: ...ffected causing the calibration slope to deviate by more than 10 from the theoretical slope of 59 mV pH unit at 25 C To troubleshoot 1 Make sure the calibration temperature is as close as possible to 25 C 2 Verify that the correct buffer is being used and that the electrode is properly immersed in the calibration buffer 3 Repeat the calibration procedure see Section 9 28 6 If the error recurs repe...

Page 281: ...gh pressure valves 1 and 2 are the valves installed in the DC lower compartment see Figure 8 5 High pressure valves 3 and 4 are the valves installed on either the IC Cubes or the AM in the upper compartment see Figure 8 6 Figure 8 5 High Pressure Valves 1 and 2 In DC Lower Compartment Figure 8 6 High Pressure Valves 3 and 4 On IC Cubes High Pressure Valve 1 High Pressure Valve 2 not installed in t...

Page 282: ... pressing the Load and Inject buttons on the front of the DC 4 If the problem persists contact Technical Support for Dionex products for assistance IC Cube 1 heater over safe temperature or IC Cube 2 heater over safe temperature This error occurs when the temperature of the IC Cube heater exceeds the maximum allowed This error may occur if the Thermo Scientific Dionex ICS 5000 Ion Chromatography S...

Page 283: ...ay the sensor signals the problem and this error message appears To troubleshoot 1 Locate the source of the leak by visually inspecting the tubing fittings and components 2 Tighten fittings or replace tubing and fittings as required Refer to Section 8 26 for detailed troubleshooting of various types of leaks 3 After fixing the leak dry the drip tray thoroughly to prevent the leak sensor from trigg...

Page 284: ...tronics To troubleshoot 1 Follow the instructions in the suppressor manual to regenerate the suppressor Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 2 Follow the instructions in the suppressor manual to clean the suppressor 3 If you suspect a malfunction in the suppressor controller contact Technical Support for Dionex products for assistance NOTE The T...

Page 285: ...ection 2 If the error persists replace the suppressor see Section 9 27 2 Suppressor stopped for flow rate This message occurs if the pump flow stops while the suppressor is on The suppressor is automatically turned off to prevent damage to the suppressor To troubleshoot If the pump stopped unexpectedly see Section 8 14 for pump troubleshooting information Upper door opened This message occurs when...

Page 286: ... 1 Make sure the liquid line connections to the transducer are tight Replace any damaged fittings see Section 9 19 2 If the leak is from behind the valve stator the rotor seal may be scratched Rebuild the injection valve see Section 9 22 Leaking cell 1 Check the waste lines for blockage trapped particles can plug the lines and cause a restriction and or leak If necessary clear the waste lines by r...

Page 287: ...oubleshooting 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 Disconnected pH Ag AgCl reference electrode Verify that the reference electrode cable is securely connected see Figure 8 8 Reference electrode short circuit Replace the reference electrode see Section 9 28 5 pH Ag...

Page 288: ...g out make sure that eluent is being pumped continuously through the cell If the cell will not be used for a short time less than 2 days disconnect the tubing from the inlet and outlet fittings and all fitting plugs For longer shutdowns remove the electrode from the cell and store it in its storage bottle filled with saturated KCl solution See Section 4 1 2 for detailed instructions 8 28 3 Shift i...

Page 289: ... 1 Soak the pH Ag AgCl reference electrode in a solution containing 1 M KCl and 1 M HCl long enough to restore the electrode potential to 30 mV when compared to an unexposed Ag AgCl reference electrode To test the electrode potential see Using a Digital Voltmeter to Determine Reference Potential Shift on page 274 2 If soaking the pH Ag AgCl reference electrode does not fix the problem replace the ...

Page 290: ...gCl reference electrode P N 061879 stored in 3 M KCl can be kept on hand for this purpose Using a Digital Voltmeter to Determine Reference Potential Shift 1 For each pH Ag AgCl reference electrode the unexposed electrode and the electrode being tested use a straightened paper clip or short piece of wire of a suitable diameter to connect the voltmeter s voltage inputs to pin 1 on the reference elec...

Page 291: ...qOn command Enter the AcqOn command after the first injection 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 program All samples scheduled for ru...

Page 292: ...ing data acquisition Selecting the Disconnect or Standby command during data acquisition will stop data transmission and cause data acquisition to stall If you attempt to issue one of these commands during data acquisition this error occurs To troubleshoot Wait until data acquisition is completed before attempting to issue either of these commands Can t find download image TC3000 HEX TC3000 HEX is...

Page 293: ...ts are not met To troubleshoot Contact your local Dionex products representative at Thermo Fisher Scientific to obtain the appropriate software version and license Can t start TC firmware A firmware download may be necessary or Error finishing download or TC Firmware download failed If the TC firmware cannot be started after a firmware download or if Chromeleon is unable to successfully download f...

Page 294: ...nical Support for Dionex products for assistance The firmware cannot be serviced by the user Can t use device x as a source of the column pressure Please check the property SystemPressure for a valid device name The device must have the Pressure property available or 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 P...

Page 295: ...ment Configuration Manager or the Chromeleon 6 8 Server Configuration program 2 In the instrument or timebase right click the TC and select Properties 3 On the General tab page clear the Simulation Mode or Demo Mode check box 4 If the 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 betw...

Page 296: ...M 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 Propertie...

Page 297: ...rrent temperature reading is outside the range specified by the Column_x Temp_UpperLimit and Column_x Temp_ LowerLimit commands To troubleshoot Select a valid temperature setting Data buffer overrun This error occurs in Chromeleon 6 8 if the system cannot write incoming data to disk fast enough To troubleshoot Increase the buffer size 1 Start the Chromeleon 7 Instrument Configuration Manager or th...

Page 298: ...tware options For Chromeleon 6 8 the license features you purchased are listed on the About Chromeleon screen and labeled On If necessary upgrade your software by acquiring the corresponding licenses Contact your local Dionex products representative at Thermo Fisher Scientific for assistance Device is not remote or TC is not remote If you try to issue certain commands for example Column_x and Inje...

Page 299: ...r the current date is later than the expiration date for x or the program or batch will end later than 24 hours before the expiration time for x Chromeleon compares the current date with the column expiration date during injection or before beginning batch processing This error occurs if the expiration date has already passed or if batch processing is scheduled to start less than 24 hours before t...

Page 300: ... refer to Section 9 30 Error programming flash memory This error occurs if during a firmware download the new firmware cannot be programmed into memory To troubleshoot Flash memory cannot be serviced by the user Contact Technical Support for Dionex products for assistance Executing this command will reset associated counter values stored in the module This error occurs when you select a command Ro...

Page 301: ... the leak 2 If you are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation Humidity leak detected This error occurs if the humidity sen...

Page 302: ... use DD MMM YYYY or current Nyear s Nmonth s Nday s Examples 31 Dec 1999 current 1 year 6 months This error occurs if you enter the date associated with an event in an invalid format To troubleshoot Enter the date in the format specified in the message Invalid enumerated value This error occurs if you attempt to enter an invalid value for a property rather than selecting a value from the drop down...

Page 303: ...the warning is first displayed The Qualification GracePeriod property determines for how many days after the due date you can continue using the TC without performing the qualification To troubleshoot Contact Technical Support for Dionex products to schedule an Operational Qualification and Performance Qualification Next service of this module is due in x day s due date is date or Next service of ...

Page 304: ...ager or the Chromeleon 6 8 Server Configuration program right click the TC and select Properties on the context menu 2 Select the Components tab in the Properties dialog box Clear the check mark beside the column name and click OK No response from x for x seconds or No response from x for x seconds Device disconnected This error occurs if there is a communication failure between the TC and the PC ...

Page 305: ...manuals are provided on the Thermo Scientific Reference Library DVD P N 053891 Parameter x value exceeded its allowed range Set to closest valid value x or Value for name parameter is not within valid range Value passed x will be substituted by y or Value x replaced by valid table entry y If you select a value outside the allowable range for certain parameters Chromeleon ignores the setting replac...

Page 306: ...cating BusBlocked This error occurs if you attempt to change column ID properties when at least one column ID chip card is inserted incorrectly To troubleshoot 1 Open the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset 2 Press the F8 key to open the Commands dialog box 3 Under TC select the column name and select the CardState property If the status is BusBlocked remove the card from th...

Page 307: ... troubleshoot Insert a column ID chip card into the appropriate slot see Section 9 30 Raw data file x cannot be created or Raw data file x cannot be created Continuing with network failure protection or Raw data file x cannot be written or Raw data file x cannot be written Continuing with network failure protection If a network failure prevents Chromeleon from creating or writing to a raw data fil...

Page 308: ...id 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 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 ...

Page 309: ...as exceeded its limit y Module should no longer be used Replace the name This error occurs if the number of hours a TC part has been in use exceeds the lifetime set by the OperationTime Limit property To troubleshoot Replace the part identified in the message before resuming operation The data format stored on the chip card is unsupported format version x This error occurs if the column ID chip ca...

Page 310: ...etting is outside the range specified by the Temperature LowerLimit and Temperature UpperLimit commands To troubleshoot Select a valid temperature setting The nominal temperature value is out of range defined by the active column ID This error occurs if the selected TC temperature setting is outside the range specified by the Column_x Temp_LowerLimit and Column_x Temp_ UpperLimit commands To troub...

Page 311: ... property can t be changed in the future This error occurs when you modify a primary column property batch or lot number date of manufacture etc To prevent any unintended changes Chromeleon requests confirmation before saving the new property To troubleshoot If you are sure that the proposed change is correct go ahead and save it The upper limit must be higher than the lower limit This error occur...

Page 312: ...cted for a parameter is higher than the Limit value Chromeleon issues a warning message in the Audit Trail when the Warning value is reached and an error message when the Limit value is reached To troubleshoot Select a Warning value that is lower than the Limit value There was already an AcqOff command for this channel before or There was already an AcqOn command for this channel before or Two Acq...

Page 313: ...r TempCtrl that affects the entire TC this error occurs To troubleshoot To avoid disrupting operation cancel the command Unknown error code This error occurs if Chromeleon does not recognize the error code sent by the TC firmware To troubleshoot The firmware cannot be serviced by the user Contact Technical Support for Dionex products for assistance Unknown format of the card data This error occurs...

Page 314: ...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 If the error occurs again contact Technical Support for Dionex products for assistance You do not have the privilege to approve the module s qualification or You do not have the ...

Page 315: ...anel click the Clear Alarm button 4 Ventilate the interior of the TC thoroughly before closing the door and resuming operation Humidity leak inside the TC 1 Find and eliminate the leak 2 If you are using Chromeleon 7 Open the Commands dialog box press the F8 key Select the TC and click the Commands tab Click the ClearAlarmLED button 3 If you are using Chromeleon 6 8 On the TC Control panel click t...

Page 316: ...ection 9 29 Blocked or improperly installed line Make sure the lines are not crimped or otherwise blocked Also make sure the waste line is not elevated at any point after it exits the TC If a line is blocked replace it see Section 9 29 Leaking injection valve 1 Make sure the liquid line connections to the valve are tight Replace any damaged fittings see Section 9 29 2 Liquid leaks from behind the ...

Page 317: ... 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 8 33 TC Temperature Stabilizer Not Operating Properly Temperature stabilizer installed incorrectly Remove the temperature stabilizer and install it...

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Page 319: ...ore replacing any part refer to the troubleshooting information in Chapter 8 to correctly identify the cause of the problem 9 1 Connecting Capillary Tubing When connecting precision cut 0 062 mm 0 0025 in ID blue PEEK tubing capillary tubing to a port make sure the ferrule and fitting bolt are at least 2 mm 0 1 in from the end of the tubing before you insert the tubing into the port Do not positio...

Page 320: ...st 2 mm 0 1 in from the end of the tubing see Figure 9 1 2 Insert the tubing into the port until it stops 3 While maintaining pressure on the tubing to keep it in place in the port tighten the fitting bolt fingertight 4 If you are installing a high pressure fitting blue bolt and ferrule follow the instructions below to tighten the fitting Figure 9 1 Correct and Incorrect Ferrule and Fitting Bolt P...

Page 321: ...ightening a high pressure fitting bolt P N 074449 and high pressure ferrule P N 074373 1 First use your fingers to tighten the fitting bolt as tight as you can Then use a wrench to tighten the fitting an additional 3 4 turn 270 degrees 2 If leaks occur replace the fitting bolt ferrule and tubing Capillary IC ...

Page 322: ... 0 25 mm 0 010 in ID PEEK 10 cm 4 in Black 042690 1 in Primary and secondary pump heads 0 51 mm 0 020 in ID PEEK 13 cm 5 in Orange 042855 1 in Microbore systems only Proportioning eluent valve to inlet check valve 1 02 mm 0 040 in ID PEEK 13 cm 5 in Tan 054410 1 in Standard bore systems only Proportioning eluent valve to inlet check valve 0 159 cm 0 0625 in ID PharMed Yellow 063268 1 in Peristalti...

Page 323: ...n 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 10 mm 0 39 in ID polyethylene Colorless 055075 Drip tray drain hose 1 16 in fitting bolt 1 16 in ferrule Tan Tan 052230 062511 Inlet check valve fitting 1 8 in fitting bolt 1 8 in ferrule Tan Yellow 052267 048949 Eluent reservoir fittings High pressure 10 32 fitting bol...

Page 324: ...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 The pump should be primed if the elu...

Page 325: ...efault 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 If the priming valve is opened too much air is drawn through the val...

Page 326: ...he Chromeleon Panel 1 Open the priming valve on the secondary pump head see Figure 9 2 by turning it one half turn counterclockwise NOTE If the priming valve is opened too much air is drawn through the valve and air bubbles can be seen exiting the waste line 2 On the Chromeleon 7 ePanel Set or the Chromeleon 6 8 panel tabset click the Pump tab 3 Gradient pump only Enter 100 for the channel A B C o...

Page 327: ... repeat the priming procedure 8 Close the priming valve by turning it clockwise Do not overtighten the priming valve 9 Enter the flow rate required for your application 10 Gradient pump only Enter the required proportions of eluents A B C and D on the Pump panel 11 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 ...

Page 328: ...e Table 9 2 Before beginning locate the 1 2 inch wrench P N 062336 in your pump ship kit Additional items Cleanroom gloves lint free particle free and oil free 0 2 micron filtered Class 10 isopropyl alcohol IPA 0 2 micron filtered canned air duster ITW Chemtronics Ultrajet or equivalent Pump Type Check Valve Assembly Part Number Capillary IC Inlet 044541 Outlet 044540 Analytical IC Inlet 045722 Ou...

Page 329: ...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 7 The check valves are installed in the primary pump head see Fi...

Page 330: ...rtridge see Figure 9 4 is visible If the double hole end is not visible remove the cartridge from the housing and install it correctly Figure 9 4 Inlet Check Valve Assembly 2 The outlet check valve assembly housing has a smaller 10 32 port Inspect the new outlet check valve assembly to verify that the single hole end of the cartridge is visible see Figure 9 5 If the single hole end is not visible ...

Page 331: ...om of each port for any particulate matter If necessary rinse and dry again until they are clean 4 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 5 Tighten the check valves fingertight and then use the 1 2 inch wrench to tighten an additional one quarter to one half turn 6 Push the component mounting...

Page 332: ...talling new seals Section 9 7 5 Reinstalling the piston and pump head Section 9 7 6 NOTE Capillary IC pumps and analytical IC pumps use different main piston seals and piston seal wash seals Before continu ing verify that you have the correct seal for your pump type Part numbers are shown on Figure 9 6 and Figure 9 7 Before beginning locate the following items in your pump ship kit 3 0 mm hex key ...

Page 333: ...d and Piston 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 Disconnect the pump from the software by clicking Connected on the Pump panel Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the DP SP ...

Page 334: ...te the inside of the pump head and result in poor pump performance Figure 9 6 DP SP Pump Primary Pump Head Assembly Inlet Check Valve Assembly P N 044541 Capillary P N 045722 Analytical Outlet Check Valve Assembly P N 044540 Capillary P N 045721 Analytical Piston P N 068646 Capillary P N 062082 Analytical Piston Seal Wash Seal P N 068628 Capillary P N 063382 Analytical Seal Wash Body P N 074446 Ca...

Page 335: ...ne side and then pull it out of the pump mecha nism Figure 9 7 DP SP Secondary Pump Head Assembly Piston P N 068646 Capillary P N 062082 Analytical Piston Seal Wash Seal P N 068628 Capillary P N 063382 Analytical Seal Wash Body P N 074446 Capillary P N 062064 Analytical Seal Retainer P N 068627 Capillary P N 062092 Analytical Main Piston Seal P N 075493 Capillary P N 064946 Analytical Secondary Pu...

Page 336: ...sing a 10 cc syringe P N 054578 inject a few drops of ASTM Type I 18 megohm cm filtered and deionized water through the main piston seal and into the piston cavity in the pump head 4 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 5 If the piston seal was not removed in Step 4 follow these steps a Verify ...

Page 337: ... 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 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 ...

Page 338: ...own on a clean work surface Make sure the open side of the piston seal faces away from the retainer for the seal wash seal 6 Using IPA rinse inside the pump head cavity where the seal will be installed Blow inside the cavity to dry it using the 0 2 micron filtered canned air duster Inspect the cavity for any particulate matter If necessary rinse and dry again until the cavity is clean Fill the cav...

Page 339: ... turn only 5 Push the component mounting panel back into the enclosure Close the DP SP door 6 Press the POWER button on the front of the DP SP to turn on the pump 7 Reconnect the pump to the software by clicking Connected on the Pump panel 8 Turn on the pump flow 9 8 Replacing the Piston If a new piston seal leaks assuming that the pump head is tight it indicates that the piston is dirty scratched...

Page 340: ...nel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following Disconnect the pump from the software by clicking Connected on the Pump panel Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the DP SP door to access the mechanical components 4 Five red Phillips screws are installed on the component m...

Page 341: ...mp mecha nism 10 If the piston is broken be sure to remove all broken pieces If necessary flush the pump head with ASTM Type I 18 megohm cm filtered and deionized water 9 8 2 Reinstalling the New Piston Slide the new piston P N 068646 for capillary P N 062082 for analytical partway into the pump head approximately 6 mm 1 4 in of the sapphire part of the piston should extend from the head 9 8 3 Rei...

Page 342: ...iston 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 s...

Page 343: ...w 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 Figure 9 9 Peristaltic Pump for Seal Wash System Pump Ship Kit Part Number DP Ship Kit Dual Capillary 072112 DP Ship Kit Dual Analytical 062463 DP Ship Kit Capillary and Analytical 07...

Page 344: ...t position with one hand c With your other hand wind the tubing around the rotor d Release the lever Figure 9 10 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 le...

Page 345: ...e pump from the software by clicking Connected on the Pump panel Press the POWER button on the front of the DP SP for 2 seconds to turn off the pump 3 Open the front door of the DP SP 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 unt...

Page 346: ...urn on the pump 12 Reconnect the pump to the software by clicking Connected on the Pump panel 13 Turn on the pump flow 9 11 Changing the DP SP Main Power Fuses 1 Turn off the pump flow 2 Begin monitoring the Current Pressure reading on the Pump panel on the Chromeleon 7 ePanel Set or Chromeleon 6 8 panel tabset When the system pressure reaches zero do the following Disconnect the pump from the sof...

Page 347: ...sher Scientific recommends always replacing both fuses 7 Reinstall the fuse cartridge 8 Reconnect the main power cord to its source and to the DP SP Figure 9 13 DP SP Fuse Cartridge 9 Turn on the main power switch 10 Press the POWER button on the front of the DP SP to turn on the pump 11 Reconnect the pump to the software by clicking Connected on the Pump panel 12 Turn on the pump flow HIGH VOLTAG...

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Page 349: ...2 mm 0 0025 in ID PEEK 18 cm 7 in Blue 072204 CR TC ELUENT IN to EGC OUT Tubing assembly 0 25 m 0 010 in ID PEEK 64 cm 25 in Black 072224 EG degas REGEN OUT to CR TC REGEN IN Tubing assembly 1 58 mm 0 062 in ID ETFE 2 1 m 7 ft Clear 072225 CR TC REGEN OUT to waste 10 mm 0 39 in ID polyethylene Colorless 055075 Drip tray drain hose High pressure 10 32 fitting bolt Blue 074449 Use high pressure fitt...

Page 350: ...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 For tightening requirements for the high pressure fitting bolt P N 074449 and ferrule P N 074373 see Section 9 2 For tightening requirements for the 10 32 fitting bolt P N 043275 and ferrule P N 043276 refer to Installation of...

Page 351: ... DC Ship Kit P N 072011 Refer to the instructions provided with the cutter Tubing Fitting Size and Type Color P N Used to connect 0 25 mm 0 010 in ID PEEK tubing Black 042690 1 in EGC to pump EGC to CR TC RFIC Eluent Degasser to injection valve RFIC Eluent Degasser to eluent reservoir 1 6 mm 0 062 in ID PTFE tubing Colorless 014157 1 in RFIC Eluent Degasser REGEN IN to CR TC RFIC Eluent Degasser R...

Page 352: ...ystem cannot be operated you must work forward through the system adding parts one at a time until an abnormal pressure increase and hence the restriction is found 9 14 Replacing the EGC Replace the EGC when the cartridge is expended or when it leaks Refer to Table 2 2 for a list of the EGC models that can be used with the Dionex ICS 5000 Eluent Generator Analytical IC systems require EGC III cart...

Page 353: ...eakage when you turn over the cartridge in Step 7 If you are removing a capillary EGC tighten the vent fitting on the top of the EGC see Figure 9 15 Figure 9 15 Capillary EGC Vent Fitting La cartouche d EGC contient un de ce qui suit une base corrosive KOH LiOH ou NaOH un acide corrosif MSA ou une solution concentrée de K2CO3 Porter des lunettes et des gants protectives en manipulant la cartouche ...

Page 354: ...e the 10 32 plug P N 053981 removed from the EGC vent opening during installation Install the plug into the vent opening 6 Lift the EGC straight up and off the cartridge holder 7 Turn the EGC upside down and place it on the EG drip tray see Figure 9 17 This is the service position for the cartridge Figure 9 17 EGC in the Service Position Analytical Version Shown 8 Disconnect the EGC IN and EGC OUT...

Page 355: ...and membranes nonhazardous however check your local state and federal regulatory agency regulations for proper disposal 9 14 3 Storing an Old EGC If the EGC is not expended follow these steps to prepare the cartridge for storage 1 Plug all fittings Tighten the vent fitting capillary EGC or cap the vent port analytical EGC This will prevent the evaporation of water in the electrolyte reservoir 2 St...

Page 356: ...apillary IC Systems EGC OUT TO PUMP DAMPER EGC IN To CR TC Regen Out blue label To CR TC Eluent In red label ELUENT OUT REGEN IN To EG Degas Regen Out blue label To CR TC Regen In orange label Vent WASTE GAS SEPARATOR To CR TC Eluent Out yellow label To EG Degas Eluent In red label EG Degas Cartridge inside DC ELUENT IN REGEN OUT ELUENT OUT To Inject Valve EGC Capillary Tubing Assembly Key 0 25 mm...

Page 357: ...lse damper see Figure 9 19 This is a temporary connection to provide backpressure during the EGC setup procedure 7 Connect a piece of 0 25 mm 0 010 in ID black PEEK tubing to the EGC OUTLET port Direct the other end of the tubing to waste This is a temporary connection Figure 9 19 Flow Schematic for Flushing the Capillary EGC To Waste Pump Outlet Tubing Assembly P N 068658 0 25 mm 0 010 in PEEK tu...

Page 358: ...n 7 ePanel Set or Chromeleon 6 8 panel tabset select the following settings a DC panel Verify that the suppressor Mode is off b EG panel Verify that the CR TC is off c Pump panel Set the flow rate to 0 02 mL min This turns on the pump flow also 12 Flush the capillary EGC for 20 minutes and then turn off the pump flow 13 Disconnect the temporary tubing from the EGC OUTLET port To ensure proper vent...

Page 359: ... temporary connection 4 Verify that the suppressor Mode is off Figure 9 21 Flow Schematic for Conditioning the Capillary EGC Capillary IC EGC OUT 0 25 mm 0 010 in Temporary connection ID PEEK Tubing To CR TC Eluent Out yellow label To CR TC Regen Out blue label To CR TC Eluent In red label To CR TC Regen In orange label ELUENT OUT REGEN IN EGC Capillary EGC IN TO PUMP DAMPER ELUENT IN 0 062 mm 0 0...

Page 360: ...e backpressure tubing from the EGC IN line 11 Use a high pressure blue fitting to connect the EGC IN line to the EGC INLET port 12 Disconnect the temporary tubing from the ELUENT OUT and REGEN IN ports of the CR TC 13 Reconnect the lines to the ELUENT OUT and REGEN IN ports of the CR TC that were disconnected in Step 2 To avoid damaging the suppressor always turn it off before conditioning the EGC...

Page 361: ... the shipping container NOTE Save the shipping container it may be required for storage or disposal of the EGC Figure 9 22 EG Flow Schematic Example for Analytical IC Systems Eluent Out EGC VENT To Waste EGC IN EGC OUT EGC Inlet Outlet TO INJ VALVE P TO PUMP WASTE GAS SEPARATOR Coupler TO SRS AES REGEN OUT Eluent In CR TC Coupler ELUENT OUT REGEN IN TO CR TC REGEN OUT blue label To CR TC Eluent In...

Page 362: ...o the EGC INLET port 6 Locate the yellow 0 5 mL min 7 MPa 1000 psi backpressure coil P N 053765 in the EG Ship Kit P N 072047 7 Connect one end of the backpressure coil to the EGC OUTLET port see Figure 9 23 leave the other end of the coil unconnected This is a temporary connection Figure 9 23 Analytical EGC Outlet Connection for Conditioning Procedure 8 While holding the EGC right side up with th...

Page 363: ...connector fingertight to secure it 11 Remove the 10 32 plug from the EGC vent opening Install a 10 32 luer adapter in the vent opening 12 Connect the luer adapter and VENT line removed from the old cartridge to the vent opening in the new cartridge see Figure 9 16 13 Place the 10 32 plug removed from the vent opening in a safe place for storage The 10 32 plug is required for shipping or storing th...

Page 364: ... panel Verify that the CR TC is off c Pump panel Gradient pump only Select the correct eluent channel A B C or D All pumps Set the flow rate to 1 0 mL min This turns on the pump flow also Figure 9 25 Flow Schematic for Conditioning an Analytical EGC EGC VENT To Waste EGC IN EGC Inlet Outlet TO PUMP To Waste Analytical EGC Conditioning EGC concentration at 50 mM Pump at 1 0 mL min for 30 min 0 5 mL...

Page 365: ...opening 4 Lift the EGC out of the holder turn it upside down and place it on the drip tray in the service position see Figure 9 17 5 Disconnect the backpressure coil from the EGC OUTLET port 6 Connect the EGC OUT line to the OUTLET port 7 Turn the EGC right side up and check for bubbles in the eluent generation chamber If necessary shake and tap the cartridge to remove bubbles 8 Install the EGC in...

Page 366: ...lectrical 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 CR TC from the EG 9 15 2 Installing and Flushing the New CR TC 1 Remove the plugs from the ports on the new CR TC 2 If you are installing a CR TC in a capillary IC system a Connect a piece of 0 25 mm 0 010 in ID PEEK tubing between the ELUENT OUT and REGEN IN...

Page 367: ... Ship Kit Figure 9 26 Plumbing for Hydrating a Capillary CR TC EGC OUT 0 25 mm 0 010 in Temporary connection ID PEEK Tubing To CR TC Eluent Out yellow label To CR TC Regen Out blue label To CR TC Eluent In red label To CR TC Regen In orange label ELUENT OUT REGEN IN EGC Capillary EGC IN TO PUMP DAMPER ELUENT IN 0 062 mm 0 0025 in ID PEEK Tubing Assembly P N 072204 1 58 mm 0 062 in ID Tefzel Tubing...

Page 368: ...st 10 minutes Capillary pumps Set the flow rate to 0 02 mL min This turns on the pump flow also Allow the pump to run for 15 minutes Figure 9 27 Plumbing for Hydrating an Analytical CR TC From EGC Out Port CR TC Hydration Kit Tubing Assembly P N 063487 Temporary connection To RFIC Eluent Degasser Regen In Port ELUENT OUT REGEN IN TO CR TC REGEN OUT blue label To CR TC Eluent In red label Eluent Ou...

Page 369: ...mpleting the New CR TC Plumbing 1 Connect the regen out and eluent in lines from the eluent degasser to their respective ports on the CR TC Refer to Figure 9 28 for a capillary IC system or Figure 9 29 for an analytical IC system Capillary IC Figure 9 28 Capillary CR TC Plumbing Diagram Installation Completed To CR TC Regen Out blue label To CR TC Eluent In red label ELUENT OUT REGEN IN To EG Dega...

Page 370: ...firmly into the CR TC 1 or CR TC 2 bulkhead connector Twist the ring on the cable connector fingertight to secure it 4 Push the tray into the module until it locks into place Close the EG door Figure 9 29 Analytical CR TC Plumbing Diagram Installation Completed To RFIC Eluent Degasser REGEN OUT Port To RFIC Eluent Degasser ELUENT IN Port To Gas Separator Waste Tube To OUTLET Port EGC WASTE GAS SEP...

Page 371: ...h the ball studs on the component mounting panel Push the degasser firmly onto the mounting ball studs The degasser clicks into place when properly installed 8 Push the tray into the module until it locks into place Close the EG door 9 17 Installing a Backpressure Coil In an analytical IC system the EGC requires at least 14 MPa 2000 psi of system backpressure this ensures optimal removal of electr...

Page 372: ...Description Flow Rate Approximate Backpressure Added 053762 4 mm ID 2 0 mL min 3 5 MPa 500 psi 1 0 mL min 1 75 MPa 250 psi 053763 4 mm ID 2 0 mL min 7 MPa 1000 psi 1 0 mL min 3 5 MPa 500 psi 053764 2 mm ID 0 50 mL min 3 5 MPa 500 psi 0 25 mL min 1 75 MPa 250 psi 053765 2 mm ID 0 50 mL min 7 MPa 1000 psi 0 25 mL min 3 5 MPa 500 psi Table 9 5 EG Backpressure Coils ...

Page 373: ...drawer 5 Pull the fuse drawer out of the rear panel and remove the old fuses 6 Replace the two fuses with new 2 A IEC 60127 2 slow blow fuses P N 954773 Thermo Fisher Scientific recommends always replacing both fuses Figure 9 30 EG Fuse Drawer 7 Insert the fuse drawer into the rear panel and press until the drawer snaps into place 8 Reconnect the main power cord and turn on the power HIGH VOLTAGE ...

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Page 375: ...n with 10 32 ferrule fitting White 057301 AS normal and concentrate modes only Injection valve to the AS inject port 0 25 mm 0 010 in ID PEEK tubing 50 cm 20 in Black 042690 1 in AS sequential modes only Injection valve to AS diverter valve ED Cell Inlet Tubing Kit N A 074221 ED cell inlet to column outlet 10 32 fitting bolt 10 32 ferrule double cone Black Tan 043275 043276 Suppressor eluent out C...

Page 376: ...parator column inlet Precision cut 0 062 mm 0 0025 in ID PEEK tubing blue labeled VALVE PORT 3 210 mm 8 27 in 072187 Separator column inlet to injection valve if a guard column is not present 0 25 mm 0 010 in ID PEEK tubing black 610 mm 24 in 042690 EG degas cartridge REGEN OUT to waste if an EG is not present 0 125 mm 0 005 in ID PEEK tubing red 610 mm 24 in 044221 Inject valve waste to AS waste ...

Page 377: ...ush with the end of the tubing For detailed connection instructions see Section 9 1 Except for capillary tubing you can use a tubing cutter to cut tubing to the required length Make sure the cut is at a right angle to the length of the tubing and there are no nicks or burrs on the end A tubing cutter P N 049584 is included in the DC Ship Kit P N 072011 Refer to the instructions provided with the c...

Page 378: ...es only Injection valve to the AS inject port 0 33 mm 0 013 in ID PEEK Light Blue 049714 1 in AS sequential modes only Injection valve to AS diverter valve 0 51 mm 0 020 in ID PEEK Orange 042855 1 in AS simultaneous mode only Each injection valve to the AS simultaneous injection tee 1 58 mm 0 062 in ID PTFE Colorless 014157 1 in Suppressor REGEN OUT 0 125 mm 0 005 in ID PEEK Red 044221 1 in Microb...

Page 379: ...ample loading port to be connected locate the following items in the DC Ship Kit P N 072011 One 1 4 28 fitting P N 052230 and ferrule P N 052231 One 10 32 fitting P N 062980 and ferrule P N 062978 0 75 mm 0 030 in ID green PEEK tubing P N 052304 One luer adapter fitting P N 024305 2 Locate the metal release tab under the sample loading port on the front of the DC see Figure 9 31 Press up on the ta...

Page 380: ...ach 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 Figure 9 32 Sample Loading Port Connection ...

Page 381: ... cable until the connectors for the two cables are outside the panel see Figure 9 34 7 Disconnect the two cables Figure 9 34 Leak Sensor Cable 8 Connect the cable from the new leak sensor to the DC cable 9 Feed the cables back inside the DC Align the leak sensor with the component panel opening and fingertighten the screw 10 Make sure the leak sensor does not touch the bottom of the drip tray Um V...

Page 382: ...nstead of rebuilding the valve Replacing the pod is easier and faster than rebuilding the valve 1 Turn off the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 3 Open the DC door 4 Disconnect each liquid line connected to the valve 5 Follow the instructions provided in the Rebuild Kit to replace the rotor seal isolation seal and stator face 6 Reconnect all...

Page 383: ...require service contact Thermo Fisher Scientific Electronics related repair procedures must be performed by Thermo Fisher Sci entific personnel NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product warranty 1 Turn off the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 3 Open the DC door To avoid ...

Page 384: ...ng 6 Grasp the front of the valve pod and pull out firmly to remove it from the DC or AM 7 Align the slots in the new pod with the runner in the valve holder on the DC or AM see Figure 9 36 Valve pods are keyed to fit only one way one slot is narrower than the other Verify that the slots are aligned with their matching runners Figure 9 35 Unscrew the Locking Ring Valve in IC Cube Shown Locking Rin...

Page 385: ... the pump flow Check for leaks from the valve Tighten fittings as required For tightening requirements refer to Installation of Dionex Liquid Line Fittings Document No 031432 The manual is on the Thermo Scientific Reference Library DVD P N 053891 12 Close the door 9 24 Installing or Replacing an I O Option Board 1 Press the POWER button on the front of the DC for 2 seconds to turn off the power 2 ...

Page 386: ...w 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 HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the DC HAUTE TENSION Débranchez le cordon d alimentation principal de sa source et du panneau arrière du DC HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose u...

Page 387: ... switch on the DC rear panel see Figure 2 31 3 Disconnect the main power cord from both its source and from the DC rear panel Figure 9 38 DC Rear Panel I O Option Installed I O Option HIGH VOLTAGE Disconnect the main power cord from its source and also from the rear panel of the DC HAUTE TENSION Débranchez le cordon d alimentation principal de sa source et du panneau arrière du DC HOCHSPANNUNG Zie...

Page 388: ...fuse drawer into the rear panel and press until the drawer snaps into place 8 Reconnect the main power cord and turn on the power 9 26 IC Cube Service Procedures 9 26 1 Replacing an IC Cube Cartridge 1 Turn off the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC power Fuse Drawer Tab To avoid injury wait for the DC to cool down before opening the door or ...

Page 389: ...dge into the IC Cube Push the cartridge firmly into the IC Cube and then tighten the thumbscrews Figure 9 40 Capillary Cartridge Thumbscrews EG Degas Cartridge Shown 7 If you are installing a suppressor or CRD cartridge hydrate them before use Refer to the instructions in the suppressor or CRD manual The manuals are included on the Thermo Scientific Reference Library DVD P N 053891 8 Reconnect the...

Page 390: ...er door 3 Disconnect the line from the ELUENT OUT port of the injection valve and the line from the ELUENT OUT fitting on the column cartridge see Figure 9 41 4 Loosen the two thumbscrews on the column cartridge and pull the cartridge out of the IC Cube Figure 9 41 Disconnect Capillary Cartridge Eluent Lines Disconnect these two lines ...

Page 391: ...llary separator column is installed Figure 9 42 Separator and Guard Columns Installed in Column Cartridge Figure 9 43 Separator Column Only Installed in Column Cartridge Separator Guard Column Guard Column Separator Precision Cut Precision Cut Column Outlet Column Inlet Inlet 1 3 4 6 7 8 5 1 3 4 7 8 Separator Column 2 2 Guard Column Outlet 5 6 Tubing Tubing Separator Separator Precision Cut Column...

Page 392: ...bing 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 ...

Page 393: ...eparator Column and 35 mm Guard Column Figure 9 47 Tubing Connections for Separator Column Only 250 mm Separator 50 mm Guard 1 3 1 3 2 65 mm 2 5 in 2 Column Precision Cut Tubing Column 115 mm 4 5 in 4 Precision Cut Tubing 4 P N 072189 P N 072188 150 mm Separator 35 mm Guard 1 3 1 3 2 75 mm 3 in 2 Column Precision Cut Tubing Column 115 mm 4 5 in 4 Precision Cut Tubing 4 P N 072189 P N 074603 Separa...

Page 394: ...lumn 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 48 NOTE If the columns are installed correctly the cartridge lid snaps closed easily If the lid does not close easily do not force it Open the lid a...

Page 395: ...3 see Figure 9 41 22 Close the DC upper door 9 27 CD Service Procedures 9 27 1 Calibrating the CD Cell NOTE Do not use this procedure to calibrate a new cell New cells are calibrated at the factory 1 On the Chromeleon 7 ePanel Set click the CD tab On the Chromeleon 6 8 panel tabset click the CD tab Items Needed Description 1 0 mM KCl solution Prepare by dissolving 0 07456 g of reagent grade KCl in...

Page 396: ...fy that backpressure at the pump is at least 7 MPa 1000 psi at 0 01 mL min for capillary or 1 00 mL min for analytical 7 Set the cell heater to 35 C Allow the cell to reach this temperature the LED stops blinking 8 Begin pumping 1 0 mM KCl through the cell at 0 01 mL min for capillary or 1 0 mL min for analytical 9 Wait until the total conductivity reading stabilizes 15 to 30 minutes 10 On the Wel...

Page 397: ...ressor before initial use Suppressor manuals are included on the Thermo Scientific Reference Library DVD P N 053891 1 Stop the pump flow 2 Press the POWER button on the front of the DC for 2 seconds to turn off the DC 3 Open the DC upper door 4 Disconnect the four liquid lines from the suppressor see Figure 9 50 To avoid injury wait for the DC to cool down before opening the door or performing any...

Page 398: ...ss the suppressor against the back of the detector and then slide it to the right to secure it onto the mounting tabs Pull out slightly on the center of the suppressor to verify that it is securely fastened 8 Reconnect the four liquid lines to the new suppressor 9 Plug in the suppressor cable 10 Close the DC door 11 Turn on the DC power and restart the pump flow 9 27 3 Replacing a CD 1 Stop the pu...

Page 399: ...e detector and the receptacle on the inside of the DC 7 Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure 8 Reconnect the cell inlet and outlet lines 9 Reinstall the suppressor see Section 9 27 2 10 Turn on the DC power and restart the pump flow 9 27 4 Removing Trapped Air from the Conductivity Cell Air bubbles in the cell can cause pul...

Page 400: ...y DVD P N 053891 3 If a bubble is still trapped in the cell try these techniques to remove it Loosen and then tighten the cell outlet fitting 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 Suppressor Type Column Format Flow Rate mL min Backpressure C...

Page 401: ...6 8 panel tabset 2 Stop the pump flow 3 Disconnect the cell inlet and outlet lines from the ED cell and disconnect the two electrical cables see Figure 9 52 NOTE For a capillary IC system disconnect the cell inlet line from the ELUENT OUT port of the IC Cube column cartridge 4 Grasp the cell by the cell body and pull straight out to remove it from the detector Figure 9 52 Disconnecting the ED Cell...

Page 402: ...able Gold Electrode Installation Guide Document No 065191 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 ED cell gasket for conventional working electrodes P N 045972 Gloves Blunt end tweezers When you install a disposable electrode m...

Page 403: ... the yoke knob on the yoke block by unscrewing it two to three turns see Figure 9 53 3 Squeeze the tabs on the sides of the yoke block and pull the block and knob off the working electrode see Figure 9 53 NOTE Handle the cell gasket and the inside surfaces of the cell carefully to prevent scratches which may subse quently cause leaks Figure 9 53 Disassembling the ED Cell Cell Configured for Analyt...

Page 404: ...olished surface of the cell with a clean damp lint free tissue 8 Install the new gasket over the alignment pins on the cell body When correctly installed one end of the gasket extends beyond the cell body to facilitate gasket installation and removal 9 Verify that the gasket is flat against the cell body and is not wrinkled Figure 9 54 ED Cell Components Figure 9 55 ED Cell Gasket for Conventional...

Page 405: ...tage 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 el...

Page 406: ...es from the other working electrodes c Designate a pad that will not be used with polishing compound This pad is for removal of particles after polishing see Step 5 d Moisten the suede side of the polishing pad slightly with water and place the pad on a smooth flat surface with the suede side facing up 3 Polish the electrode If you are polishing the electrode before initial installation use only t...

Page 407: ...the step with the fine compound 5 Using a moist piece of polishing cloth with no polishing compound added rub the polished surface free of residual polishing compound particles 6 Inspect the surface of the working electrode to make sure that it is clean Repeat Step 5 if necessary NOTE The polishing pads are reusable Do not rinse the pol ishing compound from the pads After initial use add only enou...

Page 408: ...s occur that are not corrected by regenerating the electrode Performance problems can include no pH readouts a shift in Ag AgCl reference potential or incorrect readouts baseline spikes or a decreased response even with a freshly polished working electrode The pH Ag AgCl reference electrode typically lasts from 3 months to 1 year depending on use NOTE To regenerate a pH Ag AgCl reference electrode...

Page 409: ...n 1 5 to remove any precipitated salt 5 Calibrate the pH Ag AgCl reference electrode see Section 9 28 6 Figure 9 56 Removing the pH Ag AgCl Reference Electrode Cell Configured for Analytical IC Shown Unscrew the pH Ag AgCl reference electrode Always store the electrode in the storage cap filled with saturated KCl solution when the cell is not in use This prevents the pH Ag AgCl reference electrode...

Page 410: ...ng an electrode that is currently in use a Follow the instructions in Section 9 28 1 to turn off the cell voltage stop the pump flow and disconnect the cell from the detector b Unscrew the pH Ag AgCl reference electrode and remove it from the cell body see Figure 9 56 c To remove any precipitated salt rinse the pH Ag AgCl reference electrode thoroughly in ASTM Type I 18 megohm cm filtered and deio...

Page 411: ...rode cable and the cell cable 7 Grasp the cell body and pull straight out to remove the cell from the detector If you are installing the pH Ag AgCl reference electrode in a capillary IC system go on to page 396 If you are installing the pH Ag AgCl reference electrode in an analytical IC system go on to page 398 Figure 9 58 Wellness Panel Dionex ICS 5000 Electrochemical Detector Chromeleon 7 Versio...

Page 412: ...t fittings 2 Use a sharp tool for example the tip of a safety pin or a straight pin to remove the pH Ag AgCl reference electrode O ring see Figure 9 59 3 Using tweezers install the reference electrode gasket for capillary IC P N 072162 into the bottom of the reference electrode well see Figure 9 60 Figure 9 59 pH Ag AgCl Reference Electrode O Ring Figure 9 60 Reference Electrode Gasket for Capilla...

Page 413: ...l 6 Screw the pH Ag AgCl reference electrode into the reference electrode well and tighten it fingertight see Figure 9 62 Figure 9 62 Installing the pH Ag AgCl Reference Electrode In the Reference Electrode Well 7 Orient the cell assembly with the yoke knob on the left and then push the cell onto its mounting location on the ED 8 Connect the reference electrode cable and the cell cable 9 Reconnect...

Page 414: ...et and outlet fittings 2 Verify that the pH Ag AgCl reference electrode O ring is present see Figure 9 63 and then screw the pH Ag AgCl reference electrode into the reference electrode well and tighten it fingertight see Figure 9 62 3 Orient the cell assembly with the yoke knob on the left see Figure 9 52 and push the cell onto its mounting location in the DC compartment 4 Reconnect the cell inlet...

Page 415: ...gCl reference electrode thoroughly in ASTM Type I 18 megohm cm filtered and deionized water that meets the specifications listed in Section 1 5 4 Use a sharp tool for example the tip of a safety pin or a straight pin to remove the pH Ag AgCl reference electrode O ring see Figure 9 65 5 Slide the new O ring P N 014067 onto the electrode Figure 9 64 Removing the pH Ag AgCl Reference Electrode Cell C...

Page 416: ...flow 11 Wait until the pump pressure has stabilized 30 to 60 seconds and then turn on the cell voltage 9 28 8 Replacing a PdH Reference Electrode When to Replace a PdH Reference Electrode Replace the PdH reference electrode if its sensing surface is damaged or if the electrode no longer seals properly Replace the PdH electrode if performance has degraded for example lower response higher backgroun...

Page 417: ... then remove the nut from the reference electrode well see Figure 9 66 3 Pull the reference electrode out of the well see Figure 9 67 Figure 9 66 Unscrewing the PdH Reference Electrode Nut Figure 9 67 Removing the PdH Reference Electrode from the Reference Electrode Well Nut PdH Reference Electrode ...

Page 418: ... 9 69 To avoid deforming the gasket cutout do not place the tweezer tips on the cutout 6 Align the gasket so that the notched edge of the gasket aligns with the corresponding notch in the reference electrode well and press the gasket into the well Figure 9 68 Removing the PdH Reference Electrode Gasket Figure 9 69 Installing the PdH Reference Electrode Gasket PdH Reference Electrode Gasket Notch i...

Page 419: ...ing align with the grooves in the reference electrode well see Figure 9 70 9 Insert the fitting into the well 10 Screw the nut on the PdH reference electrode into the reference electrode well and tighten it fingertight see Figure 9 71 After fingertightening use a wrench to tighten the nut an additional 20 to 30 degrees Figure 9 70 Inserting the PdH Reference Electrode Fitting into the Reference El...

Page 420: ...anel Enter 100 mM in the Target Concentration field This turns on the power to the EGC also c Verify that eluent is exiting the cell d ED panel Set the reference electrode mode to PdH e Select DC amperometry mode set the cell voltage to 0 000 V and turn on the cell voltage Switch to integrated amperometry mode and select the PdH referenced carbohydrate waveform 2 Condition the electrode for 1 hour...

Page 421: ...the inside of the DC 8 Push the new detector into the opening in the DC and press firmly to ensure the electrical connection is secure 9 Reinstall the cell and reconnect the cell inlet and outlet lines and the cables NOTE If you are installing an ED detector in a system that previ ously was set up for conductivity detection remove the sup pressor cartridge from the IC Cube and replace it with a su...

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Page 423: ...ength of the tubing and there are no nicks or burrs on the end ICS 5000 TC To avoid injury wait for the TC to cool down before opening the door or performing any maintenance or service procedures Afin d éviter toute brûlure laisser refroidir le compartiment thermique avant d ouvrir la porte ou d effectuer des opérations de maintenance Um Verletzungen zu vermeiden warten Sie bitte bis der TC abgekü...

Page 424: ...o monitor Install a column ID chip card for the column Close the TC door and select the column properties to be monitored To select the column to be monitored 1 Start the Chromeleon 7 Instrument Configuration program or the Chromeleon 6 8 Server Configuration program 2 Under the instrument or timebase right click the TC and select Properties on the context menu 3 In the TC Properties dialog box se...

Page 425: ...onex logo facing up into the appropriate card reader A B C or D along the top of the compartment see Figure 9 74 When the chip card is installed correctly the LED next to the slot is green Figure 9 74 Inserting a Column ID Chip Card 3 Install a chip card for any other columns to be monitored To select the column properties to be monitored 1 Close the TC door if it is open You cannot select column ...

Page 426: ...sier 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 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 To avoid injury wait for the TC to cool down before opening the door o...

Page 427: ... the pod of the TC injection valve NOTE If the valve electronics require service contact Thermo Fisher Scientific Electronics related repair procedures must be performed by Thermo Fisher Scientific personnel NOTE Substitution of non Dionex Thermo Fisher Scientific parts may impair valve performance and void the product war ranty Figure 9 75 Injection Valve Plumbing 6 Port Valve SAMPLE IN from door...

Page 428: ...t number of ports for the injection valve being serviced 7 Align the slots in the new pod with the runner in the valve holder in the TC see Figure 9 77 Valve pods are keyed to fit only one way one slot is narrower than the other Verify that the slots are aligned with their matching runners To avoid injury wait for the TC to cool down before opening the door or performing any maintenance or service...

Page 429: ... 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 Figure 9 77 Injection Valve Pod and Pod Holder Slot large...

Page 430: ...C 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 HAUTE TENSION Débranchez le cordon d alimentation principal de sa source et du panneau arrière du TC HOCHSPANNUNG Ziehen Sie das Netzkabel aus der Steckdose und der Netzbuchse auf der Rückseite des TC Figure 9 78 TC...

Page 431: ... with settable flow increments at 0 001 mL min Analytical 0 001 3 000 mL min with settable flow increments at 0 0001 mL min Capillary Flow Rate Precision 0 1 Analytical Flow Rate Accuracy 0 1 Analytical at 14 MPa 2000 psi Pressure Ripple 1 0 Analytical at 1 0 mL min typical 0 2 with damper at 10 μL min at 14 MPa 2000 psi Pressure None required Vacuum Degasser Integrated optional 1 channel for isoc...

Page 432: ...hy Management Software supports Microsoft Windows XP or Vista Automated Procedure Wizards Yes standard feature System Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Application Templates Yes standard feature Automation Support of 3rd Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers i...

Page 433: ...in Power Requirements 90 264 VAC 47 63 Hz Auto sensing power supply no manual voltage or frequency adjustment required Typical input power 28 W Maximum line draw 1 2 A at 110 VAC Fuse Requirements Two IEC 60127 2 slow blow fuses P N 954773 rated at 2 A 250 V Physical Dimensions h w d 36 21 48 cm 14 8 25 19 in Weight SP 20 4 kg 45 lb DP 24 1 kg 55 lb Flow Path All polymeric PEEK anion or cation con...

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Page 435: ...pillary Maximum Solvent Concentration Analytical and Capillary Cations None Anions 25 methanol Gradient Profiles Standard any combination of an unlimited number of linear convex and concave positive and negative gradient profiles Number of Cartridges Supported Two dual cartridge support RFIC Eluent Degasser Analytical Only Eluent degasser housed in the EG module System Software Software Chromeleon...

Page 436: ...igger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature Eluent Cartridge Information Storage Yes serial number and expiration date Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance Yes optional package provides security system modification history and electronic signatures Electrical ...

Page 437: ...luent Regeneration Specifications Analytical IC Only Eluents Carbonate and carbonate bicarbonate combinations up to 20 mM MSA up to 34 mM Flow Rates 1 00 2 00 mL min Continuous Operation with 4 L of Eluent Up to 28 days or 2000 samples typically Always On Always Ready Capable Yes standard feature Remains Fully Calibrated for Extended Periods of Time 28 Days Yes standard feature Results are traceab...

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Page 439: ...umn Heat Exchangers two 2 mm or 4 mm column ID version Automation Manager Optional Analytical Only Injection Valves Up to two high pressure valves either 6 or 10 port 2 position Low Pressure Valves Up to two inert 2 or 3 way Reaction Coil Heater RCH Holds two reaction coils RCH Temperature Range 5 C above upper zone 80 C maximum AutoPrep Kit Dual loop with sample pre concentration All valves and h...

Page 440: ...ay valves for fluidic automation Suppression Non suppressed conductivity Yes supported Suppressor wear parts None No valves pumps peristaltic pump tubin g or inline filters required Chemical Suppression 2 mm and 4 mm anion and cation membrane suppression available Displacement Chemical Suppression 2 mm and 4 mm anion and cation membrane suppression available Electrolytic Suppression Self Regenerat...

Page 441: ...eq min AMMS ICE N A Anion CES 0 4 mm 2 μeq min Cation CES 0 4 mm 1 5 μeq min Suppressor Void Volumes SRS 300 4 mm 50 μL SRS 300 2 mm 15 μL MMS 300 4 mm 50 μL MMS 300 2 mm 15 μL AMMS ICE 300 4 mm 50 μL AMMS ICE 300 2 mm 15 μL AES Anion or Cation 35 μL Anion CES 0 4 mm 1 0 μL Cation CES 0 4 mm 1 0 μL System Software Software Chromeleon Chromatography Data System requires Microsoft Windows XP or Vist...

Page 442: ...tandard feature System Trigger Commands and Conditionals Yes standard feature Daily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory current and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance Yes optional Electrical Main Power Requirements 90 265 VAC 47 63 Hz...

Page 443: ... signal processing autoranging Cell Drive 8 kHz square wave Linearity 1 Resolution 0 00238 nS cm Output Range Digital Signal Range 0 15 000 µS cm Analog Signal Range 0 15 000 µS cm Noise Wet 0 2 nS at 23 µS cm background 0 1 nS at 1 µS cm background Filter Rise times 0 to 10 s programmable Sampling Rate 1 to 100 Hz user settable or automatic Cell Temperature 5 C above DC upper zone temperature to ...

Page 444: ...rt of Third Party Instruments Yes fully controls over 300 different instruments from more than 30 manufacturers including GC HPLC and MS Customizable System Control Panels Yes standard feature Signal Channels Conductivity Total Conductivity Data Trending Yes all device numerical parameters plotted System Status Virtual Channels Yes standard feature Power Failure Protection Yes standard feature Sys...

Page 445: ... s response time user settable Control Mode Local or remote control using relay closures or TTL or control using Chromeleon via DC module Cell Body Titanium body with narrow bore PEEK inlet tubing for capillary format titanium inlet tubing for analytical format Compatible with 0 2 0 6 mm ID columns PEEK inlet 2 7 mm ID columns titanium inlet Working Electrodes Conventional gold glassy carbon plati...

Page 446: ...w integrated amperometry data set with crosshairs on an isoamperometric plot used to select slices of the plot along the applied voltage axis to render a chromatogram and along the time axis to render a voltammogram Automated Procedure Wizards Yes standard feature System Smart Startup and Shutdown Yes standard feature System Wellness and Predictive Performance Yes standard feature Application Temp...

Page 447: ...ily Audit Trail Yes standard feature Sample Audit Trail Yes standard feature System Calibration Storage Yes factory present and previous Completely user selectable Customized Reporting Yes standard feature with unlimited report workbooks GLP Compliance Yes optional Physical Dimensions h x w x d 6 9 16 7 9 9 cm 2 7 6 5 3 9 in Weight 400 g 1 6 lb ICS 5000 ED Electrochemical Detector Specifications C...

Page 448: ...Dionex ICS 5000 Operator s Manual 432 Doc 065342 06 12 11 ...

Page 449: ...e column sets 1 9 mm Maximum Column Length 300 mm 50 mm guard column Precolumn Heat Exchangers optional Two low delay volume exchangers Leak Detection Humidity and vapor sensors TTL and Relay Inputs and Outputs Two digital inputs outputs Two relay outputs Control Chromeleon Chromatography Data System Computer Connection USB Electrical Main Power Requirements 90 264 VAC 47 63 Hz Auto sensing power ...

Page 450: ... ICS 5000 Operator s Manual 434 Doc 065342 06 12 11 Environmental Operating Temperature 10 35 C 50 95 F Operating Humidity 5 80 relative noncondensing ICS 5000 TC Thermal Compartment Specifications Continued ...

Page 451: ...embly for primary pump head includes outlet nut and 1 8 in cartridge 075493 capillary 064946 analytical Main piston seal 074371 Backup ring for capillary pumps 040695 O ring for capillary or analytical pump 074446 capillary 062064 analytical Seal wash body 068628 capillary 063382 analytical Piston seal wash seal 068627 capillary 062092 analytical Retainer for piston seal wash seal 068646 capillary...

Page 452: ...ICS 5000 Eluent Organizer with 2 2 liter reservoirs 072058 Dionex ICS 5000 Eluent Organizer with 4 2 liter reservoirs 063291 Eluent reservoir plastic 1 liter 062510 Eluent reservoir plastic 2 liter 063292 Eluent reservoir plastic 4 liter 074423 EO Regulator Accessory and Stand 064792 TC VWD PDA Regulator Bracket Kit 074422 Regulator 045987 Filter end line 044105 Filter high pressure inline Miscell...

Page 453: ...cc 954773 Fuse IEC 60127 2 slow blow rated at 2 A 250 V 063246 USB cable 1 m 3 ft long 005 9001A Cinch connector 2 pin Maintenance Kits 075038 ICS 5000 Analytical Pump Preventive Maintenance Kit 075039 ICS 5000 Capillary Pump Preventive Maintenance Kit Part Number Item ...

Page 454: ...Dionex ICS 5000 Operator s Manual 438 Doc 065342 06 12 11 ...

Page 455: ... ATC 060478 CR CTC 080135 EPM III Electrolytic pH Modifier 061686 EGC CO3 Mixer 4 mm 063443 EGC CO3 Mixer 2 mm Precision Cut Tubing for Capillary EG 072203 0 062 mm 0 0025 in ID PEEK 61 cm 24 in CR TC ELUENT OUT to EG Degas ELUENT IN 072204 0 062 mm 0 0025 in ID PEEK 18 cm 7 in CR TC ELUENT IN to EGC OUT Backpressure Coils 053762 Backpressure coil 2 0 mL min 500 psi 4 mm 053763 Backpressure coil 2...

Page 456: ...e used with system pressures up to 35 MPa 5000 psi 074218 RFIC Eluent Degasser f5or analytical IC systems 954773 Fuse IEC 60127 2 slow blow rated at 2 A 250 V 063246 USB cable 1 m 3 ft long 043276 Ferrule fitting 10 32 double cone 043275 Fitting bolt 10 32 for double cone ferrule fitting 046985 Mini screwdriver Part Number Item ...

Page 457: ... 1 4 28 for manual injections 016388 Syringe 1 cc for manual injections 074698 Valve rebuild kit 4 port 057896 Valve rebuild kit 6 port 061759 Valve rebuild kit 10 port IC Cube and Accessories for Capillary IC 072000 Dionex IC Cube 072186 IC Cube tubing kit includes precision cut tubing for column connections 074459 EG degas cartridge capillary Can be used with system pressures up to 35 MPa 5000 p...

Page 458: ... 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 AgCl reference electrode for analytical 072162 Gasket for pH Ag AgCl reference electrode for capillary 072075 PdH reference electrode 072214 Gasket...

Page 459: ...ets 060141 Gaskets for disposable working electrodes PTFE 0 002 in 4 gaskets for analytical systems 069339 Gasket for carbon disposable working electrodes ULTEM 0 001 in for analytical systems 072117 Gasket for disposable working electrodes PTFE 0 001 in 2 gaskets for capillary systems 062158 ED cell polypropylene support block for use with disposable electrodes 036313 Polishing kit 036319 Coarse ...

Page 460: ...ctor plug 12 position 043598 Twisted pair of wires Miscellaneous 954772 Fuse IEC 60127 2 slow blow rated at 10 A 250 V 960777 USB cable 1 8 m 6 ft long 062437 Leak sensor 043276 Ferrule fitting 10 32 double cone 043275 Fitting bolt 10 32 for double cone ferrule fitting 044105 Filter high pressure inline Maintenance Kits 075040 0 4 L Internal Loop High Pressure Valve Preventive Maintenance Kit 0750...

Page 461: ...10 port valve 042857 Sample loop 25 µL Consumables 6710 1505 Column ID Kit includes five column ID chip cards 064786 Column Clips Kit includes six column clips 064548 Temperature stabilizer standard bore 0 25 mm 0 010 in ID 064650 Temperature stabilizer microbore 0 125 mm 0 005 in ID Miscellaneous 954776 Fuse IEC 60127 2 time lag rated at 2 A two fuses required 063246 USB cable 1 m 3 ft 6000 1004 ...

Page 462: ...Dionex ICS 5000 Operator s Manual 446 Doc 065342 06 12 11 ...

Page 463: ...rile 76 Ag AgCl half cell 77 Air bubbles conductivity cell 383 Air particulate samples 147 Air pressure requirements 146 154 Alarm conditions See Error messages Alarm LED DC 51 Alarm LED DP SP 22 Alarm LED EG 256 LED is lighted 253 Troubleshooting 253 Alarm LED TC 115 Amperometry cell Cell design 76 Cell gasket replacement 386 Description 75 Electrodes 75 Maintenance 143 Monitoring the pH readout ...

Page 464: ...trolytic Suppressor AES 62 Gas separator waste tube 72 Audit Trail 22 37 Error messages 203 Icons 203 Automation Manager AM 3 94 Description 8 94 High pressure valves 96 Low pressure valves 97 Ordering 443 RCH 1 Reaction Coil Heater 101 Autorecycle mode 73 74 Autosampler Controlling with relays TTLs 87 Filling vials 146 149 Injecting samples 178 Loading the tray 146 149 Sample loading 178 Autozero...

Page 465: ...a 111 Dips instead of peaks 86 Pulsed amperometry example 109 Water dip in 148 Chromeleon 11 Alarm conditions 259 275 Application Wizard 174 176 Audit Trail 22 37 203 Audit Trail error messages 203 Commands dialog box 26 126 156 Connected LED 51 Controlling external valves 82 Controlling high pressure valves 98 Controlling low pressure valves 98 Controlling power relays and TTL outputs 89 Controll...

Page 466: ... Cell calibration 379 Cell description 69 Cell temperature control 69 Description 69 Effect of temperature on conductivity 69 Leaking 270 Replacement procedure 382 Specifications 427 Temperature compensation 70 Configuration drawings 129 139 Connected LED DC LED is lighted 51 Connected LED DP SP LED is lighted 22 Connected LED EG LED is lighted 37 115 Connected LED TC LED is lighted 115 Counter el...

Page 467: ...eplacement procedure 323 Piston seal replacement procedure 316 321 323 324 Piston seal wash tubing replacement procedure 326 Pressure limit tripped 223 255 256 Pressure limits for EG 158 Priming procedures 308 311 Priming valve knob seal replacement 329 Product warranty 303 Pulse damper for capillary pump 27 Selecting pressure limits 158 Shutdown procedure 183 Spare parts 435 Specifications 415 St...

Page 468: ...e eluent concentration 161 Shutdown procedures 185 Spare parts 439 Specifications 419 Status bar buttons and LEDs 37 System configuration 129 USB connections 45 Waste lines 46 47 Eluent generator cartridges 41 Backpressure requirement 43 141 142 255 256 Conditioning procedure 186 Electrical connections 44 Frit outlet 223 336 Leaks 223 253 254 Replacement procedure 336 349 Selecting the eluent conc...

Page 469: ...2 CR TC stopped due to zero flow 243 EG cartridge disconnected 244 EG invalid concentration 245 EG invalid flow 246 EG invalid flow rate concentration 246 EG over current 247 EG over power 248 EG over voltage 248 249 Leak sensor wet 252 Error messages TC AcqOff with previous AcqOn 275 Acquisition still on at program end 275 All samples must specify same value 275 Can t execute Disconnect command 2...

Page 470: ...was already an AcqOff 296 There was already an AcqOn 296 This function cannot be adjusted 297 This operation may affect 297 Two AcqOn commands for channel 296 Unknown error code 297 Unknown format of card data 297 Upper limit must be higher 295 USB LAN communication error 283 Value for parameter is not within 289 Value x replaced by 289 Warning threshold must be higher 296 Warning threshold must b...

Page 471: ...8 4 port valve 66 6 port valve 67 For analytical IC system 65 For capillary IC system 65 High pressure valves TC 117 122 Reordering 445 Humidity leak in TC 115 126 285 Humidity sensor 126 285 Hybrid system configuration 129 132 I I O option DC 82 83 444 5V output 83 Analog outputs 83 Connections 84 Power output 87 Relay outputs 83 TTL inputs and outputs 83 IC Cube 55 Cartridge replacement procedur...

Page 472: ...ailable 117 Inline filter 36 Instrument method Chromeleon 172 Integrated amperometry 103 3D data 109 Data storage 109 Integration interval 104 107 Waveform characteristics 107 Waveform example 104 Interior components DC 53 Analytical IC components 61 Conductivity Detector CD 54 61 Electrochemical Detector ED 54 61 IC Cube 55 Lower compartment description 62 Suppressor types 62 Upper compartment de...

Page 473: ...C 119 Maintenance annual DC 200 DP 196 EG 197 SP 196 TC 202 Maintenance daily DC 199 201 DP SP 195 EG 197 TC 201 Maintenance periodic DP SP 196 TC 201 Maintenance weekly DC 199 DP SP 195 EG 197 TC 201 Manuals for ICS 5000 system 14 15 Mark analog output 86 Matrix elimination 61 94 System configuration 137 138 Methanesulfonic acid eluent 41 Methanol 76 Microbore IC applications 2 MicroMembrane Supp...

Page 474: ...fier 43 pH reading Adjusting potentials for 77 Always 7 0 271 Cannot be set to 7 0 272 Effect on potentials 77 Monitoring 78 Nonexistent 273 pH Ag AgCl reference electrode 75 77 Long term storage 187 O ring replacement procedure 399 Replacement procedure 392 See also Reference electrode Photodiode Array Detector 3 9 Regulator Bracket Kit 35 Piston seal wash solution 26 183 Piston seal wash system ...

Page 475: ...leshooting Processing samples 172 Product warranty voiding 303 Program Wizard Waveforms 108 Programs Chromeleon Autosampler control 178 180 Creating programs 172 Proportioning valves 25 Leaks 237 Malfunction 218 220 Pulse damper for capillary pump 27 Pulsed amperometry 103 3D data 109 Chromatogram example 110 Data storage 109 Integration interval 103 Waveform example 103 See also Integrated ampero...

Page 476: ... Configuring 87 Relay outputs DC 82 Controlling 89 Reordering information DC 441 DP SP 435 EG 439 TC 445 Reprocessing amperometry data 109 Reproducibility Affected by amperometry cell pH 78 Affected by temperature changes 70 Reproducibility is poor 218 Reservoirs eluent 34 Cleaning 214 219 308 Installation in EO 6 34 35 Pressurizing 34 Retention time Troubleshooting 220 Variations 118 Reversed pha...

Page 477: ...2 Replacing capillary columns 375 379 Suppressor replacement 381 Tubing and fittings replacement 359 Working electrode polishing 389 Service procedures DP SP Check valve cartridge replacement 312 Eluent reservoir cleaning 308 Fuse replacement 330 Piston replacement 323 Piston seal replacement 316 321 323 324 Piston seal wash tubing replacement 326 Priming 310 311 Priming valve knob seal replacemen...

Page 478: ...up procedures DC 165 DP SP 153 EG 161 Equilibrate the system 166 170 Offsetting the background 167 TC 169 Static mixer 219 See also GM 3 Gradient Mixer Status bar DC 51 LEDs described 51 115 Status bar DP SP LEDs described 22 Status bar EG LEDs described 38 Status bar TC LEDs described 115 Sulfite in samples 147 Suppressor Description 71 For analytical IC system 71 For capillary IC system 71 Leaki...

Page 479: ... Theory of operation 127 Trace analyses 9 Trap column 5 Tray autosampler Loading 146 149 Triangle waveform 106 Troubleshooting DC Alarm conditions DC 259 Amperometry cell 271 Error messages DC 259 Liquid leaks DC 270 pH readout always at 7 0 271 pH readout cannot be set to 7 0 272 pH readout nonexistent 273 Reference electrode leaks 274 Reference potential shifts 274 VALVE button not working 271 T...

Page 480: ...egassing module 25 Daily maintenance 195 On off control 26 Vacuum is low 238 VALVE buttons DC 52 Enabling disabling 52 Troubleshooting 271 Valve LEDs DC LED is flashing 52 LED is lighted 52 Valve LEDs TC LED is flashing 115 299 LED is lighted 115 Valves See High pressure valves Injection valves Low pressure valves Variable Wavelength Detector 3 10 Regulator Bracket Kit 35 Vials 146 149 Filling 146...

Page 481: ... amperometry 107 Integrated amperometry example 104 Maximum length 107 Pre programmed 108 Pulsed amperometry example 103 Weekly maintenance DC 199 DP SP 195 EG 197 TC 201 Wellness 128 Wireframe plot 112 Working electrodes 75 Maintenance 143 Materials 75 Polishing 389 Z Zero position analog out 86 ...

Page 482: ...Dionex ICS 5000 Operator s Manual Index 20 Doc 065342 06 12 11 ...

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