Man IC ICS5000 Operators Dec2011 DOC065342 06
Man IC ICS5000 Operators Dec2011 DOC065342 06
1 • Introduction
1.1 Thermo Scientific Dionex ICS-5000 System Overview . . . . . . . . . . . 1
1.1.1 Dionex ICS-5000 System Components . . . . . . . . . . . . . . . . . 2
1.1.2 Dionex ICS-5000 System Control . . . . . . . . . . . . . . . . . . . . 11
1.2 Dionex ICS-5000 System Documentation . . . . . . . . . . . . . . . . . . . . . 14
1.3 The Dionex ICS-5000 System Operator’s Manual . . . . . . . . . . . . . . 15
1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . 16
1.4.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . 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 Degassing Module . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.2.5 Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
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 Analytical IC . . . . . . . . . . . . . 61
2.12 DC Temperature Control Zones . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
2.13 High-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
2.13.1 4-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
TC Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
2.20 TC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
2.21 TC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
2.22 TC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
2.23 Injection Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
2.23.1 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 Preparing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 147
4.3.1 Collecting and Storing Samples . . . . . . . . . . . . . . . . . . . . . 147
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 Operational Readiness . . . 166
TC Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.13 Starting the TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.14 Equilibrating the System and Verifying Operational Readiness . . . 170
5 • Operation
5.1 Controlling Modules Directly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
5.2 Analyzing Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
5.2.1 Creating a New Sequence in Chromeleon 7 . . . . . . . . . . . . 173
5.2.2 Creating a New Sequence in Chromeleon 6.8 . . . . . . . . . . 174
5.2.3 Starting a Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 176
5.3 Loading Samples Into the Sample Loop or 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
6.4.1 Short-term Storage of the ED Cell . . . . . . . . . . . . . . . . . . . 187
6.4.2 Long-term Storage of the pH-Ag/AgCl Reference
Electrode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
TC Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.5 Consumables Storage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.6 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.7 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
7 • Maintenance
7.1 System Maintenance Checklists . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.2 Weekly Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
7.1.3 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
7.1.4 Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
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 System Backpressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 223
8.10 Low Detector Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 224
8.11 High Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 225
EG Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 241
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 7.0 . . . . . . . . . . . . . . . . . . . . 271
8.28.2 Cannot Set ED Cell pH Readout to 7.0 . . . . . . . . . . . . . . . . 272
8.28.3 Shift in ED Cell pH Readout . . . . . . . . . . . . . . . . . . . . . . . 272
8.28.4 No ED Cell pH Readout or Intermittent Readout . . . . . . . . 273
TC Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275
8.29 Troubleshooting TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 275
8.30 TC ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 299
8.31 Liquid Leaks from TC Components . . . . . . . . . . . . . . . . . . . . . . . . 300
8.32 TC Temperature Does Not Increase . . . . . . . . . . . . . . . . . . . . . . . . . 301
8.33 TC Temperature Stabilizer Not Operating Properly . . . . . . . . . . . . 301
9 • Service
9.1 Connecting Capillary Tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
9.2 Tightening Guidelines for High-Pressure Fittings . . . . . . . . . . . . . . 305
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 Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . 339
9.14.3 Storing an Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339
9.14.4 Installing and Conditioning a New Capillary EGC . . . . . . 340
9.14.5 Installing and Conditioning a New Analytical EGC . . . . . . 345
9.15 Replacing the CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 349
9.15.1 Removing the Old CR-TC . . . . . . . . . . . . . . . . . . . . . . . . . 350
DC Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 359
9.19 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 359
9.19.1 Tubing and Fittings for Capillary IC Systems . . . . . . . . . . 359
9.19.2 Tubing and Fittings for Analytical IC Systems . . . . . . . . . 362
9.20 Connecting a Sample Loading Port to the Injection Valve . . . . . . . 363
9.21 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 364
9.22 Rebuilding a High-Pressure (Injection) Valve . . . . . . . . . . . . . . . . . 366
9.23 Replacing a High-Pressure (Injection) Valve Pod . . . . . . . . . . . . . . 367
9.24 Installing or Replacing an I/O Option Board . . . . . . . . . . . . . . . . . . 369
9.25 Changing the DC Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . 371
9.26 IC Cube Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 372
9.26.1 Replacing an IC Cube Cartridge . . . . . . . . . . . . . . . . . . . . . 372
9.26.2 Replacing Capillary Columns . . . . . . . . . . . . . . . . . . . . . . . 374
9.27 CD Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 379
9.27.1 Calibrating the CD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . 379
9.27.2 Replacing an Analytical Suppressor . . . . . . . . . . . . . . . . . . 381
9.27.3 Replacing a CD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 382
9.27.4 Removing Trapped Air from the Conductivity Cell . . . . . . 383
9.28 ED Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 385
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 Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . 413
A • Specifications
DP/SP Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 415
EG Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 419
DC Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 423
TC Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 433
B • Reordering Information
DP/SP Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . 435
3 Dionex ICS-5000
Detector/Chromatography Module
3 2
Dionex ICS-5000 Dual Pump (DP) and Dionex ICS-5000 Single Pump (SP)
IMPORTANT
Capillary IC pumps shipped before February 17, 2011 were rated for lower
operating pressures than the pumps currently being shipped. The older
pumps can be operated at pressures up to 35 MPa (5000 psi) (without
RFIC) and up to 21 MPa (3000 psi) (with RFIC). Before operating at
pressures above these limits, verify that you have the appropriate pump.
• HPC is stamped on the secondary
pump heads of the older (lower
pressure rated) capillary IC pumps.
Analytical IC pumps operate at flow rates ranging from 0.00 to 10.0 mL/min
and operating pressures up to 35 MPa (5000 psi) without RFIC and up to
21 MPa (3000 psi) with RFIC. Both microbore and standard bore IC
applications are supported.
The EG generates high purity acid or base eluents online from deionized
water. The EG can be configured for single- or dual-channel operation. Each
channel includes:
• A high precision programmable current source (power supply)
For each channel, the following options must be ordered separately for
installation inside the EG.
• A disposable eluent generator cartridge (EGC). Each cartridge contains an
electrolyte concentrate solution, appropriate 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-TC are available: one for capillary IC systems
and one for analytical IC systems.
Capillary IMPORTANT
IC
If your system includes a capillary pump linked to an
EGC, check the label on the EG degas (capillary)
cartridge in the IC Cube and verify that 5000 psi is
printed on the label (see the figure on the right).
If 5000 psi is not on the label, you must change the high 5000 psi
pressure limit to 21 MPa (3000 psi) (see page 158) or
replace the cartridge with an EG degas (capillary)
cartridge that is rated for 35 MPa (5000 psi)
P/N 074459
(P/N 074459).
The EO holds eluent reservoirs in a liner that contains spills and leaks. Up to
two EOs can be installed on top of the DC. Each EO accommodates up to four
1-liter or 2-liter reservoirs or up to two 4-liter reservoirs. The EO is typically
ordered configured with four 2-liter reservoirs (P/N 072058).
All eluent reservoirs available for use with the DP/SP can be pressurized. If
you plan to pressurize the eluent reservoirs, the optional EO Regulator
Accessory and Stand (P/N 074423) is required.
The Regulator Accessory includes a pressure regulator and gauge assembly
with four outputs (for connections to four eluent reservoirs), as well as the
tubing and connection fitting required. If more reservoirs are required, order a
second regulator (P/N 074422).
the Home panel in Chromeleon 7 and Figure 1-3 shows the Home panel in
Chromeleon 6.8
All Adobe® PDF files listed above are shipped on the Thermo Scientific
Reference Library DVD (P/N 053891), which is included in the ship kit of
each Dionex ICS-5000 system module. In addition, the software manuals are
provided as PDF files on the Chromeleon DVD. A printed copy of the
software installation instructions is provided in the software ship kit.
Signale une situation de danger immédiat qui, si elle n'est pas évitée,
entraînera des blessures 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 de
blessures.
Warnhinweise in Deutsch
Notes
Informational messages also appear throughout this manual. These are labeled
NOTE and are in bold type:
Capillary Sections preceded with the Capillary IC flag indicate that the information in
IC the section applies to capillary 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.
Alternating current
Power supply is on
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
ICS-5000
DP/SP DP/SP Description
FLOW PRIME
1 1 Status Bar
2 Priming Valve
9
10 Tubing Chase (2)
12 Handle (2)
1 Vacuum Degas
1 Chambers (four
channels)
Proportioning
2 Valve Fittings
Proportioning
Valve Outlet to
3 2 3
Primary Pump
Head
4 4 Static Mixer
5
Pump Outlet to
5 EG or Injection
Valve
the pulsation increases as the operating pressure increases, because part of the
delivery stroke is required to compress eluent in the pump head.
During the pre-compression phase, pulsation is minimized. A patented
secondary control system (automatic compressibility compensation) ensures
highly constant eluent delivery. The flow rate remains constant in relation to
the pressure.
NOTE Make sure the run time is long enough to ensure that the vac-
uum degassing module delivers the optimal degassing perfor-
mance.
The piston seal wash system is designed for use with only one of the two
pumps in a DP module. When the DP is shipped from Thermo Fisher
Scientific, the seal wash system is connected to pump 1 (the bottom pump). If
necessary, connect the seal wash system to pump 2 (the top pump), instead.
For instructions on how to replumb the system, refer to Section 4.7.
NOTE For users who need to operate a piston seal wash system for
both pumps in the DP, Thermo Fisher Scientific offers an
External Seal Wash Kit (P/N 063518) or a second seal wash
system (P/N 068661).
OUTLET
CHECK VALVE DI WATER
OR
ELUENT
SECONDARY PRIMARY
PUMP PUMP
HEAD HEAD
INLET
VACUUM
CHECK VALVE DEGAS
PULSE
DAMPER*
• Eluent flows from the reservoir, through the vacuum degas chamber,
through the eluent supply on/off valve, and into the inlet check valve on
the primary pump head.
• The inlet check valve opens, drawing eluent into the primary pump head.
At the same time, the secondary piston pushes forward, pushing eluent
into the system. After completing the intake, the primary piston pushes
eluent through the outlet check valve and into the secondary pump head.
• 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.
SECONDARY PRIMARY
PUMP PUMP
HEAD HEAD
INLET
CHECK VALVE
VACUUM
DEGAS
STATIC
MIXER
A B
PROPORTIONING
VALVE D C
TO ELUENT GENERATOR
OR INJECTION VALVE
• Eluent flows from the reservoirs and through the vacuum degas
chambers. The selected proportions of eluent flow out of the
proportioning valve assembly and into the inlet check valve on the
primary pump head.
• The inlet check valve opens, drawing eluent into the primary pump head.
At the same time, the secondary piston pushes forward, pushing eluent
into the system. After completing the intake, the primary piston pushes
eluent through the outlet check valve and into the secondary pump head.
• 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.
2 6 USB Receptacle
5 (“B” Connectors)
Tubing Chases
The tubing chases route tubing from the front of the DP/SP, through the
interior of the module, and to the rear panel.
The rear panel power switch is the main power switch for the DP/SP. Turn on
the main power switch before initial operation and leave it on unless
instructed to turn it off (for example, before performing a service procedure).
NOTE For routine on/off control, use the POWER button on the front
of the DP/SP (see Figure 2-1 and Figure 2-2). To turn off the
pump, press and hold the POWER button for 2 seconds.
The fuse cartridge contains two 2-amp IEC 60127-2 slow-blow fuses
(P/N 954773). For instructions on how to change the fuses, see Section 9.11.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the DC and is easily accessible.
The digital I/O port provides a connection to auxiliary devices. The connector
includes three TTL inputs and four relay outputs. Table 2-1 indicates the
functions assigned to the connector pins.
The maximum switching voltage of the relays is 24 V. The switching
current must not exceed 100 mA.
The analog pressure output indicates the operating pressure of the pump. The
pressure output is set to 50 mV/MPa (5 mV/14.51 psi). To monitor the
pressure, connect the pressure output to a recorder or an A/D converter. These
are the pin assignments for the 2-pin Cinch connector (P/N 8005.9001A):
The analog pressure output defaults to the pump 1 (bottom pump) output
signal. To redirect the output to pump 2 (the top pump), follow these steps:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the pump name.
4. Select the AnalogOut property and select PumpTop. For Chromeleon
6.8, click Execute.
USB Connections
• One USB receptacle (“B” type connector) allows a connection from the
PC on which Chromeleon is installed.
• Three USB (Universal Serial Bus) ports (“A” type connectors) are
provided for connections to other Dionex ICS-5000 modules.
One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the pump ship kit:
• 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 and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
pump.
For correct drainage, make sure the waste lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.
2.5.1 EO (Optional)
The Dionex ICS-5000 Eluent Organizer (EO) holds eluent reservoirs in a liner
that contains spills and leaks. Up to two EOs can be installed on top of the
DC. Each EO accommodates up to four 1-liter or 2-liter reservoirs or up to
two 4-liter reservoirs. The EO is typically ordered configured with four 2-liter
reservoirs (P/N 072058).
Setzen Sie den Eluentbehälter auf keinen Fall einem Druck über
0,07 MPa aus.
1 2 1 2
1 EGC (Capillary)
3 CR-TC (Capillary)
4 Leak Sensor
1
5 Drip Tray
Note:
For a capillary IC
3 system, the eluent
4 degasser is installed in
the IC Cube.
5 6
4 CR-TC (Analytical)
5 Drip Tray
6 5
Table 2-2 lists the versions of eluent generator cartridges available for use
with the EG. Each EGC contains an electrolyte concentrate solution
appropriate for the particular eluent generation. Each EGC is designed to be
used in either a capillary IC system or an analytical IC system. An EGC
designed for a capillary IC system cannot be used in an analytical IC system,
and vice versa.
Analytical IC systems require EGC III cartridges and (if used) the EPM III
Electrolytic pH Modifier. Previous versions of EGC or EPM are not
compatible with the Dionex ICS-5000 Eluent Generator.
For more information, refer to the EGC manual. The manual is included on
the Thermo Scientific Reference Library DVD (P/N 053891).
For more information, refer to the CR-TC manual. The manual is included on
the Thermo Scientific Reference Library DVD (P/N 053891).
For analytical IC systems, the EGC requires at least 14 MPa (2000 psi) of
system backpressure for removal of electrolysis gas from the eluent produced
by the cartridge. A system backpressure of 16 MPa (2300 psi) is ideal.
If necessary, increase the system backpressure by installing a backpressure
coil between the injection valve and the EGC OUTLET port. For details, refer
to Section 9.17.
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 adjusts the
eluent concentration to produce the carbonate/bicarbonate mixture. The
carbonate mixer provides mixing necessary to produce a homogenous
solution of electrolytically-generated K2CO3 and KHCO3 eluent.
For more information about these products, refer to the EGC manual. EGC
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).
Leak Sensor
If liquid collects in the drip tray in the bottom of the EG, a leak sensor reports
the leak to Chromeleon, and an error message is displayed in the Audit Trail.
In addition, the Alarm LED on the EG front panel lights.
Electrical Connections
1 1 Exhaust Fan
2
USB Receptacle
3 (“B” Connector)
8 Drain Port
7
Exhaust Fan
The exhaust fan cools the interior of the EG and exhausts any hydrogen and
oxygen gases that escape during operation.
USB Connections
• 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.
One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the EG Ship Kit
(P/N 072047).
The fuse cartridge contains two 2-amp slow-blow fuses (P/N 954773). For
instructions on how to change the fuses, see Section 9.18.
The rear panel power switch is the main power switch for the EG. Turn on the
main power switch before initial operation and leave it on unless instructed to
turn it off (for example, before performing a service procedure).
NOTE For routine on/off control, use the POWER button on the front
of the EG (see Figure 2-8). To turn off the EG, press and hold
the POWER button for 2 seconds.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the EG and is easily accessible.
Tubing Chase
The tubing chase routes tubing from the front of the EG, through the interior
of the module, and to the rear panel.
• 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 electrolysis gas (H2 or O2)
that is vented from the electrolyte reservoir of the EGC.
• The drain port removes any liquid that collects in the drip tray in the
bottom of the EG. A clear corrugated drain hose (P/N 055075) is
connected to this port during installation.
Place the free ends of the vent lines and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
EG.
For correct drainage, make sure the vent lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.
Vent
EGC
(Capillary)
EGC
IN
EGC
OUT
TO PUMP/DAMPER
WASTE, GAS
SEPARATOR
EG To CR-TC
Degas Regen Out
Cartridge (blue label)
(inside DC)
To CR-TC To CR-TC
ELUENT OUT
REGEN IN
REGEN OUT
EGC VENT
EGC
RFIC
Eluent
Degasser
Regen Regen
To Waste Out In
Eluent Eluent
Out In
Inlet Outlet
EGC
IN
EGC
TO PUMP OUT
Coupler
TO INJ VALVE - P
Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Regen In
TO CR -TC (orange label)
WASTE, GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
ELUENT OUT
To CR-TC
REGEN IN
Eluent In
(red label)
CR-TC
NOTE The VALVE 1 and VALVE 2 buttons can be enabled and dis-
abled in Chromeleon. When disabled, you can control the
valve only from the software. To enable or disable a button,
open the Commands dialog box (press the F8 key), select the
Advanced or Expert user level, and select the Valve1Button
(or Valve2Button) property in the list of properties for the
DC.
The front of the DC has two sample loading ports (see Figure 2-16) that can
be connected to injection valves installed inside the DC. A syringe can then be
used to manually load sample through the ports. For automated sample
Sample
Loading Ports
Figure 2-17 shows the upper compartments of a DC that is configured for two
capillary IC systems. Both systems are configured for conductivity detection.
1 3
2 4
1 2 3 4 Suppressor Cartridge
2 or Suppressor Bypass
Cartridge
4 EG Degas Cartridge
5 Injection Valve
contains the plumbing connections necessary for eluent and waste flow
through the system.
ELUENT IN
ELUENT IN REGEN OUT
ELUENT OUT
6 5 14
ELUENT IN
9 ELUENT OUT
7 To CR-TC
ELUENT OUT 2 Regen In Port
ELUENT OUT
4 ELUENT IN
8 3 EG
CRD 200 CES 300 DEGAS
The numbers on the schematic shown in Figure 2-20 indicate the flow path of
eluent and regenerant through the plumbing connections on an IC Cube
configured for electrochemical detection.
ELUENT IN
REGEN OUT
ELUENT OUT
5 10
6
ELUENT OUT
To CR-TC
ELUENT OUT 2 Regen In Port
4
CRD SUPPRESSOR
3 ELUENT IN EG
BYPASS BYPASS DEGAS
REGEN IN
From
Autosampler SAMPLE IN
1
9 SAMPLE OUT ELUENT IN
To Waste From CR-TC
Eluent Out Port
EC CELL
8 OUT
IN 7
Upper Compartment
1
Automation
1 Manager
Components
Electrochemical
2 Detector and Cell
3
2
Conductivity
3 Detector and
Suppressor
Lower Compartment
Columns and
4 4 Injection
Valves
The lower compartment can hold up to two column sets (four columns) with
IDs of 1 mm to 9 mm and lengths of 100 mm to 250 mm.
The lower compartment also holds one or two injection valves. Two valve
versions (6-port and 10-port) are available. Both versions are electrically-
activated, two position valves. See Section 2.13 for details about the injection
valves.
The compartment tray slides forward about 10 cm (4 in) for easy access to
columns and valves. To pull the tray forward, use the handle installed in the
center of the compartment (see Figure 2-22).
Internal Internal
Sample In Sample In
Loop Loop
S S
To To
5 5
Column Column
W 6 3 W 6 3
To 2 To 2
Waste Waste
= Sample = Eluent
• In the Load position, sample flows from the syringe or autosampler line
(if installed), through the valve, and into the internal sample loop, where
it is held until injection. Excess sample flows out to waste. Eluent flows
from the pump, through the valve, and to the column, bypassing the
sample loop.
• In the Inject position, eluent flows from the pump, through the internal
sample loop, and on to the column, carrying the contents of the sample
loop with it. Section 5.3.1 describes how to inject samples with an
autosampler and Section 5.3.2 describes how to inject samples manually.
Sample Sample
Sample In Sample In
Loop Loop
S L S L
To To
5 4 5 4
Column Column
W 6 3 W 6 3
To 1 2 To 1 2
Waste L Waste L
= Sample = Eluent
• In the Load position, sample flows from the syringe or autosampler line
(if installed), through the valve, and into the sample loop, where it is held
until injection. Excess sample flows out to waste. Eluent flows from the
pump, through the valve, and to the column, bypassing the sample loop.
• In the Inject position, eluent flows from the pump, through the sample
loop, and on to the column, carrying the contents of the sample loop with
it. Section 5.3.1 describes how to inject samples with an autosampler and
Section 5.3.2 describes how to inject samples manually.
A 10 L PEEK sample loop (P/N 042949) is installed between ports L (1) and
L (4). Thermo Fisher Scientific offers sample loops in various sizes. If
needed, the pre-installed 10 L loop can be replaced with a loop that has a
different sample injection volume.
NOTE Other plumbing configurations for the 10-port valve are pos-
sible, depending on the components to be connected to the
valve and the application to be run. Refer to the appropriate
Application Note for more information.
Concentrator Concentrator
To Column To Column
6
Eluent 6
Eluent
Pump In Pump In
8 7 5 4 8 7 5 4
Large 9 3 Large 9 3
Loop 1 Loop 1
10 2 10 2
To Waste To Waste
Sample Sample
In Carrier In Carrier
To Waste Pump In To Waste Pump In
Liquid flows through either the Load or Inject path, depending on the valve
position. For the example shown in Figure 2-26, the flow occurs as follows:
• In the Load position, sample flows from the syringe or autosampler line,
through the valve, and into the sample loop. Excess sample flows out to
waste. Eluent flows from the eluent pump, through the valve, through the
concentrator column, and to the separator column. If sample was
previously loaded onto the concentrator column, it is swept to the
separator column for analysis.
• In the Inject position, carrier liquid flows through the sample loop and on
to the concentrator column, carrying the contents of the sample loop with
it. Excess flows out to waste. Eluent flows from the pump, through the
valve, and to the separator column, bypassing the concentrator column.
Temperature Control
Temperature Compensation
2.14.2 Suppressor
The suppressor reduces the eluent conductivity and enhances the conductivity
of the sample ions, thereby increasing detection sensitivity. Installation of a
suppressor is optional.
The capillary and analytical CDs can operate with the following suppressors:
For details about any of the suppressors, including guidelines for selecting a
suppressor for your application, refer to the suppressor manuals. The manuals
are on the Thermo Scientific Reference Library DVD (P/N 053891).
Analytical IC Suppressor
Conductivity
1 Detector
3 1
Suppressor
2 (Optional)
(ASRS 300
2
model shown)
Suppressor
3
Cable
NOTE The basic flow path is the same for both capillary IC and ana-
lytical IC systems. However, in capillary IC systems, connec-
tions to components installed inside IC Cube cartridges
(columns, suppressor, and CRD) are not visible.
8 SUPPRESSOR
SEPARATOR COLUMN
GUARD 4
SAMPLE
TEMP
= Eluent Flow STABILIZER
S L
= Regenerant Flow
4
5 For analytical
W C IC only
6 3 3
1 2
L P
2 PUMP or
WASTE VALVE 1 ELUENT
(Inject Position) ELUENT IN GENERATOR
chamber. Flow is again routed through the CRD (if installed) 9 and then
to waste 10 .
Figure 2-29 illustrates the flow path through an EG and a DC for a
conductivity detection application using suppression in recycle mode.
DI WATER IN
FROM PUMP
1 7
9
SEPARATOR COLUMN
GUARD 6
SAMPLE 3
2 1 TEMP
= Eluent Flow VALVE STABILIZER
S L
= Regenerant Flow
4
5
W C For analytical
6 5 3
IC only.
1 2 4P
L ELUENT IN
WASTE (Inject Position)
• Deionized water from the pump 1 enters the EGC, which generates the
eluent. Eluent exits the EGC and passes through the CR-TC 2 (which
traps ionic contaminants), through the EG degas tubing, 3 and then into
the injection valve 4 .
• After sample is loaded into the sample loop 5 and the injection valve is
toggled to the Inject position, eluent passes through the loop.
Working
1 Electrode
Cell Body
3 2 (counter
2 electrode)
1
4 pH-Ag/AgCl
3 Reference
Electrode
Titanium Inlet
4 Tubing (for
analytical IC)
Cell Design
pH Dependence
2 Switched AC Sockets
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.
Switched AC Sockets
The two AC receptacles can be used to control the power to external devices.
Use Chromeleon to switch the power on and off. TTL inputs can also be used
to control the AC sockets (see Section 2.17.4).
The fuse holder contains two 10-amp slow-blow fuses (P/N 954772). For
instructions on how to change the fuses, see Section 9.22.
The rear panel power switch is the main power switch for the DC. Turn on the
main power switch before initial operation and leave the switch on unless
instructed to turn it off (for example, before performing a service procedure).
NOTE For routine on/off control, use the POWER button on the front
of the DC (see Figure 2-16). To turn off the DC, press and
hold the POWER button for 2 seconds.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the DC and is easily accessible.
USB Connections
The USB (Universal Serial Bus) receptacle (“B” type connector) allows
connection to the PC on which Chromeleon software is installed.
The two USB ports (“A” type connectors) allows connection to other USB
devices in the system (for example, the pump and eluent generator).
A 1.8 m (6 ft) USB cable (P/N 960777) is included in the DC Ship Kit
(P/N 072011).
If the I/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 to this
port during installation. Place the drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
DC.
For correct drainage, make sure the drain hose is not bent, pinched, or
elevated at any point. Do not allow the end of the hose to be submerged
in waste liquid.
2. For each I/O function to be used, connect an active wire (red) and a
ground wire (black) to the 12-position connector plug at the appropriate
pin locations. Refer to Figure 2-32 or the label on the DC rear panel for
the connector pin assignments.
To attach a wire to the plug, strip the end of the wire, insert it into the
plug, and use a screwdriver to tighten the locking screw. If necessary,
multiple ground wires can be attached to a single ground pin.
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.
5. If you connected a TTL input, verify that the correct function is assigned
to the input and that the correct input control type is selected. Select
different settings if necessary. Input functions and control types are
assigned from the Chromeleon 7 Instrument Configuration program or the
Chromeleon 6.8 Server Configuration program (see Section 2.17.4).
You can control the power, relays, and TTL outputs from the DC ePanel in
Chromeleon 7 (see Figure 2-36) or the DC Control panel in Chromeleon 6.8.
NOTE It is possible to change the settings for the power, relays, and
TTL outputs while a Chromeleon 7 instrument method or
Chromeleon 6.8 program is running.
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.
4. Select the name of the input and press the F2 key (or double-click the
name).
The Device Configuration dialog box for the selected input appears.
5. In the Control Functions list, select the check box of one or more
functions to be controlled by this input. When connected to a controlling
device, the device can send a signal to the input to trigger the selected
functions.
6. By default, several functions are selected. Scroll down the list and disable
all unwanted functions.
controlling device and the information below to determine the correct type.
Select the input control type in the Device Configuration dialog box for each
TTL input (see Figure 2-38).
• Normal Edge: In normal edge Action Off or No Effect
operation, the negative (falling)
TTL +5 V
edge of a signal turns on the NORMAL
function. EDGE
+0 V
RCH-1
Reaction Coil
High-Pressure High-Pressure
Valve #1 Valve #2
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:
In addition to the configurations described above, you can order the following
components separately for installation on an AM:
POSITION A POSITION B
5 4 5 4
6 3 6 3
1 2 1 2
POSITION A POSITION B
6 6
5 7
8 7 4 8 5 4
3 9
9 3
1 1
10 2 10 2
Note:
0 0 When the valve is
off (i.e., it is not
COM (N.O.) COM (N.O.)
energized), port 0 is
open (N.O.) and port
1 1 1 is closed (N.C.).
(N.C.) (N.C.) Conversely, when
the valve is on, port
1 is open and port 0
N.C. = normally closed
is closed.
N.O. = normally open
COM = common flow
For direct control of the heater, use the controls on the DC ePanel in
Chromeleon 7 or the Control panel in Chromeleon 6.8.
The applied voltage can be changed up to 10 times during the run. The actual
number of potential changes allowed depends on the available data storage
capacity, which is determined by the length of the run and the data sampling
rate.
For direct control, enter the potentials on the DC ePanel in Chromeleon 7 or
the Control panel in Chromeleon 6.8.
t2
+0.7
Delay Integration
Potential
(Volts)
+0.1
t1
-0.1
t3
E1. Detection Potential
E2. Positive Cleaning
0.0 0.2 0.4 0.6 Potential
Time (Seconds) E3. Negative Cleaning
E1 E2 E3 Potential
The potentials, labeled E1, E2, and E3, are applied for durations t1, t2, and t3,
respectively. At t1, the E1 potential is applied. After a delay, the signal is
measured by integrating the current for a fixed time. Current integrated for a
fixed time is charge and the units are coulombs. At t2 and t3, positive and
negative cleaning pulses are added to the waveform. This waveform period
repeats until the end of data acquisition or until another waveform is
specified.
+0.60
+0.35
Potential
(Volts)
-0.10
-0.60 Integration
With the example waveform shown in Figure 2-51, the current is integrated
both while the potential is swept across the metal oxide formation wave and
also during the reverse sweep across the oxide reduction wave. This technique
minimizes baseline shift and the peak dips that can occur when an eluting
analyte’s effect on oxide suppression is greater than the detector response
from the analyte.
As with pulsed amperometric detection, the waveform period repeats until the
end of data acquisition or until another waveform is specified.
2.19.4 Waveforms
A waveform is a series of steps, defined as points on a plot of potential vs.
time. Waveforms must be defined for the cyclic voltammetry and integrated
amperometry modes.
Cyclic voltammetry waveforms are defined by three points, each with a time
and a potential. The waveform forms a triangle, with the first point always at
time zero and the first and third points always having the same potential.
0.40
0.20
0.00
Volts 0.00 5.00 10.00 15.00 20.00 25.00 30.00
-0.20
-0.40
-0.60
In this example, the potential is scanned from -0.80 to +0.60 V and then from
+0.60 to -0.80 V. The total time for one waveform period is 28 s. This
provides a sweep rate of 0.1 V/s as shown in the equation below.
2 V - = Sweep Rate
-----------------------------------
CV Cycle Time
1.4 V = 0.1 V
2-------------------- ---
28s s
To view the Waveform Editor, click Edit on the ED Options page in the
Instrument Method Wizard (Chromeleon 7) or Program Wizard (Chromeleon
6.8).
E4
1.0
E2
0.0
Potential
(Volts) E1 E1
-1.0 Integration E3
-2.5
0.0 0.5 1.0 1.5 2.0
Time (Seconds)
time (in minutes) is on the x-axis and the detector response (in
nanoCoulombs) is on the y-axis.
0 5 10
Retention Time (Minutes)
Minutes
Sample Chromatogram
Injection Data Plot*
I-t Plot
3D Amperometry
(current vs.
Data Plot
waveform
time)
Waveform
Plot
In Chromeleon 6.8, the raw 3D amperometry data plot can be viewed as either
an Iso or a 3D (wireframe) plot. For both plot types, colors are used to
represent the ranges of response values.
The Iso view is the default view for the 3D raw data. This is a top down view
of the data (imagine you are looking down on the data from above the plot)
(see Figure 2-58). The x-axis is the retention time (min) and the y-axis is the
waveform period (ms). The z-axis, which is represented by different colors in
the plot, is the response (nA).
)
nA
e(
ns
po
res
x
retention time (min)
NOTE The 3D data shown in Figures 2-58 and 2-59 were collected
using an analytical waveform (see “Analytical vs. Scanning
Waveforms” on page 108).
To switch to the 3D plot view, right-click on the Iso plot, select Decoration
and click the Iso/3D Plot tab. The 3D view projects the response values in the
third dimension, which allows you to see the height of responses as well as the
colors representing different magnitudes of detection signal along the z-axis
(see Figure 2-59). For this view, imagine you are standing in front and slightly
to the left of the plot.
z y
s)
(m
response (nA)
e
ti m
m
or
ef
av
w
x
retention time (min)
Baseline Correction
2 3
4
5
6
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).
1 2 3
The rear panel power switch is the main power switch for the TC. Turn on the
main power switch before initial operation, and leave the switch on unless
instructed to turn it off (for example, before performing a service procedure).
NOTE For routine on/off control of the TC, use the POWER button
on the front of the module. To turn off the TC, press and hold
the POWER button for 2 seconds.
The fuse holder contains two 2-amp fuses (P/N 954776). For instructions on
how to change the fuses, see Section 9.33.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the TC and is easily accessible.
The two 6-pin mini-DIN connectors can be used to exchange digital signals
with any external device capable of being controlled through a relay or TTL
input. The two connectors are identical in function.
Relay_Com Relay_N.O.*
When the relay is activated, the connection is between Com and N.O.
Connection Description
Digital Input <---> Digital_GND 0 to +5 V
Relay_Com <---> Relay_N.O. Switching voltage: 100 VDC
Switching current: 0.25 A
Carry current: 1.0 A
Switching capacity: 3 W
Contact resistance: Max. 150 megohms
Use the 6-pin mini-DIN signal cable (P/N 6000.1004) provided in the TC
Ship Kit (P/N 064789) to connect the TC to an external device. For details
about the pin assignments, refer to Table 2-5.
USB Receptacle
The USB (Universal Serial Bus) receptacle (“B” type connector) provides a
connection to the PC on which Chromeleon is installed. Select one of the
following methods to establish the connection:
• Connect the TC directly to the USB receptacle on the PC.
• Connect the TC to the PC through another USB device in the system (for
example, the pump).
The TC Ship Kit (P/N 064789) includes a 1 m (3 ft) USB cable (P/N 063246).
Drain Port
The drain port removes any liquid that collects in the drip tray in the bottom
of the TC. A clear corrugated drain hose (P/N 055075) is connected to this
port during installation. Place the drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
TC.
For correct drainage, make sure the drain hose is not bent, pinched, or
elevated at any point. Do not allow the end of the hose to be submerged
in waste liquid.
To Waste To Waste
Sample In Sample In
W (6) W (6)
S (5) S (5)
L (4) L (4)
To Column To Column
From Pump From Pump
= Sample = Eluent
• In the Load position, sample is loaded into the sample loop, where it is
held until injection. Eluent flows from the pump, through the valve, and
to the column, bypassing the sample loop. Sample flows from the syringe
or autosampler line (if installed), through the valve, and into the sample
loop. Excess sample flows out to waste.
• In the Inject position, sample is swept to the column for analysis. Eluent
flows from the pump, through the sample loop, and on to the column,
carrying the contents of the sample loop with it. Section 5.3.1 describes
how to inject samples.
The 10-port injection valve has two operating positions: 10_1 and 1_2. Liquid
flows through the path between either ports 10 and 1 or ports 1 and 2,
depending on the valve position.
Figure 2-65 shows example flow schematics for the 10-port valve when it is
connected for an application that uses a concentrator column.
Concentrator Concentrator
To Column To Column
6 6
Eluent Eluent
5 Pump In 7 4 Pump In
7 4 5
8 8
9
Large 9 3 To Waste Large 3
Loop To Waste
10 1 Loop 1
10 2
2
= Sample
= Carrier
= Eluent
• In the 10_1 position, sample flows from the syringe or autosampler line,
through the valve, and into the sample loop. Excess sample flows out to
waste. Eluent flows from the eluent pump, through the valve, through the
concentrator column, and to the separator column. If sample was
previously loaded onto the concentrator column, it is swept to the
separator column for analysis.
• In the 1_2 position, carrier liquid flows through the sample loop and on to
the concentrator column, carrying the contents of the sample loop with it.
Excess flows out to waste. Eluent flows from the pump, through the
valve, and to the separator column, bypassing the concentrator column.
(Green)
TO INJECT SAMPLE IN
VALVE -W (from door
inject port or
autosampler)
W (6)
S (5)
25 μL SAMPLE LOOP
(Orange) L (4)
TO INJECT
VALVE -P TO INJ (Red - microbore)
VALVE -C (Black - standard bore)
Column Properties
Follow these steps to change the sensitivity setting of the gas or humidity
sensor, or to turn off a sensor:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Select the TC.
4. If you are using Chromeleon 7: Click the Parameters tab page for the
TC, click the GasLeakSensor or HumidityLeakSensor parameter.
Select the new sensitivity setting (or select Off to disable the sensor).
5. If you are using Chromeleon 6.8, click the plus sign beside TC to display
the items underneath. Under TC_Temp, select the GasLeakSensor or
The temperature achieved may vary from the control range, depending on the
ambient temperature (see the table below).
For example, if the ambient air temperature in the lab is 30 °C and you set the
temperature to 5 °C, the actual temperature achieved will be about 12 °C.
Do not touch any metal parts inside the TC while it is heating up or after
it reaches the set point temperature. Wait for the compartment to cool
down before servicing any parts.
3.1 Overview
This chapter provides example component and plumbing drawings for the
following Dionex ICS-5000 system configurations:
To pump #2 inlet via the pump rear chase Pump (front view)
System #2
To EGC
#2 In Piston
Seal
Wash
System #1
Deionized Deionized
Water Water
To EGC
#1 In To waste
System #1 System #2
From
autosampler
To waste
To waste
From IC Cube #1
EG Degas Regen Out Regen Out
Regen Out
Regen In Regen In
To waste
To waste
System #2
To waste
(pump not to scale)
To EGC
#2 In Piston
Seal
Wash
System #1
Deionized Deionized
Water Water
To waste
To EGC
#1 In
From IC Cube #2 EG Degas Regen Out
DC (front view) To IC Cube #2 EG Degas Eluent In
ELUENT IN
EG EG
System #1
ELUENT IN
System #1 System #2
From
autosampler
To waste
To waste
From IC Cube #1
EG Degas Regen Out Regen Out
Regen Out
Regen In Regen In
To waste
To waste
To pump #2 inlet via the pump rear chase Pump (front view)
System #2
To EGC
#2 In
(pump not to scale) To waste
A
Piston B
Seal C
Wash
System #1 D
Deionized Deionized
A B
Water Water
D C
Mixer To waste
To EGC #1 In
From the suppressor Regen Out via the DC rear chase
From the IC Cube EG Degas Regen Out
DC (front view) To the IC Cube EG Degas Eluent In
ELUENT IN
EG EG
ELUENT IN
ELUENT OUT
REGEN OUT
(left side view) System #1 System #2 (right side view)
ELUENT IN
ELUENT OUT
ELUENT OUT
ELUENT OUT
ELUENT IN EG
DEGAS
From autosampler CRD 200 CES 300
To waste
ELUENT OUT REGEN IN EGC
SAMPLE IN
Regen
Out Regen Out
In Out Eluent
Eluent
Out
ELUENT OUT
System #1 In
REGEN IN
Regen In
Separator
Regen In
CR-TC Eluent In Eluent
Guard
(5) S L (4) Out
Temp .
Stabilizer W C
(6) (3) Backpressure
Device To the degasser Regen In via the EG rear chase
From autosampler
(1) L P (2) To waste
To waste
To waste
Figure 3-3. Hybrid System: Dual RFIC-EG System (CD Analytical/CD Capillary)
Eluent
Seal
Wash
Pump
Eluent In Regen In
Piston
Seal
Wash
Pump inlet
Separator
Guard
(5) S L (4)
Temp.
Stabilizer W C
(6) (3)
Mixer On/Off Valve
(1) L P (2)
From AS
To waste
To AS/Waste
Piston
Seal
Pump inlet
Wash
Deionized
Water
On/Off
Mixer
Valve
To waste
From the suppressor Regen Out via the DC rear chase
DC (front view)
EG
(left side view)
EGC
Regen Regen
Cell In Cell Out Out In
ELUENT OUT
In
REGEN IN
Separator
Regen In
Guard CR-TC
(5) S L (4)
Temp .
Stabilizer W C
(6) (3) Backpressure
Device
(1) L P (2) To the degasser Regen In via the EG rear chase
From AS
To AS /Waste
To Waste
To pump #2 inlet via the pump rear chase Pump (front view)
A
To pump #1 inlet via the pump rear chase Seal B
Wash
Pump C
D
System #2 A B
D C
Mixer
To waste
(pump not to scale)
A
Piston B
Seal C
System #1 Wash D
Deionized Deionized
Water Water A B
Mixer D C
To waste
From suppressor #1 Regen Out via the DC rear chase From suppressor #2 Regen Out via the DC rear chase
DC (front view)
EG EG
(left side view) (right side view)
System #1 System #2
Cell In
Regen Regen Regen Regen
Cell Out Cell In Cell Out
Out In Out In
Regen Out Eluent Out Regen Out Eluent Out Eluent Eluent Eluent Eluent
Out In Out In
Eluent In Regen In Eluent In Regen In
Regen
Regen To inject valve
Out #2 port P (2)
Eluent Eluent Out Eluent
In Out Out In Out
ELUENT OUT
In Out
REGEN IN
ELUENT OUT
REGEN IN
Separator #2
Separator #1
Regen In Eluent
Guard #2 Guard #1 Regen In
Backpressure Device
In
CR-TC CR-TC
(5) S L (4) (5) S L (4)
Temp. Temp.
Stabilizer W C W C Stabilizer
(6) (3) From AS (6) (3)
To the degasser #1 Regen In via the EG rear chase
From AS (1) L P (2) To AS /Waste (1) L P (2) To waste
To AS /Waste Backpressure Device
To pump #2 inlet via the pump rear chase Pump (front view)
To pump #1 inlet via the pump rear chase A
Seal B
Wash
Pump C
D
System #2 A B
Mixer
Mixing D C
Chamber
To waste
(pump not to scale)
A
Piston B
Seal
C
Wash
System #1 D
Deionized
Eluent
Water A B
Mixing
Mixer D C
Chamber
To waste
ELUENT OUT
ELUENT OUT
In
REGEN IN
Separator #2
REGEN IN
In
Separator #1 To inject
valve #1 Eluent Eluent
Regen In Regen In
Out
Backpressure Device
Seal
Pump inlet
Wash
Pump
Pump #2
On/Off
Mixer Valve
To waste
(pump not to scale)
A
Piston B
Seal C
Wash D
Pump #1
Deionized Deionized
Water Water
(carrier) A B
Mixer D C
To waste
From the suppressor Regen Out via the DC rear chase
DC (front view)
EG
(left side view)
5 4
3 Large Loop
6
1 2
From AS
To AS/Waste
EGC
ELUENT OUT
In
REGEN IN
Separator Eluent
Regen In Out
Guard CR-TC
(5) S L (4)
Temp .
Stabilizer W C
(6) (3)
Backpressure
(1) L P (2) Device To the degasser Regen In via the EG rear chase
To AS /Waste
To Waste
Figure 3-8. Analytical IC: Single RFIC-EG System with Matrix Elimination Using a DP and a 6-Port Valve
Pump inlet
Wash
Concentrator Pump
To column
Pump #2
Sample in 6 Eluent in
On/Off
Mixer Valve
7 5 To waste
8 4
9 (pump not to scale)
1 3 To waste
10 A
2 Piston B
Seal
Carrier pump in Wash
C
D
To waste Pump #1
Deionized Deionized
Water Water
(carrier) A B
Mixer D C
To waste
From the suppressor Regen Out via the DC rear chase
DC (front view)
EG
(left side view)
EGC
ELUENT OUT
In
REGEN IN
Separator
Regen In Eluent
Out
Guard CR-TC
6
7 5
8 4
Concentrator
9 3
1 Backpressure Device
10 2 To the degasser Regen In via the EG rear chase
From AS
Large Loop
To AS /Waste
To Waste
Figure 3-9. Analytical IC: Single RFIC-EG System with Matrix Elimination Using an SP and a 10-Port Valve
138 Doc. 065342-06 12/11
3 • Configurations
Pump inlet
Wash
via the DC rear chase
Pump
Pump #2
On/Off
Mixer Valve
To waste
(pump not to scale)
A
Piston B
Seal C
Wash D
Deionized To the
Water
Deionized Pump #1
Reagent absorbance
Water
(Regen) or PDA
detector A B
Mixer D C
From the suppressor Regen Out via the DC rear chase To waste
DC (front view)
plug EG
Reagent in M N.O. M
CO N.O.
(left side view)
CO
from pump #2 N.C. N.C.
RCH-1
EGC
To waste
ELUENT OUT
In
REGEN IN
Separator Eluent
Regen In Out
CR-TC
(5) S L (4) Guard
Temp.
Stabilizer W C
(6) (3)
Backpressure
From AS
(1) L P (2) To the degasser Regen In via the EG rear chase
Device
To AS /Waste
To Waste
Figure 3-10. Analytical IC: Single RFIC-EG System with Post-Column Reagent Addition (Bromate)
DC (front view)
EG
(left side view)
Regen Regen
Out In
Eluent Eluent
To the CR -TC Regen In Out In
Regen
Out
In Out Eluent Eluent
Out Plu
ELUENT OUT
In
REGEN IN
CarboPac PA20
Regen In
CR-TC
(5) S L (4)
Temp . Amino Trap or PA 20 Guard
Stabilizer W C
(6) (3) Backpressure
Device
(1) L P (2) To the CR-TC Regen In via the EG rear chase
From AS From the degasser Eluent Out
To AS /Waste
To Waste
Figure 3-11. Analytical IC: Single RFIC-EG System with ED and VP (for Carbohydrate Analysis)
This section is an overview of the steps required to start up the Dionex ICS-
5000 system components and prepare the system to run samples. The
operating parameters (flow rate, compartment temperature, suppressor
current, etc.) depend on the application you plan to run. Refer to the column
manual, as well as the schematics in Chapter 3 of this manual, for the required
operating parameters.
If you select a low flow rate that allows the system pressure to drop below
14 MPa (2000 psi) and you do not turn off the EG, the EG will continue to
generate eluent at the concentration set for the last step of the last Chromeleon
7 instrument method or Chromeleon 6.8 program.
If this occurs, the eluent concentration will increase in proportion to the
decrease in the flow rate. In extreme cases, excessive heat buildup can occur
and damage the EGC.
For a complete list of operating precautions for EGCs and CR-TC trap
columns, refer to the product manuals. The manuals are provided on the
Thermo Scientific Reference Library DVD (P/N 053891).
You can set upper and lower pH limits in the Chromeleon 7 Instrument
Method Wizard (see Figure 4-2) or Chromeleon 6.8 Program Wizard. The
Audit Trail displays an alarm if the limits are exceeded.
NOTE To disable the alarm, set the upper limit to 14 and the lower
limit to 0.
NOTE You can use the Smart Startup feature in Chromeleon to auto-
mate system startup and equilibration. Refer to the Chrome-
leon Help for details.
4.3.4 Filling the Autosampler Vials and Loading the Sample Tray
Follow the instructions in the autosampler manual to fill the vials or well
plates and load them into the sample tray or carousel. The autosampler
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).
Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water to remove any loose
particles.
5. Install an end-line filter on the end of each reservoir’s eluent line.
6. Install the reservoir caps, making sure the end of each line extends to the
bottom of the reservoir, and that each filter is submerged in liquid. This
prevents air from being drawn through the eluent lines. Hand-tighten the
caps.
The standard piston seal wash system is designed for use with only one of the
two pumps in a DP module. When the DP is shipped from Thermo Fisher
Scientific, the seal wash system is connected to pump 1 (the bottom pump). If
you want to connect the seal wash system to pump 2 (the top pump), follow
the instructions in this section.
NOTE For users who need to operate a piston seal wash system for
both pumps in the DP, Thermo Fisher Scientific offers an
External Seal Wash Kit (P/N 063518) or a second seal wash
system (P/N 068661).
1. Note the tubing connected from the peristaltic pump to the seal wash tube
on the secondary pump head on pump 1 (see Figure 4-5, item 1 ).
Disconnect this tubing from the pump head and connect it to the seal wash
tube on the secondary pump head on pump 2.
Connection from
peristaltic pump to
1 secondary pump
head
Connection between
4 2 pump heads
2. Disconnect the short piece of tubing between the primary and secondary
pump heads on pump 1 (see Figure 4-5, item 2 ). 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 3 ). 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.
1. Add ASTM Type I (18 megohm-cm) filtered and deionized water that
meets the specifications listed in Section 1.5 to the seal wash reservoir
(P/N 064155).
The liquid level should be between the Min. and Max. markers on the
reservoir label. Do not overfill the reservoir.
2. Place the cap on the reservoir and tighten fingertight.
3. Insert the reservoir into the holder on the component panel.
4. Check that the tubing is engaged in the peristaltic pump (see Figure 4-6).
If it is not, lift the lever on the peristaltic pump up and to the right, insert
the tubing neatly between the lever and the rotor, and release the lever to
secure the tubing.
Tubing to
Secondary
Pump Head Lever
Outlet Tubing
from Seal Wash
Reservoir
Rotor
Figure 4-7. Setting the Pump Flow Rate and Pressure Limits
(Chromeleon 7 Version Shown)
4. Enter the Flow rate required for your application. This starts the pump
flow, also.
5. If the preferred flow rate is already selected, but the pump flow is off,
click the switch to start the pump at the selected flow rate.
NOTE After starting the pump or changing the flow rate, wait
at least 5 minutes (longer for flow rates below
1.0 mL/min) before beginning an analysis. This allows
the DP/SP to stabilize the flow rate.
6. Enter the minimum and maximum pressure limits. Setting pressure limits
ensures that the DP/SP will automatically stop if a system malfunction
occurs. Table 4-1 lists the default pressure limits for capillary and
analytical pumps.
Capillary IMPORTANT
IC
Capillary IC pumps shipped before February 17, 2011 were rated for lower
operating pressures than the pumps currently being shipped. The older
pumps can be operated at pressures up to 35 MPa (5000 psi) (without
RFIC) and up to 21 MPa (3000 psi) (with RFIC). Before operating at
pressures above these limits, verify that you have the appropriate pump.
• HPC is stamped on the secondary
pump heads of the older (lower
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 an EGC III K2CO3 and an EPM III Electrolytic pH Modifier are installed
(EGC_1 and EGC_2, respectively):
1. Set EGC_1 Target Concentration to the concentration of K2CO3
required for your application
2. Set EGC_2 Target 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 field for the K2CO3 EGC). The EPM modifies the 4.50 mM
K2CO3 eluent to achieve the required 3.50 mM K2CO3/1.00 mM KHCO3
mixture.
4. Offset the detector background and zero the reading by clicking the
Autozero button.
5. Verify that the detector baseline is at the expected reading for your
application and is stable. See Section 8.11 for troubleshooting
information if the reading is too high. See Section 8.2 for troubleshooting
information if the baseline is drifting or is excessively “noisy” (there are
large fluctuations in readings).
6. Monitor the DP/SP pressure and make sure it is at the expected reading
for the installed column and it is stable.
7. Verify that all installed temperature control devices are at their set points
and are stable.
The system is now ready for operation.
Capillary Because capillary IC systems use low flow rates and consume very little
IC eluent, you can leave a capillary IC system on at all times, allowing it to
remain equilibrated and always ready to run the next sample.
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 control.
1. On the ePanel Set or panel tabset, click the tab for the module.
2. Use the controls (buttons, sliders, etc.) on the panel to issue commands.
3. If the function that you want to perform is not available from the panel,
press the F8 key to open the Commands dialog box. You can access all
commands available for the system from this dialog box.
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
details about an eWorkflow Wizard page, click the Help icon .
4. After you finish the eWorkflow Wizard, the sequence is displayed in the
Console Data view (see Figure 5-3).
NOTE If preferred, you can create the sequence first and then
specify the methods and report template later. You can
also edit other details of the sequence (for example,
add or remove samples) after you finish the wizard.
3. After you finish the wizard, the new sequence is displayed in the Console
Data view (see Figure 5-3).
1. On the Sequence Control panel in the Chromeleon 6.8 panel tabset, click
Create Sequence (see Figure 5-4).
NOTE If preferred, you can create the sequence first and then
specify the program and quantitation method later.
You can also edit other details of the sequence (for
example, add or remove samples) after you finish the
wizard.
3. After you finish the Sequence Wizard, the new sequence is displayed in
the Chromeleon 6.8 Browser.
3. Click Next> and select the 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
method appropriate for the selected application are copied to the
sequence.
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).
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
to the sample port on the injection valve. If not, refer to Section 9.20 for
connection instructions.
2. Fill a syringe with a calibration standard or sample.
3. Insert the syringe into the sample loading port on the front of the DC.
4. Verify that the injection valve is in the Load position. If it is not, switch
the valve by clicking the valve control on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset, or by pressing the VALVE button on the
front of the DC.
5. Overfill the sample loop with several sample loop volumes. Excess
sample will exit through the injection valve waste line.
6. Leave the syringe in the port. This prevents the sample from exiting the
loop before injection.
7. Switch the injection valve to the Inject position.
Sample Port
g e
Syrin
W C
(6) (3)
(1) L P (2)
Valve
Sample
Figure 5-9 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS-AP Autosampler.
Figure 5-9. Commands for Loading and Injecting a Sample with a Dionex
AS-AP (Chromeleon 7 Script Editor Shown)
Figure 5-10 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS-DV Autosampler.
Figure 5-10. Commands for Loading and Injecting Sample with a Dionex
AS-DV (Chromeleon 7 Script Editor Shown)
Figure 5-11 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS Autosampler.
Figure 5-11. Commands for Loading and Injecting a Sample with a Dionex
AS (Chromeleon 7 Script Editor Shown)
ICS-5000
DP/SP DP/SP Shutdown
If the Dionex ICS-5000 Dual Pump (DP) or Dionex ICS-5000 Single Pump
(SP) will not be operated for a period of one week or more, follow the
instructions below:
• Fill the pump with methanol (or a similar alcohol, such as 2-propanol or
ethanol). If the eluents in the pump are not miscible with water, replace
the eluents step-by-step.
• Fill the seal wash reservoir 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).
Tubing
Rotor
Lever
2. Verify that the current to the EGC and the suppressor is off.
Supplying power to the EGC when there is no eluent flow can severely
damage the cartridge.
3. If you plan to store the EGC in the EG, no further action is required.
If you plan to store the cartridge outside the EG (for example, in the
original shipping container), follow the instructions in Section 9.14.1, to
remove the EGC from the EG, and the instructions in Section 9.14.3, to
store the EGC.
To restart the EG:
1. Select the parameters for the analysis on the Chromeleon 7 ePanel Set or
the Chromeleon 6.8 panel tabset. For EG startup information, see
Section 4.9.
2. Condition the EGC. For instructions, see “Conditioning the Capillary
EGC” on page 343 or “Conditioning the Analytical EGC” on page 348.
3. Hydrate the CR-TC (see “Installing and Flushing the New CR-TC” on
page 350).
4. Hydrate the 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.
1. Follow the instructions in Section 9.14.1, to remove the EGC from the
EG.
2. 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.
Make sure the EGC packaging conforms to hazardous material
shipping requirements. Refer to the Material Safety Data Sheet (MSDS)
shipped with the EGC for the chemical description.
5. Make sure there is no air bubble in the cap. Add more KCl solution if
needed.
Storage
Cap
This section describes routine maintenance procedures for the Dionex ICS-
5000 system that users may perform. All other maintenance procedures must
be performed by Thermo Fisher Scientific personnel.
For information about maintenance procedures for the EGC, CR-TC trap
column, or suppressor, refer to the appropriate product manual. These
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).
This section describes routine maintenance procedures that users may perform
for the Dionex ICS-5000 Dual Pump (DP) or Dionex ICS-5000 Single Pump
(SP). All other maintenance procedures must be performed by Thermo Fisher
Scientific personnel.
Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5 to remove any loose particles.
• Replace the seal wash solution. ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5 is
appropriate for most applications.
• Check the tubing connected to the peristaltic pump. If the tubing is
blocked or crimped, replace it (see Section 9.9).
Capillary • Check the liquid level in each eluent reservoir and refill as required.
IC
This section describes routine maintenance procedures for the Dionex ICS-
5000 Eluent Generator (EG) that users may perform. All other maintenance
procedures must be performed by Thermo Fisher Scientific personnel.
For information about maintenance procedures for the EGC, CR-TC trap
column, or suppressor, refer to the appropriate product manual. These
manuals are included on the Thermo Scientific Reference Library DVD
(P/N 053891).
This section describes routine maintenance procedures for the Dionex ICS-
5000 Detector/Chromatography Module (DC) that users may perform. All
other maintenance procedures must be performed by Thermo Fisher Scientific
personnel.
NOTE If you are using an electrochemical detector, also see the spe-
cial maintenance considerations that are described in
Section 4.1.2.
This section describes routine maintenance procedures for the Dionex ICS-
5000 Thermal Compartment (TC) that users may perform. All other
maintenance procedures must be performed by Thermo Fisher Scientific
personnel.
• Check for excess condensation inside the TC. Condensation may build up
when the TC is operated in a highly humid environment and the majority
of applications are run at cold temperatures. To remove condensation, run
the TC at its maximum temperature for at least 72 hours.
Some IC columns should not be operated at temperatures above 70 °C
(158 °F). Remove all columns from the TC before beginning the
maintenance procedure above.
• Inspect the door seal for signs of damage. A defective seal impairs the
performance of the instrument. If the seal is defective, contact Technical
Support for Dionex products.
This chapter is a guide to troubleshooting minor issues that may arise during
operation of the Dionex ICS-5000 system. Turn to the section of this chapter
that best describes the operating problem or symptom that has been observed.
Each section lists possible causes of the problem or symptom in order of
probability. A systematic troubleshooting approach is the most effective way
to determine the root cause.
If you are unable to resolve a problem by following the instructions here,
contact Technical Support for Dionex products. In the U.S. and Canada, call
1-800-346-6390. Outside the U.S. and Canada, call the nearest Thermo Fisher
Scientific office. Please have this chapter at hand when talking with Technical
Support personnel.
5. Prepare fresh eluent. To ensure eluent purity, prepare all eluents with
spectro-grade eluents, reagent-grade chemicals, and ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5.
• DP/SP not properly primed
Prime the pump (see Section 9.5).
• Piston seal is damaged
If the piston seal is damaged, it allows liquid leaks. Leaks are usually
visible, and thus easily detected. If necessary, replace the piston seal (see
Section 9.7).
• Inadequate system or cell backpressure
Add backpressure tubing to the cell outlet (see Section 9.27.4) or to the
pump (if no column is installed).
• (Analytical EG only) System backpressure is below 14 MPa (2000 psi)
The optimal system backpressure is 16 MPa (2300 psi) in an analytical IC
system with an EG installed,. Low system backpressure may cause high
baseline noise as the eluent concentration increases in the gradient. To
correct this, install a backpressure coil in the EG after the RFIC Eluent
Degasser (see Section 9.17).
• Flow system leak ahead of cell
Check all fittings and liquid lines for leaks. Tighten or, if necessary,
replace all liquid line connections (see Section 9.19).
• Rapid changes in ambient temperature
Make sure the column is installed in a thermostatically controlled
compartment and the compartment door is closed.
• Insufficient system equilibration following changes to operating
parameters; especially apparent when operating at high sensitivities
Allow a longer system equilibration time (up to 2 hours) before starting
operation.
3 seconds. Repeat two or three times. If the baseline does not improve,
check the other causes of baseline instability described in this section.
Do not block the end of the cell outlet tubing for longer than the
recommended 2 to 3 seconds. Doing so creates high backpressure,
which can break the pH-Ag/AgCl reference electrode glass membrane.
NOTE To prevent air from becoming trapped in the cell in the future,
increase the backpressure on the cell by 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.
Repeat two or three times. If the baseline does not improve, check the
other causes of baseline instability described in this section.
Do not block the end of the cell outlet tubing for longer than the
recommended 2 to 3 seconds. Doing so creates high backpressure,
which can break the pH-Ag/AgCl reference electrode glass membrane.
3. The water used to prepare the eluent may contain trace contaminants.
Remake the eluent, using ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
8.6 No Peaks
• EG power is not turned on
1. Check that the POWER button on the front of the EG is turned on.
2. Check that the EG main power switch (on the rear panel) is turned on.
3. Check that the main power cord is plugged into both the EG rear
panel connector and the power source. Check that the wall outlet has
power.
• Injection valve is not actuating or the sample loop is plugged
1. Test the valve by manually switching the position from the DC ePanel
in Chromeleon 7 or Control panel in Chromeleon 6.8.
2. Check the sample loop for blockage. Clean or replace the loop if
needed.
• Detector not properly installed
CD: An electronics connector on the back of the detector plugs into a
receptacle on the detector compartment. Push on the detector to make
certain the connector is securely connected (see Figure 8-1).
• ED: Verify that the signal cables from the cell are connected to the
detector block. In addition, an electronics connector on the back of the
detector plugs into a receptacle on the detector compartment. Push on the
detector to make certain the connector is securely connected (see
Figure 8-1).
ED Only
• Cell is off
Turn on the cell from the detector ePanel (in Chromeleon 7) or Control
panel (in Chromeleon 6.8).
ED Only
CD Only
ED Only
If this error occurs, the tubing between the pump heads may be blocked or the
fitting may be overtightened.
To troubleshoot:
Inspect the tubing for blockage or crimping and replace if needed (see
Section 9.3). Be careful to not overtighten fittings. If the message appears
again, contact Technical Support for Dionex products for assistance.
Degasser malfunction.
This error occurs if the drive current is above the allowed value. When this
message appears, the DP/SP stops running.
To troubleshoot:
One or more tubing connections may be plugged, blocked, or crimped. Check
all tubing connections and replace as needed (see Section 9.3). Be careful not
to overtighten fittings.
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
enclosure. When this error occurs, the pump stops running.
To troubleshoot:
To find and eliminate the source of the leak, see Section 8.15.
This error occurs if the pressure in the primary pump head exceeds the
maximum allowed. (“Right-hand” refers to the bottom pump; “left-hand”
refers to the top pump in a dual-pump module.)
To troubleshoot:
1. Make sure that the tubing between the pump heads and the tubing leading
to the priming/outlet block is not plugged or blocked. Replace tubing
connections as needed (see Section 9.3). Be careful not to overtighten
fittings.
2. Inspect the outlet check valve for blockage. Replace the check valve
cartridge if needed (see Section 9.6).
Motor malfunction.
This error occurs if an internal error in the pump drive mechanism occurs.
To troubleshoot:
Turn off the DP/SP power for 30 seconds, and then turn on the power again. If
the error message appears again, contact Technical Support for Dionex
products for assistance.
This error occurs if the DP/SP pressure falls below the low pressure limit
specified in Chromeleon.
To troubleshoot:
1. The eluent supply may be depleted. Check the Eluent Level Display on
the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset to verify
that eluent is present in the selected channel. If the eluent reservoir is
empty, refill it (or select a channel that does have eluent). Prime the pump
before resuming operation (see Section 9.5).
2. Check all eluent lines for air bubbles. If air is trapped in a line, replace the
end-line filter (P/N 045987). See Section 4.6 for instructions. Verify that
the end of each filter extends to the bottom of the reservoir and is
submerged in eluent. Prime the pump (see Section 9.5).
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 priming valve is closed (see Figure 2-3). To close the
valve, turn the knob clockwise until closed. Tighten no more than
fingertight.
Do not use any tools to tighten the priming valve! Overtightening may
destroy the cap seal. Open or close the priming valve only when the
system pressure is down.
6. A check valve may be defective. Replace the check valve cartridges (see
Section 9.6) and then prime the pump (see Section 9.5).
If the DP/SP pressure exceeds 5 MPa (725 psi) during priming, this error
occurs and the priming process is aborted.
To troubleshoot:
1. Verify that the priming valve is open. (To open the valve, turn the knob
one-half turn counterclockwise.)
2. Check fittings for overtightening. Check tubing for crimping and replace
it as necessary (see Section 9.3). Be careful not to overtighten fittings.
4. Observe a run to see whether the high pressure limit is triggered when
injection occurs; if it is, the injection valve may be the source of the
blockage (i.e., the rotor seal or stator may need to be replaced). Contact
Technical Support for Dionex products for assistance.
This error occurs if you attempt to change a parameter that users are not
allowed to adjust.
To troubleshoot:
Only Thermo Fisher Scientific Service Representatives can change this
parameter.
This error occurs if the upper pressure limit specified in the program is
exceeded. The running batch is aborted (default) and this message appears.
To troubleshoot:
1. Inspect the tubing for blockage or crimping; replace as needed (see
Section 9.3). Be careful not to overtighten fittings.
2. To determine the source of the high backpressure, isolate segments of the
flow path:
a. Remove the pump outlet tubing at the injection valve.
b. Press the POWER button on the front of the DP/SP to turn on the
pump.
c. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, set
the Flow rate to 0.01 mL/min for a capillary IC system or 1.0 mL/min
for an analytical IC system and record the backpressure.
d. Disconnect all components after the injection valve.
e. One at a time, reconnect each component of the flow path. If
reconnecting a component causes an abnormal increase in
backpressure, replace the component. Replace as many components
The allowable eluent concentration depends on the flow rate and the EGC
type. This message appears if the selected eluent concentration is out-of-range
for the flow rate. The time indicated in the message refers to the time
specified in the Chromeleon 7 instrument method or Chromeleon 6.8
program.
To troubleshoot:
Check the information in Section 4.10 to verify that the selected concentration
is within the accepted range for the cartridge type and flow rate. Adjust the
flow rate or concentration as needed.
To troubleshoot:
1. Check that the CR-TC is correctly plugged into the EG. Push the CR-TC
electrical cable firmly into the CR-TC 1 (or CR-TC 2) bulkhead connector.
Twist the ring on the cable connector fingertight to secure it.
2. If the error persists, the CR-TC may be faulty. Replace the CR-TC (see
Section 9.15).
This error occurs when the current applied to the CR-TC exceeds the
maximum current allowed. (The CR-TC current is automatically turned off to
prevent damage to the CR-TC.) This error may also occur if liquid flow to the
CR-TC is interrupted.
To troubleshoot:
1. Check the CR-TC cable connection to the electrical bulkhead (see
Figure 2-10).
2. Refer to Section 8.23 to determine why liquid flow stopped.
3. If the error message appears again, contact Technical Support for Dionex
products for assistance. The CR-TC control electronics may have
malfunctioned.
This error occurs if you attempt to turn on the CR-TC when the EGC is turned
off. The CR-TC current is automatically turned off to prevent damage to the
CR-TC.
To troubleshoot:
Verify that the pump flow and the EGC are on before turning on the CR-TC.
This error occurs if you turn off the pump flow while the EGC current (and
CR-TC) are on. The CR-TC current is automatically turned off to prevent
damage to the CR-TC.
To troubleshoot:
If the pump stopped unexpectedly, follow the troubleshooting steps in
Section 8.23.
This error occurs when a “live” EG is linked to a virtual pump and you try to
turn on the CR-TC. The mode is automatically turned off to ensure that the
EG does not operate when there is no flow.
CR-TC mode will be turned off for invalid flow. Flow range for
analytical EGC: 0.100 – 3.000 mL/min, capillary EGC: 0.001 –
0.100 mL/min.
This error occurs when the flow to the CR-TC is out of range or there is no
pumped linked to the EGC.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.
2. Check the EGC configuration properties in the Chromeleon 7 Instrument
Controller Service or the Chromeleon 6.8 Server Configuration program
to verify that the pump and EGC are linked.
This error occurs if the type of pump linked to the EGC does not match the
EGC type. A capillary EGC can only be used with a capillary pump and an
analytical EGC can only be used with an analytical pump.
To troubleshoot:
1. Install the correct type of EGC for the pump type.
2. For a hybrid system (a dual system with both an analytical and a capillary
pump), check the EGC configuration properties in the Chromeleon 7
Instrument Controller Service or the Chromeleon 6.8 Server
Configuration program to verify that the correct pump is linked to the
EGC.
This error occurs if the activation date for the EGC is not a valid date. This
may indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.
This error occurs if the eluent concentration is outside the range allowed by
the EG. This may indicate corrupted memory or a problem in the EG
instrument control firmware.
To troubleshoot:
Contact Technical Support for Dionex products for assistance.
This error occurs if the flow rate is set to a value the EG does not support.
To troubleshoot:
Set the flow rate to a value within the allowed range. Refer to Appendix A for
flow rate specifications.
This error occurs if the selected concentration is too high for the current flow
rate.
To troubleshoot:
Set the flow rate to a value within the allowed range. The allowable eluent
concentration for a particular application depends on several factors: the flow
rate, suppressor type, EGC type, and cartridge configuration. For details, refer
to Section 4.9.
This error occurs if the ion count reported by the EGC is invalid. This may
indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.
This error occurs if the serial number reported by the EGC is invalid. This
may indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.
This error occurs when the current applied to the EGC exceeds the maximum
current allowed. (The EGC current is automatically turned off to prevent
damage to the cartridge.) This error may also occur if the liquid flow to the
cartridge is interrupted.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. Refer to Section 8.23 to determine why there is no flow.
3. If the error message appears again, contact Technical Support for Dionex
products for assistance. The cartridge control electronics may have
malfunctioned.
This error occurs when, in order to maintain the selected current, the power
supply is required to supply a higher voltage than the EGC can support.
To troubleshoot:
Replace the EGC (see Section 9.14).
This error occurs when the current applied to the EGC exceeds the maximum
current allowed. (The EGC current is automatically turned off to prevent
damage to the cartridge.) This error may also occur if the liquid flow to the
cartridge is interrupted.
To troubleshoot:
1. Refer to Section 8.23 to determine why there is no flow.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance. The EGC control electronics may have
malfunctioned.
This error occurs when an EGC is plugged into the EG that is not one of the
supported types.
To troubleshoot:
Refer to Table 2-2 for a list of the supported EGC types for capillary and
analytical IC systems.
This error occurs if the pump flow is turned off because of a pump pressure
alarm or leak. The EG is automatically turned off to prevent damage to the
EG.
To troubleshoot:
Check the troubleshooting information for the pump in Section 8.14 and
Section 8.15.
This error occurs when a “live” EG is linked to a virtual pump and you try to
turn on the EGC. To prevent damage to the EGC, the mode is automatically
turned off to ensure that the EG does not operate when there is no flow.
This error occurs when the flow to the EG is out of range or there is no
pumped linked to the EG.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.
EG mode will be turned off for invalid flow. Flow range for
analytical EGC: 0.100 – 3.000 mL/min, capillary EGC: 0.001 –
0.100 mL/min.
This error occurs when the flow to the EGC is out of range or there is no
pumped linked to the EGC.
To troubleshoot:
1. Set the flow rate to a value within the allowed range. Refer to Appendix A
for flow rate specifications.
2. Check the EGC configuration properties in the Chromeleon 7 Instrument
Controller Service or the Chromeleon 6.8 Server Configuration program
to verify that the pump and EGC are linked.
This error occurs if the type of pump linked to the EGC does not match the
EGC type. A capillary EGC can only be used with a capillary pump and an
analytical EGC can only be used with an analytical pump.
To troubleshoot:
1. Install the correct type of EGC for the pump type.
2. For a hybrid system (a dual system with both an analytical and a capillary
pump), check the EGC configuration properties in the Chromeleon 7
Instrument Controller Service or the Chromeleon 6.8 Server
Configuration program to verify that the correct pump is linked to the
EGC.
This error occurs if the ion count reported by the EGC is invalid. This may
indicate a problem with the memory chip in the EGC.
To troubleshoot:
1. Make sure the EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
2. If the error message appears again, contact Technical Support for Dionex
products for assistance.
This error occurs when liquid accumulates in the drip tray in the bottom of the
EG.
To troubleshoot:
1. Locate the source of the leak by visually inspecting the tubing, fittings,
and components in the EG.
2. Tighten fittings (or replace tubing and fittings) as required (see
Section 9.12). Refer to Section 8.22 for detailed troubleshooting of
various types of leaks.
3. After fixing the leak, dry the drip tray and leak sensor thoroughly to
prevent the leak sensor from triggering additional error messages.
• Electrical error
The EG current and/or voltage may have become unstable. Contact
Technical Support for Dionex products for assistance.
8.23 No Flow
• DP/SP power is off
Turning off the DP/SP automatically turns off the EG and the suppressor.
Current to the CR-TC is automatically turned on and off when the EG
power is turned on and off.
Check that the power to the DP/SP is turned on. Prime the pump (see
Section 9.5) and resume operation.
• DP/SP pressure limit tripped
Verify that the Current Pressure reading on the Chromeleon 7 ePanel Set
or the Chromeleon 6.8 panel tabset is between the high and low limits
displayed on the panel. For details, see Section 4.8.
• EGC is expended
Replace the cartridge (see Section 9.14).
• No communication with Chromeleon
1. Check that the POWER button on the front of the EG is turned on.
2. Check that the EG main power switch (on the rear panel) is turned on.
3. Check that the main power cord is plugged into both the EG rear
panel connector and the power source. Check that the wall outlet has
power.
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).
To troubleshoot:
1. Check the detector connection: An electronics connector on the back of
the detector plugs into a receptacle on the detector compartment. Push on
the upper part of the detector (see Figure 8-3) to make certain the
connector is securely connected.
2. If the error persists, there may be a problem in the detector electronics.
Contact Technical Support for Dionex products for assistance.
Push here to
ensure the
detector’s
electrical
connection is
secure.
This error occurs when the temperature of the conductivity detector is higher
than the maximum allowed. This error may occur if the Thermo Scientific
Dionex ICS-5000 Ion Chromatography System is operating in an
environment in which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
1. Refer to Appendix A for environmental specifications.
2. Verify that the compartment setpoint is at least 5 °C less than the CD cell
setpoint.
3. Check the suppressor current setting. Running the suppressor at a higher
current than is recommended for the application can cause heat-up of the
CD cell.
This error occurs when the temperature of the column compartment exceeds
the maximum allowed. This error may occur if the Thermo Scientific Dionex
ICS-5000 Ion Chromatography System is operating in an environment in
which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.
To troubleshoot:
Repeat the calibration procedure. Follow the instructions provided in the DC
Temperature Calibration Kit (P/N 063782). If the error appears again, contact
Technical Support for Dionex products for assistance.
To troubleshoot:
Repeat the calibration procedure, following the instructions provided in the
DC Temperature Calibration Kit (P/N 063782). If the error appears again,
contact Technical Support for Dionex products for assistance.
This error can have multiple causes (for example, a cell potential that is too
high for a given salt concentration, a cell potential that is too high because the
reference mode is incorrect, injection of excessive amounts of electroactive
ED Cell Cable
2. If the error appears again, contact Technical Support for Dionex products
for assistance. The detector electronics may have malfunctioned.
This error occurs when the cable on the working electrode is disconnected
from the cell electronics.
To troubleshoot:
Check the cable connection: Verify that the signal cable from the working
electrode is connected to the detector block (see Figure 8-4).
This error occurs when the pH reading differs by more than 1.0 pH unit from
7.0, which is the value specified for offset calibration. This can be caused by
too large a change in the Ag/AgCl reference potential or by a damaged glass
membrane in the pH sensing part of the reference electrode
To troubleshoot:
This error occurs when the pH sensing glass membrane of the Ag/AgCl
reference electrode is broken or otherwise affected, causing the calibration
slope to deviate by more than ±10% from the theoretical slope of 59 mV/pH
unit at 25 C.
To troubleshoot:
1. 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,
repeat the calibration at least one more time.
4. If the error recurs after repeating the calibration at least two times, replace
the Ag/AgCl reference electrode (see Section 9.28.5).
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).
High-Pressure
1 Valve #1
High-Pressure
1 2 2 Valve #2 (not
installed in this
system)
High-
3 Pressure
Valve #3
High-
3 4 4 Pressure
Valve #4
3 High-
4 Pressure
3
Valve #3
High-
4 Pressure
Valve #4
To troubleshoot:
1. If a sequence is being executed, terminate the sequence by selecting Stop
on the Chromeleon 7 ePanel or Chromeleon 6.8 Control panel.
2. Turn off the Thermo Scientific Dionex ICS-5000 Ion Chromatography
System power briefly by pressing the POWER button on the front of each
module. Then press each button again to restart the system.
3. Try to toggle the valve from Load to Inject by pressing the Load and
Inject buttons on the front of the DC.
4. If the problem persists, contact Technical Support for Dionex products for
assistance.
This error occurs when the temperature of the IC Cube heater exceeds the
maximum allowed. This error may occur if the Thermo Scientific Dionex
ICS-5000 Ion Chromatography System is operating in an environment in
which the temperature is greater than 40 °C (104 °F).
To troubleshoot:
Refer to Appendix A for environmental specifications.
This message occurs when the door to the lower compartment is opened
during a run.
To troubleshoot:
1. Verify that the door is fully closed.
2. Check for—and remove—any obstruction.
3. If the door is fully closed and the error persists, contact Technical Support
for Dionex products for assistance.
The leak sensor is installed in the drip tray at the bottom of the column
compartment (see Figure 9-33). If liquid accumulates in the tray, the sensor
signals the problem and this error message appears.
To troubleshoot:
1. Locate the source of the leak by visually inspecting the tubing, fittings,
and components.
2. Tighten fittings or replace tubing and fittings as required. Refer to
Section 8.26 for detailed troubleshooting of various types of leaks.
3. After fixing the leak, dry the drip tray thoroughly to prevent the leak
sensor from triggering additional error messages.
This error occurs when the reaction coil heater is unplugged from the DC.
To troubleshoot:
1. Check that the reaction coil heater is correctly plugged into the
component panel.
2. If the error persists, the heater may be faulty. Replace the heater
(P/N 061746).
Suppressor over-current.
Suppressor over-power.
This error appears when, in order to maintain the selected current, the Thermo
Scientific Dionex ICS-5000 Ion Chromatography System is required to apply
a higher voltage than the suppressor can support.
To troubleshoot:
1. Reduce the flow rate.
Suppressor over-voltage.
This error appears if you turn on the suppressor and the system cannot
establish a connection with the suppressor.
To troubleshoot:
1. Check the suppressor cable connection.
2. If the error persists, replace the suppressor (see Section 9.27.2).
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.
This message occurs when the door to the upper compartment is opened
during a run.
To troubleshoot:
1. Verify that the door is fully closed.
2. Check for—and remove—any obstruction.
3. If the door is fully closed and the error persists, contact Technical Support
for Dionex products for assistance.
Check the
cable
connection
3. If soaking does not fix the problem, replace the electrode (see
Section 9.28.5).
When a TC is shared by two timebases, the same values must be selected for
certain parameters. If the Chromeleon Ready Check detects a discrepancy,
this error occurs and batch processing cannot be started.
To troubleshoot:
Find and eliminate any discrepancies in the parameter settings. For example,
all samples must turn on TempCtrl or all samples must turn off TempCtrl.
This error occurs if you attempt to execute the AcqOn command while
retention times are negative.
To troubleshoot:
Wait until the retention time value is positive.
-or-
This error occurs if the device selected to monitor the system pressure is
ineligible to do so.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name, and select the SystemPressure
command.
4. Enter the name of the pump currently delivering flow for this column.
5. For Chromeleon 6.8, click Execute.
This error indicates that the column ID chip card memory is corrupted.
To troubleshoot:
Replace the column ID chip card (see Section 9.30).
This error occurs if you attempt to issue a command that is not available when
the TC is in demo (or simulation) mode.
To troubleshoot:
If a TC is present and connected, disable the demo mode:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. In the instrument or timebase, right-click the TC and select Properties.
3. On the General tab page, clear the Simulation Mode or Demo Mode
check box.
4. 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 between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.
Communication time-out.
This error occurs if a TC firmware command is not executed within the time
allotted for its completion.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.
This error occurs if there is a discrepancy between the TC properties and the
actual configuration.
To troubleshoot:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. In the instrument or timebase, right-click the TC and select Properties.
3. Correct any discrepancies in the Properties dialog box.
This error occurs if the current flow rate exceeds the value specified by the
Column_x.FlowRate_UpperLimit command.
To troubleshoot:
Select a valid flow rate.
This error occurs if the current pressure reading is outside the range specified
by the Column_x.Pressure_UpperLimit and Column_x.Pressure_
LowerLimit commands.
To troubleshoot:
• Find and eliminate any liquid leaks or blockages in tubing connections
(see Section 8.31). Adjust the flow rate accordingly.
This error occurs if the current temperature reading is outside the range
specified by the Column_x.Temp_UpperLimit and Column_x.Temp_
LowerLimit commands.
To troubleshoot:
Select a valid temperature setting.
This error occurs in Chromeleon 6.8 if the system cannot write incoming data
to disk fast enough.
To troubleshoot:
Increase the buffer size:
1. Start the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program.
2. Right-click the computer name and select Properties on the menu.
3. Click the Advanced tab and enter a new value (in seconds) in the Buffer
field. Click OK.
4. If the error occurs again, contact Technical Support for Dionex products
for assistance.
This error occurs if you attempt to select or define a feature that is not
available for your TC.
To troubleshoot:
Select Help > About Chromeleon... to open the About Chromeleon screen.
• For Chromeleon 7, click Details to view all license features you
purchased (devices controlled, number of timebases, and other software
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.
TC is not remote.
This error occurs if there is a problem with the connection between the TC
and the Chromeleon server or with the power supply.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.
Either the current date is later than the expiration date for x or the
program or batch will end later than 24 hours before the
expiration time for x.
Chromeleon compares the current date with the column expiration date during
injection or before beginning batch processing. This error occurs if the
expiration date has already passed or if batch processing is scheduled to start
less than 24 hours before the expiration date.
To troubleshoot:
Replace the column.
This error occurs if, during a firmware download, the existing firmware
cannot be erased from memory.
To troubleshoot:
Flash memory cannot be serviced by the user. Contact Technical Support for
Dionex products for assistance.
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.
This error occurs if you attempt to issue a command while firmware is being
downloaded to the TC.
To troubleshoot:
Wait until the firmware download is complete. Audit Trail messages will
inform you of the status of the download.
This error occurs if the gas sensor detects an increased concentration of gas
inside the TC.
To troubleshoot:
1. Find and eliminate the leak.
2. 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.
3. If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
4. Ventilate the interior of the TC thoroughly before closing the door and
resuming operation.
Illegal parameter.
This error occurs if you enter a parameter that is not valid for the TC.
To troubleshoot:
Select a valid parameter.
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.
This error occurs if you attempt to enter an invalid value for a property, rather
than selecting a value from the drop-down list box in the Commands dialog
box.
To troubleshoot:
Select a valid option from the drop-down list box available for this property.
Chromeleon monitors the date on which qualification was last performed and
displays an appropriate message (shown above) at the following times: when
the due date for the next qualification is approaching; when the due date is
overdue, but the TC can still be used; and when the due date is overdue and
the TC can no longer be used.
The Qualification.WarningPeriod property determines the number of days
before the due date that the warning is first displayed. The
Qualification.GracePeriod property determines for how many days after the
due date you can continue using the TC without performing the qualification.
To troubleshoot:
Contact Technical Support for Dionex products to schedule an Operational
Qualification and Performance Qualification.
Chromeleon monitors the date on which service was last performed and
display an appropriate message (shown above) at the following times: when
the due date for the next service is approaching and when the due date is
overdue. The Service.WarningPeriod property determines the number of
days before the due date that the warning is first displayed.
To troubleshoot:
Contact Technical Support for Dionex products for information about
performing annual preventive maintenance.
This error occurs if a column ID chip card is not installed for the column
identified in the message.
To troubleshoot:
Install a column ID chip card for the column (see Section 9.30). Or, if you do
not want to store information about this column, follow the steps below to
disable this option.
1. In the Chromeleon 7 Instrument Configuration Manager or the
Chromeleon 6.8 Server Configuration program, right-click the TC and
select Properties on the context menu.
2. Select the Components tab in the Properties dialog box. Clear the check
mark beside the column name and click OK.
This error occurs if there is a communication failure between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.
This error occurs if you select a TC temperature setting above 70 °C (158 °F).
To troubleshoot:
Refer to the column manual for the recommended operating conditions.
Column manuals are provided on the Thermo Scientific Reference Library
DVD (P/N 053891).
Value for [name] parameter is not within valid range. Value passed
(x) will be substituted by y.
-or-
If you select a value outside the allowable range for certain parameters,
Chromeleon ignores the setting, replaces it with the closest valid setting, and
this error occurs.
To troubleshoot:
No immediate action is required. In future, specify a valid setting for the
parameter.
This error occurs if you attempt to change one of the primary column
properties (batch or lot number, date of manufacture, etc.) used for column
identification.
To troubleshoot:
Once a primary column property has been assigned, it cannot be changed. As
an alternative, consider changing a secondary column property. For a list of
primary and secondary properties, refer to the Chromeleon Help.
This error occurs if you attempt to change column ID properties when at least
one column ID chip card is inserted incorrectly.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name and select the CardState property. If
the status is BusBlocked, remove the card from the card slot and reinsert
it.
When the card is properly installed, the Dionex logo on the card faces up and
the LED on the memory slot is green.
This error occurs if you attempt to change column ID properties when the TC
door is open (or is not fully closed).
To troubleshoot:
1. Verify that the door is fully closed.
2. If the door is not fully closed, check for—and remove—any obstruction.
3. If the door is fully closed but the error persists, contact Technical Support
for Dionex products for assistance.
This error occurs if you attempt to change column ID properties for a column
for which no chip card is installed.
To troubleshoot:
Insert a column ID chip card into the appropriate slot (see Section 9.30).
This error occurs if you attempt to start data acquisition manually while a
batch is already running.
To troubleshoot:
To retain the data already acquired, cancel manual data acquisition; otherwise,
go ahead and start data acquisition.
The command can format only chip cards with an invalid data
structure.
This error occurs if you select the FormatChipCard command for a column
ID chip card that is not defective.
To troubleshoot:
Cancel the command. Do not attempt to reinitialize a chip card unless it
contains invalid or corrupted data.
This error occurs if there is a communication failure between the TC and the
PC on which Chromeleon is installed.
To troubleshoot:
1. Check the USB connections.
2. Check the connection from the TC to the power supply.
3. If you cannot identify the cause of the error, contact Technical Support for
Dionex products for assistance.
This error occurs if you attempt to operate the TC when the door is open (or
not fully closed).
To troubleshoot:
1. Verify that the door is fully closed.
2. If the door is not fully closed, check for—and remove—any obstruction.
3. If the door is fully closed but the error persists, contact Technical Support
for Dionex products for assistance.
The counter [name] (value: x) has exceeded its limit (y). Module
should no longer be used. Replace the [name].
This error occurs if the number of hours a TC part has been in use exceeds the
lifetime set by the OperationTime.Limit property.
To troubleshoot:
Replace the part identified in the message before resuming operation.
This error occurs if the column ID chip card data is inadvertently saved in an
invalid format.
To troubleshoot:
1. To reinitialize the chip card, open the Chromeleon 7 ePanel Set or the
Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name and select the FormatChipCard
command.
4. For Chromeleon 6.8, click Execute.
Chromeleon monitors the number of injections done with each column and
display an appropriate message (shown above) at the following times: when
the injections limit is about to be exceeded or has been exceeded.
To troubleshoot:
Replace the column.
This error occurs if the selected TC temperature setting is outside the range
specified by the Temperature.LowerLimit and Temperature.UpperLimit
commands.
To troubleshoot:
Select a valid temperature setting.
This error occurs if the selected TC temperature setting is outside the range
specified by the Column_x.Temp_LowerLimit and Column_x.Temp_
UpperLimit commands.
To troubleshoot:
Select a valid temperature setting.
The oven is not fully operable yet. Check the values of “Standby,”
“Ready,” “Door,” and “CardState.”
Each time the TC power is turned on, the firmware runs a series of self-
diagnostics in which the status of the main components is checked. This error
occurs if a component is not ready for operation.
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. Check the status of each property listed in the error message. The table
below indicates the status required for operation.
Command Status
CardState OK
Door Closed
Ready Ready
Standby NoStandby
4. When you identify the component that is not ready for operation, find and
eliminate the cause of the problem.
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.
This error occurs if the value entered for a parameter’s upper limit (for
example, TC_Temp.Signal.UpperLimit) is less than the lower limit for the
parameter.
To troubleshoot:
Increase the value of the upper limit setting.
This error occurs if the Warning value selected for a Predictive Performance
command (for example, LeftRotorSealSwitches) is lower than the Limit
value. Chromeleon issues a warning message in the Audit Trail when the
Warning value is reached and an error message when the Limit value is
reached.
To troubleshoot:
Select a Warning value that is higher than the Limit value.
This error occurs if the Warning value selected for a parameter is higher than
the Limit value. Chromeleon issues a warning message in the Audit Trail
when the Warning value is reached and an error message when the Limit
value is reached.
To troubleshoot:
Select a Warning value that is lower than the Limit value.
This error occurs if you attempt to change the setting for a read-only
parameter.
To troubleshoot:
Do not attempt to reset read-only parameters.
This 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.
This error occurs if Chromeleon does not recognize the format of data stored
on the column ID chip card.
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Commands dialog box.
3. Under TC, select the column name and select the FormatChipCard
command.
4. For Chromeleon 6.8, click Execute.
5. If the error occurs again, insert a new column ID chip card (see
Section 9.30).
X position error.
This error occurs if a TC injection valve fails to switch position within the
time allotted.
To troubleshoot:
1. If a sequence is being executed, terminate the sequence by clicking Abort
Batch on the Sequence Control panel.
2. Press the POWER button on the front of the TC to turn off the power; after
30 seconds, press the button again to turn on the power.
3. Try to toggle the injection valve from Load to Inject by clicking the Load
and Inject buttons on the TC ePanel or Control panel.
4. If the error occurs again, contact Technical Support for Dionex products
for assistance.
To troubleshoot:
The Chromeleon 6.8 administrator assigns various privileges to individual
users or to user groups. Contact the administrator if you need one or more of
the above privileges assigned to you.
Figure 9-1 illustrates the correct and incorrect placement of the ferrule and
fitting bolt on the tubing.
Correct Incorrect
2 mm
Figure 9-1. Correct and Incorrect Ferrule and Fitting Bolt Placement for
Capillary Tubing Connections (High-Pressure Fitting and Ferrule Shown)
ICS-5000
DP/SP DP/SP Service
Notes
• For tightening requirements for the 10-32 fitting bolt (P/N 043275) and
ferrule (P/N 043276), refer to Installation of Dionex Liquid Line Fittings
(Document No. 031432). The manual is on the Thermo Scientific
Reference Library DVD (P/N 053891).
• For tightening requirements for the high-pressure fitting bolt
(P/N 074449) and ferrule (P/N 074373), see Section 9.2.
• Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing and there are no nicks or burrs
on the end. A tubing cutter (P/N 049584) is included in the DC Ship Kit
(P/N 072011). Refer to the instructions provided with the cutter.
5. Open the priming valve on the secondary pump head (see Figure 9-2) by
turning it one-half turn counterclockwise.
1 Priming Valve
6. Press PUMP PRIME 1 (or PUMP PRIME 2) on the front of the DP/SP. The
pump will begin pumping at the priming flow rate selected on the
Chromeleon panel.
7. Prime the pump until all air is purged and no air bubbles can be seen
exiting the waste line.
8. Gradient pump only: To prime additional eluent lines, select another
eluent channel and repeat the priming procedure.
9. After priming all eluent lines, press PUMP PRIME 1 (or PUMP PRIME 2) to
stop priming and return to the flow rate last selected.
10. Close the priming valve by turning it clockwise. Do not overtighten the
priming valve.
Do not use any tools to tighten the priming valve! Overtightening may
destroy the cap seal. Open or close the priming valve only when the
system pressure is down.
11. Reconnect the pump to the software by clicking Connected on the Pump
panel.
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, or D) to be
primed.
4. Set the priming flow rate to the desired rate. The default rate for a
capillary IC pump is 3.0 mL/min. The default rate for an analytical IC
pump is 6.0 mL/min.
5. Click the Prime button on the Pump panel. A warning message asks you
to verify that the purge (priming) valve is open. Click Execute despite
warnings (Chromeleon 7) or OK (Chromeleon 6.8). Priming starts.
6. Prime the pump until all air is purged and no air bubbles can be seen
exiting the waste line. Click the Prime button to stop priming.
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)
7. The check valves are installed in the primary pump head (see Figure 9-3).
8. Disconnect the tubing connections from the inlet and outlet check valves.
9. Loosen both check valve assemblies using the 1/2-inch wrench
(P/N 062336).
10. Remove both check valve assemblies from the pump head.
3. Before installing the inlet and outlet check valves, rinse the bottom of the
check valve ports in the pump head with isopropyl alcohol and blow them
clean using a 0.2 micron filtered, canned air duster. Inspect the bottom of
each port for any particulate matter. If necessary, rinse and dry again until
they are clean.
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.
Overtightening may damage the pump head and check valve housing
and crush the check valve seats.
6. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
7. Press the POWER button on the front of the DP/SP to turn on the pump.
8. Reconnect the pump to the software by clicking Connected on the Pump
panel.
Before beginning, locate the following items in your pump ship kit:
• 3.0 mm hex key (P/N 062338)
• 10-32 fitting plugs (P/N 042772)
• 10 cc syringe (P/N 054578)
• Seal insertion tool (P/N 063675)
Additional items:
• Cleanroom gloves (lint-free, particle-free, and oil-free)
• Small beaker
• ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5
• Methanol (optional)
• 0.2 micron filtered, Class 10, isopropyl alcohol (IPA)
• Lint-free paper towels (KIMWIPES® or equivalent)
• Large flat-blade screwdriver
• 0.2 micron filtered, canned air duster (ITW Chemtronics Ultrajet or
equivalent)
7. Disconnect all tubing connections to the pump head with the defective
piston seal.
8. The primary and secondary pump heads have different components.
When disassembling a pump head, refer to Figure 9-6 for a primary pump
head or Figure 9-7 for a secondary pump head.
7
6
4
3
2
C
1
10 B
12
8 10
11
5
7
6
4
3
8 Secondary Pump Head
2 P/N 074240 (Capillary)
P/N 062079 (Analytical)
1
4 Seal Wash Body 9 Priming Valve
P/N 074446 (Capillary) P/N 063968
P/N 062064 (Analytical) (Capillary and Analytical)
1 Piston 5 10 Priming Valve Seal
P/N 068646 (Capillary) P/N 063382
P/N 062082 (Analytical) (Capillary and Analytical)
9. Using a 3.0 mm hex key (P/N 062338), loosen the two screws on the
pump head with the defective seal. Remove the screws, and then carefully
remove the head and place it on a clean surface.
10. Remove the seal wash body from the pump head. Or, if the seal wash
body was not removed with the pump head in Step 9, pull it straight out of
the pump mechanism now.
11. Pull the piston out of the pump mechanism.
5. If the piston seal was not removed in Step 4, follow these steps:
a. Verify that the 10-32 fitting plugs in the inlet and outlet holes are
tightened enough to prevent any leaks from the pump head.
b. Fill the piston cavity with water and check for bubbles.
c. If there are no bubbles, repeat Step 4.
Figure 9-8. Piston Seal Wash Seal and Seal Insertion Tool
c. Insert this end of the tool partway into the seal wash body. Make sure
the tool is centered and does not rock back and forth. Then, press
firmly on the tool and the seal wash body until they snap together.
d. Remove the seal insertion tool from the seal wash body.
e. The seal wash seal is now partially installed. To complete the seal
installation, place the retainer in the seal wash body and use the large
flat-blade screwdriver to tighten the retainer.
f. Place the new O-ring (P/N 040695) on the seal wash body.
5. Place the front of the pump head, flat side down, on a clean work surface.
Make sure the open side of the piston seal faces away from the retainer for
the seal wash seal.
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 cavity
with ASTM Type I (18 megohm-cm) filtered and deionized water.
7. Place the components on the pump head and gently press the housing until
the piston seal snaps into place.
When pressing the seal in place, ensure that the piston is free to move out,
to relieve the pressure in the pump head during seal installation.
Do not use a sharp tool (such as tweezers) to install the piston seal.
This will scratch the seal and the inside of the pump housing; these
scratches will prevent a proper seal and cause leakage.
Before beginning, locate the 3.0 mm hex key (P/N 062338) in your pump ship
kit:
Additional items:
• Cleanroom gloves (lint-free, particle-free, and oil-free)
• ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5
7. Disconnect all tubing connections to the pump head with the damaged
piston.
8. Using a 3.0 mm hex key (P/N 062338), loosen the Allen screws on the
pump head with the damaged piston. Remove the Allen screws, and then
carefully remove the head and place it on a clean surface.
9. If the piston was not removed with the pump head in Step 8, remove the
piston now by pulling it straight out of the pump mechanism.
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.
d. Pull on the fitting slightly to remove the PharMed tubing from the
upper notch on the pump mounting plate.
PharMed Tubing
1 (P/N 063268)
2 Rotor
6 1 3 Lever
4 Mounting Plate
2
5 Tygon 2075 Tubing
3 5 (P/N 064079)
4 6 Fitting
5. Pull off the PharMed and Tygon 2075 tubing from the fitting. Save the
fitting.
6. Pull off all seal wash tubing from the seal wash reservoir and the primary
and secondary pump heads(see Figure 9-10).
7. Cut three new pieces of Tygon 2075 tubing (0.15 cm (0.060 in) ID;
P/N 064079) and one piece of PharMed tubing (0.159 cm (0.0625 in) ID;
P/N 063268) to the same lengths as the tubing just removed. The tubing is
included in the pump ship kit:
Pump Ship Kit Part Number
DP Ship Kit Dual Capillary 072112
DP Ship Kit Dual Analytical 062463
DP Ship Kit Capillary and Analytical 072111
SP Ship Kit Capillary or Analytical 063342
e. Pull on the fitting slightly to slide the tubing into the upper notch.
f. Make sure there is no slack in the tubing. If necessary, lift the lever
again, adjust the tubing around the rotor and through the lower notch
to remove any slack, and release the lever.
11. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
12. Turn on the pump flow.
1 Priming Valve
Secondary
1 2
Pump Head
7. Pull the old seal off the end of the priming valve knob.
8. Hold the new seal (P/N 063382) with the groove in the priming valve seal
facing away from the knob (see Figure 9-12). Carefully slide the seal onto
the knob; avoid scratching or nicking the sides.
Do not use a sharp tool (such as tweezers) to install the seal. This may
scratch the seal and the surface of the priming valve knob. These
scratches will prevent a proper seal and cause leakage.
9. Insert the priming valve knob into the secondary pump head, turn the
knob clockwise, and tighten fingertight.
10. Push the component mounting panel back into the enclosure. Close the
DP/SP door.
11. Press the POWER button on the front of the DP/SP to turn on the pump.
12. Reconnect the pump to the software by clicking Connected on the Pump
panel.
13. Turn on the pump flow.
• Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
3. Turn off the main power switch on the rear panel of the pump (see
Figure 2-7).
4. Disconnect the main power cord from both its source and from the rear
panel of the pump.
HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the pump.
The EGC contains one of the following: a corrosive base (KOH, LiOH, or
NaOH), a corrosive acid (MSA), or a concentrated K2CO3 solution. Wear
protective eyewear and gloves when handling the cartridge.
5. Close or cap the EGC vent opening to prevent leakage when you turn over
the cartridge in Step 7.
Capillary EGC
Capillary If you are removing a Vent Fitting
IC capillary EGC, tighten the Vent Fitting
vent fitting on the top of the
EGC (see Figure 9-15).
b. Locate 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 Generation
Figure 9-17). This is the Chamber
“service position” for the
cartridge.
Electrolyte
Reservoir
Drip Tray
8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET
ports on the EGC.
2. Rinse the electrolyte reservoir and membranes three times with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Rinsing should render the reservoir
and membranes nonhazardous; however, check your local, state, and
federal regulatory agency regulations for proper disposal.
5 WASTE, GAS
SEPARATOR
EG To CR-TC
Degas Regen Out
Cartridge (blue label)
(inside DC)
To CR-TC To CR-TC
ELUENT OUT
REGEN IN
REGEN OUT
4 3
To Inject ELUENT IN To EG Degas
Valve Eluent In
(red label)
Electrolyte Reservoir
EGC
Electrolyte Generation IN 38 cm (15 in) of 0.025 mm
Chamber (0.001 in) ID tan
PEEK tubing
(Temporary connection
for backpressure)
EGC
0.25 mm (0.010 in) ID OUT
Pump Outlet
PEEK tubing
Tubing Assembly
(Temporary
connection) (P/N 068658)
To Waste TO PUMP/DAMPER
9. Push the EGC electrical cable firmly into the EGC 1 (or EGC 2) bulkhead
connector (see Figure 9-14). Twist the ring on the cable connector
fingertight to secure it.
10. Unscrew the fitting on the top of the EGC a few turns to vent the EGC.
To ensure proper ventilation, always loosen the fitting on the top of the
capillary EGC before operation.
11. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. DC panel: Verify that the suppressor Mode is off.
b. EG panel: Verify that the CR-TC is off.
To avoid damaging the suppressor and CR-TC, always turn them off
before flushing the EGC. The pump flow is on during flushing; however,
no flow reaches the suppressor or CR-TC.
c. Pump panel: Set the flow rate to 0.02 mL/min. This turns on the
pump flow, also.
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.
EGC
IN
0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly EGC
(P/N 072204) OUT ELUENT
IN
TO PUMP/DAMPER
To CR-TC
Regen Out
(blue label)
6. Set the EGC concentration to 50 mM and turn on the EGC and CR-TC
power.
7. Condition the EGC for 15 minutes.
8. Turn off the EGC and CR-TC power.
9. Turn off the pump flow.
10. Remove the 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.
EGC VENT
EGC RFIC
Eluent
Degasser
Regen Regen
To Waste Out In
Eluent Eluent
Out In
Inlet Outlet
EGC
IN
EGC
TO PUMP OUT
Coupler
TO INJ VALVE - P
Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Regen In
TO CR -TC (orange label)
WASTE, GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
ELUENT OUT
To CR-TC
REGEN IN
Eluent In
(red label)
CR-TC
2. Verify that a plug is installed in the vent port. This will prevent leakage
from the vent opening when you turn over the cartridge.
3. Turn the cartridge upside down and place it on the EG drip tray in the
service position (see Figure 9-17).
4. Remove the plugs from the INLET and OUTLET fittings on the eluent
generation chamber.
5. Connect the EGC IN line from the pump to the EGC INLET port.
6. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil
(P/N 053765) in the EG Ship Kit (P/N 072047).
7. Connect one end of the
backpressure coil to the EGC Backpressure
OUTLET port (see Figure 9-23); Coil
10. Push the EGC electrical cable firmly into the EGC 1 (or EGC 2) bulkhead
connector (see Figure 9-14). Twist the ring on the cable connector
fingertight to secure it.
11. Remove the 10-32 plug from the EGC vent opening. Install a 10-32 luer
adapter in the vent opening.
12. Connect the luer adapter and VENT line removed from the old cartridge to
the vent opening in the new cartridge (see Figure 9-16).
13. Place the 10-32 plug removed from the vent opening in a safe place for
storage. The 10-32 plug is required for shipping or storing the cartridge.
To ensure proper ventilation, always connect the vent line to the
analytical EGC before operation.
TO PUMP
To Waste
1. Set a small temporary waste container (for example, a beaker) next to the
EG. Direct the yellow backpressure coil from the EGC OUTLET port to
the waste container. The backpressure must be at least 1.4 MPa (200 psi).
2. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. DC panel: Verify that the suppressor Mode is off.
b. EG panel: Verify that the CR-TC is off.
To avoid damaging the suppressor and CR-TC, always turn them off
before conditioning the EGC. The pump flow is on during conditioning;
however, no flow reaches the suppressor or CR-TC.
c. Pump panel:
• 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.
1. Twist the ring on the EGC electrical cable counterclockwise to loosen it,
and then pull the cable straight out of the EGC 1 (or EGC 2) bulkhead
connector.
2. Remove the backpressure tubing from the waste container and remove the
waste container.
3. Replace the 10-32 plug in the EGC vent 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 the holder. Remove the 10-32 plug from the vent
opening and reinstall the luer adapter and vent line.
9. Reconnect the EGC electrical cable.
Refer to Figure 9-18 for a flow schematic of the EG and CR-TC for capillary
IC and to Figure 9-22 for analytical IC.
d. Connect the EGC OUT line to the CR-TC ELUENT IN port and connect
the waste line to the CR-TC REGEN OUT port.
EGC
IN
0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly EGC
(P/N 072204) OUT ELUENT
IN
TO PUMP/DAMPER
To CR-TC
Regen Out
(blue label)
TO CR -TC
REGEN OUT
(blue label)
Eluent Out
(yellow label)
To CR-TC
ELUENT OUT
REGEN IN
Eluent In
(red label)
Regen In
(orange label)
CR-TC Hydration Kit
Tubing Assembly
(P/N 063487)
(Temporary connection)
b. Pump panel:
• Gradient pump only: Select the correct eluent channel (A, B, C,
or D).
• Analytical pumps: Set the flow rate recommended for your
application. This turns on the pump flow, also. Allow the pump to
run for at least 10 minutes.
• 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.
To EGC
OUTLET Port
WASTE , GAS
SEPARATOR
To CR-TC
Regen Out
(blue label)
To CR-TC To CR-TC
ELUENT OUT
REGEN IN
To CR-TC
Regen In
(orange label)
To EG Degas
Cartridge
Regen Out
To EG Degas
Cartridge
Eluent In
To CR-TC
To Gas Separator Regen In
Waste Tube (orange label)
TO CR -TC
WASTE , GAS REGEN OUT To CR-TC
SEPARATOR (blue label) Eluent Out
(yellow label)
To CR-TC
ELUENT O UT
REGEN IN
Eluent In
(red label)
CR-TC
2. Check that no liquid lines are caught under the CR-TC. Align the two
mounting holes on the CR-TC back plate with the ball studs on the
mounting plate, and then push the CR-TC firmly onto the mounting ball
studs. The CR-TC clicks into place when properly installed.
3. Push the CR-TC electrical cable firmly into the CR-TC 1 (or CR-TC 2)
bulkhead connector. Twist the ring on the cable connector fingertight to
secure it.
4. Push the tray into the module until it locks into place. Close the EG door.
The EG Ship Kit (P/N 072047) includes four backpressure coils (see
Table 9-5).
HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the EG.
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.
Capillary Table 9-7 lists the tubing and fittings in the IC Cube Tubing Kit (P/N 072186)
IC
on the end. A tubing cutter (P/N 049584) is included in the DC Ship Kit
(P/N 072011). Refer to the instructions provided with the cutter.
• For 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).
Sample Loading
1
Ports
1 1 2 Release Tabs
2 2
4. Attach the luer adapter fitting to the front of the port (see Figure 9-32).
5. Cut a length of green, 0.75 mm (0.030 in) ID PEEK tubing. The tubing
will be used to connect the sample loading port and the sample port on the
valve.
6. Attach a 1/4-28 fitting and ferrule to one end of this tubing and connect it
to the rear of the sample loading port.
7. Thread the free end of the tubing through the sample loading port opening
on the DC. Insert the port into the opening and turn it until it snaps into
place.
8. Attach a 10-32 fitting and ferrule to the free end of the tubing and connect
it to sample port S (5) on the injection valve.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
Leak
Sensor
Loosen
this
screw
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.
NOTE If you prefer, you can replace the high-pressure valve “pod,”
instead of rebuilding the valve. Replacing the pod is easier
and faster than rebuilding the valve.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.
3. Open the DC door.
Locking Ring
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.
8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-36). If necessary, twist the end of the
pod to adjust the position of the splines.
Slot (larger)
Runner (larger)
Splines
9. Push the pod into the holder until it clicks into place. Replace the black
locking ring.
10. Reconnect all liquid lines to the valve.
11. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required. For tightening requirements, refer to Installation of Dionex
Liquid Line Fittings (Document No. 031432). The manual is on the
Thermo Scientific Reference Library DVD (P/N 053891).
12. Close the door.
3. Disconnect the main power cord from both its source and from the DC
rear panel.
HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the DC.
4. On the DC rear panel, remove the two screws that attach the I/O option
cover plate or the existing I/O option board to the rear panel (see
Figure 9-37). Save the screws.
Remove two
screws
Figure 9-37. DC Rear Panel: Removing the I/O Option Cover Plate
5. Slide the new I/O option board (P/N 062201) into the rear panel opening
and press firmly to connect the board to the DC motherboard.
6. Replace the two screws.
I/O
Option
HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the DC.
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.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
Disconnect
these two lines
4. Loosen the two thumbscrews on the column cartridge and pull the
cartridge out of the IC Cube.
5. Lift the lid of the column cartridge to open it. Figure 9-42 shows the
column cartridge when a capillary guard column and a capillary separator
column are installed.
Separator
1 Column Outlet
Separator
8 2 Column
1
Separator
3 7 3 Column Inlet
4
2 4 Precision Cut
5 Tubing
Guard Column
5 Outlet
6
6 Guard Column
7 Guard Column
Inlet
8 Precision Cut
Tubing
Figure 9-43 shows the column cartridge when only a capillary separator
column is installed
Separator
1 Column Outlet
1
3 4
Separator
2 Column
2
Separator
3 Column Inlet
4 Precision Cut
Tubing
NOTE Do not cut the tubing that you removed from the col-
umns and do not substitute different tubing. To ensure
good chromatographic results, capillary tubing is cut
at the factory using a specialized precision cutter. If
you need to replace the tubing or to install a different
length tubing (to accommodate a new column configu-
ration), order an IC Cube Tubing Kit (P/N 072186).
9. Before installing the new separator column, tear off the column label and
slide it into the holder on the front of the cartridge (see Figure 9-48).
10. If the new column configuration is the same as the previous, connect the
precision cut tubing that you removed in Step 8 to the new columns.
3 250 mm Separator
2 1 Column
65 mm (2.5 in)
2 Precision Cut Tubing
4 (P/N 072188)
50 mm Guard
3 Column
3 150 mm Separator
1 Column
75 mm (3 in)
2 4 2 Precision Cut Tubing
(P/N 074603)
35 mm Guard
3 Column
1
115 mm (4.5 in)
4 Precision Cut Tubing
(P/N 072189)
Separator
1 Column
11. Remove the fitting plug from the outlet fitting on the separator column.
Orient the fitting with a flat side up and push the fitting into the opening at
the front of the column cartridge until it stops (see Figure 9-44).
12. Coil the separator column tubing inside the cartridge as shown in
Figure 9-42 or Figure 9-43. Secure the column and the inlet fitting in the
clips on the column cartridge.
13. Secure the inlet and outlet fittings on the guard column (if used) in the
column clips on the lid of the column cartridge.
14. Route the column inlet tubing from the guard column (if used) or the
separator column through the clip on the top edge of the cartridge lid.
15. Close the lid (you should hear a click) and route the tubing into the slot on
the front of the column cartridge (see Figure 9-48).
Separator Column
1
Outlet
2
2 Column Label
16. Slide the column cartridge into the IC Cube column oven and tighten the
two thumbscrews.
17. Turn on the pump flow.
18. Wait until liquid is flowing out of the Eluent Out port (3) of the injection
valve.
19. Connect the tubing from the Eluent In port of the column cartridge to the
Eluent Out port (3) of the injection valve.
20. Wait until liquid is flowing out of the Eluent Out port of the column
cartridge.
21. Reconnect the line to the Eluent Out fitting on the column cartridge that
was disconnected in Step 3 (see Figure 9-41).
22. Close the DC upper door.
12. Flush the KCl solution from the system by pumping ASTM Type I
(18 megohm-cm) filtered and deionized water through the cell. When the
conductivity drops to less than 1 S/cm, stop the pump.
13. Reconnect the pump to the injection valve and reconnect the line from the
suppressor to the cell inlet.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
Unplug cable
Disconnect lines
6. Remove the suppressor from the detector by sliding it to the left a few
millimeters to detach it from the mounting tabs on the detector. Then, pull
the suppressor toward you.
7. Orient the new suppressor with the ELUENT IN and REGEN OUT ports on
the bottom (see Figure 9-50). Press the suppressor against the back of the
detector and then slide it to the right to secure it onto the mounting tabs.
Pull out slightly on the center of the suppressor to verify that it is securely
fastened.
8. 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 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 and disconnect the tubing from the CD CELL IN
and CELL OUT ports (see Figure 9-51).
Disconnect tubing
Release Lever
4. For an analytical CD, remove the suppressor from the detector. For
instructions, refer to Section 9.27.2.
5. Press the release lever located below the detector (see Figure 9-51). The
detector pops out slightly from the DC compartment. Grasp the top of the
detector and pull outward to remove the detector from the compartment.
Do not pull from the CELL IN and CELL OUT fittings.
6. Note the electrical plug on the back of the detector and the receptacle on
the inside of the DC.
7. Push the new detector 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.
Table 9-10 lists the correct pressure range for each type of suppressor.
NOTE For a capillary IC system, disconnect the cell inlet line from
the ELUENT OUT port of the IC Cube column cartridge.
Cables
Inlet line
Outlet line
4. Grasp the cell by the cell body and pull straight out to remove it from the
detector.
Replace the gasket if there is a leak between the gasket and electrode, or
between the gasket and cell body.
Items Needed
NOTE Always wear gloves when handling the ED cell. Never touch
the electrode surface.
1. Follow the instructions in Section 9.28.1, to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.
2. Loosen the yoke knob on the yoke block by unscrewing it two to three
turns (see Figure 9-53).
Then, squeeze
the tabs on
the yoke block
and pull to
remove it
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.
Conventional
Working
Electrode Block
Yoke
Block
Cell
Body
Cell
Gasket
5. Use tweezers to remove the old cell gasket from the cell body (see
Figure 9-55).
Alignment
Conventional
Pins
Working Electrode
Gasket
6. Rinse the surface of the cell with ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5.
7. Clean the polished surface of the cell with a clean, damp lint-free tissue.
8. Install the new gasket over the alignment pins on the cell body. When
correctly installed, one end of the gasket extends beyond the cell body, to
facilitate gasket installation and removal.
9. Verify that the gasket is flat against the cell body and is not wrinkled.
10. Reinstall the working electrode block and the yoke knob and block.
Fingertighten the yoke knob by turning it a full 360 degrees.
11. Orient the cell assembly with the yoke knob on the left and push the cell
onto its mounting location in the DC compartment.
12. Reconnect the cell’s inlet and outlet lines.
13. Reconnect the electrical cables.
14. Start the pump flow.
15. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.
Items Needed
• Polishing kit (P/N 036313) shipped with the electrode. The kit contains
polishing pads (P/N 036321), a bottle of fine polishing compound
(P/N 036318), and a bottle of coarse polishing compound (P/N 036319).
• Gloves
• Tweezers
NOTE Do not use the same fine polishing pad to polish more
than one type of working electrode; this can contami-
nate the electrode surface with microparticles from the
other working electrodes.
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
the fine polishing compound.
• If you are polishing the electrode because of degradation of
performance, such as increased baseline noise or tailing peaks, first
use the coarse polishing compound. Then, repeat with the fine
compound.
a. Sprinkle about one-half gram of polishing compound in the center of
the suede side of the polishing pad. Add enough ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5 to make a thick paste.
b. Using the working electrode block, spread the paste evenly over the
pad. Then, applying firm pressure in a figure eight motion, polish the
surface of the electrode block for about one minute. If the pad dries
out while polishing, add water sparingly. However, never allow the
polishing compound to dry on the electrode.
c. Use ASTM Type I (18 megohm-cm) filtered and deionized water that
meets the specifications listed in Section 1.5 to rinse off all traces of
polishing compound from the electrode block. An ultrasonic cleaner
is effective for thoroughly cleaning the electrode block. Carefully
rinse the surface of the block with ASTM Type I (18 megohm-cm)
filtered and deionized water.
4. If you used the coarse polishing compound in Step 3, repeat the step with
the fine compound.
5. Using a moist piece of polishing cloth (with no polishing compound
added), rub the polished surface free of residual polishing compound
particles.
6. Inspect the surface of the working electrode to make sure that it is clean.
Repeat Step 5, if necessary.
NOTE The polishing pads are reusable. Do not rinse the pol-
ishing compound from the pads. After initial use, add
only enough polishing compound to maintain the coat-
ing on the pad.
7. Replace the working electrode block and yoke knob. Fingertighten the
knob by turning it a full 360 degrees.
8. Orient the cell assembly with the yoke knob on the left and push the cell
onto its mounting location in the DC compartment.
9. Reconnect the cell’s inlet and outlet lines.
10. Reconnect the electrical cables.
11. Start the pump flow.
12. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.
13. Reapply the electrode potential. The baseline will drift for more than
1 hour as the cell re-equilibrates. Peak area values may require up to
12 hours to stabilize.
Items Needed
1. Follow the instructions in Section 9.28.1 to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.
2. Unscrew the pH-Ag/AgCl reference electrode and remove it from the cell
body (see Figure 9-56).
Unscrew
the pH-Ag/AgCl
reference electrode
3. Unscrew the storage cap from the new pH-Ag/AgCl reference electrode
(see Figure 9-57). Save the cap.
Always store the electrode in the storage cap filled with saturated KCl
solution when the cell is not in use. This prevents the pH-Ag/AgCl
reference electrode membrane from drying out and damaging the
electrode. See Section 6.4 for storage instructions.
Save the
storage cap
Items Needed
4. Click the Calibration button. The Wellness panel opens, see Figure 9-58.
Capillary Installing the pH-Ag/AgCl Reference Electrode in the Cell for a Capillary
IC IC System
pH-Ag/AgCl
Reference
Electrode
O-Ring
(remove for
capillary IC)
Reference
Electrode Gasket
for Capillary IC
4. Make sure the gasket is centered in the bottom of the well and that it does
not block the inlet and outlet of the well. The inlet and outlet are small
round openings in the bottom of the well (see Figure 9-61).
Reference
Electrode Well
Inlet
Reference
Electrode Well
Outlet
7. Orient the cell assembly with the yoke knob on the left and then push the
cell onto its mounting location on the ED.
8. Connect the reference electrode cable and the cell cable.
9. Reconnect the cell inlet and outlet lines.
pH-Ag/AgCl
Reference
Electrode
O-Ring
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 and outlet lines.
5. Start the pump flow.
6. Turn on the DC power.
7. Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.
Unscrew the
pH-Ag/AgCl
reference
electrode
pH-Ag/AgCl
Reference
Electrode
O-Ring
Replace the PdH reference electrode if its sensing surface is damaged or if the
electrode no longer seals properly. Replace the PdH electrode if performance
has degraded (for example, lower response, higher background, or spikes).
The PdH reference electrode typically lasts several years, depending on use.
Items Needed
1. Follow the instructions in Section 9.28.1 to turn off the cell voltage, stop
the pump flow, and disconnect the cell from the detector.
2. Use a wrench to unscrew the PdH reference electrode nut and then
remove the nut from the reference electrode well (see Figure 9-66).
Nut
3. Pull the reference electrode out of the well (see Figure 9-67).
PdH Reference
Electrode
4. Using tweezers, remove the PdH reference electrode gasket from the well
(see Figure 9-68).
Notch in
well
PdH Reference
Electrode Gasket
6. Align the gasket so that the notched edge of the gasket aligns with the
corresponding notch in the reference electrode well and press the gasket
into the well.
PdH Reference
Electrode
Knobs
Grooves
Figure 9-70. Inserting the PdH Reference Electrode Fitting into the
Reference Electrode Well
10. Screw the nut on the PdH reference electrode into the reference electrode
well and tighten it fingertight (see Figure 9-71). After fingertightening,
use a wrench to tighten the nut an additional 20 to 30 degrees.
Nut
11. Orient the cell assembly with the yoke knob on the left and then push the
cell onto its mounting location on the ED.
12. Connect the reference electrode cable and the cell cable.
13. Reconnect the cell inlet and outlet fittings.
14. Condition the PdH reference electrode (refer to the instructions below).
6. Press the release lever located below the detector. The detector pops out
slightly from the DC compartment. Grasp the detector and pull outward to
remove the detector from the compartment.
7. Note the electrical plug on the back of the detector and the receptacle on
the inside of the DC.
8. Push the new detector into the opening in the DC and press firmly to
ensure the electrical connection is secure.
9. Reinstall the cell and reconnect the cell inlet and outlet lines and the
cables.
To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.
Use double-cone 10-32 ferrule fittings (P/N 043276) and 10-32 bolts
(P/N 043275) for all tubing connections. For tightening requirements, refer to
Installation of Dionex Liquid Line Fittings (Document No. 031432). The
manual is on the Thermo Scientific Reference Library DVD (P/N 053891).
Use a tubing cutter to cut tubing to the required length. Make sure the cut is at
a right angle to the length of the tubing and there are no nicks or burrs on the
end.
4. Select the check box for the column to be monitored (A, B, C, or D) and
click OK.
NOTE If you prefer, you can replace the injection valve “pod,”
instead of rebuilding the valve. Replacing the pod is easier
and faster than rebuilding the valve.
To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.
6. Reconnect all liquid lines to the injection valve (see Figure 9-75).
(Green)
TO INJECT SAMPLE IN
VALVE -W (from door
inject port or
autosampler)
W (6)
S (5)
25 μL SAMPLE LOOP
(Orange) L (4)
TO INJECT
VALVE -P TO INJ (Red - microbore)
VALVE -C (Black - standard bore)
1. Turn off the pump flow from the Control panel in Chromeleon 6.8 or
Chromeleon 7 or press PUMP FLOW on the front of the pump.
To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.
6. Check that the new pod has the correct number of ports for the injection
valve being serviced.
7. Align the slots in the new pod with the runner in the valve holder in the
TC (see Figure 9-77). Valve pods are keyed to fit only one way (one slot
is narrower than the other). Verify that the slots are aligned with their
matching runners.
8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-77). If necessary, twist the end of the
pod to adjust the position of the splines.
Slot (larger)
Runner (larger)
Splines
9. Push the pod into the holder until it clicks into place. Replace the black
locking ring.
10. Reconnect all liquid lines to the valve.
11. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required (see Section 9.29).
12. Close the TC door.
HIGH VOLTAGE—Disconnect the main power cord from its source and
also from the rear panel of the TC.
3. The fuse cartridge is located next to the main power switch (see
Figure 9-78). Use a small screwdriver to remove the fuse cartridge.
Fuse Cartridge
4. Replace the two fuses with new 2 A IEC 60127-2 time lag fuses
(P/N 954776). Thermo Fisher Scientific recommends always replacing
both fuses.
5. Reinstall the fuse cartridge.
6. Reconnect the main power cord and turn on the power.
ICS-5000
DP/SP DP/SP Specifications
ICS-5000
DP/SP DP/SP Reordering Information
Operation pH half-cell, 77
Analyzing samples, 172 pH limits, 145
Creating a sequence, 173 – 174 pH modifier, 43
Direct control of modules, 171 pH reading
Filling vials, 146, 149 Adjusting potentials for, 77
Loading samples, 178 Always 7.0, 271
Overview, 172 Cannot be set to 7.0, 272
Sample preparation, 147 Effect on potentials, 77
Starting a sequence, 176 – 177 Monitoring, 78
Organic solvent, 77 Nonexistent, 273
Oven (TC), 116 pH-Ag/AgCl reference electrode, 75, 77
See also Temperature control (TC) Long-term storage, 187
Oven LED (TC) O-ring replacement procedure, 399
LED is flashing, 116, 300 Replacement procedure, 392
LED is lighted, 116 See also Reference electrode
Oven LEDs (DC) Photodiode Array Detector, 3, 9
LED is flashing, 51 Regulator Bracket Kit, 35
LED is lighted, 51 Piston seal wash solution, 26, 183
Piston seal wash system, 26, 154
Activation, 26
P Dual pump seal wash option, 27, 154, 436
Replumbing the DP connections, 154
PAD Setup, 156
See Pulsed amperometry Piston seals
Palladium hydrogen (PdH) reference Replacement procedure, 316
electrode, 79 Pistons
Replacement procedure, 400 Replacement procedure, 323
Panel tabset, 11 Platinum working electrodes, 75
Home panel, 11, 149, 151 Plot, I-t, 111
How to display, 157, 165, 169, 255 – 256 Plumbing
Parameters Replacing DC tubing and fittings, 359
Chromeleon commands, 172 Replacing DP/SP tubing and fittings, 306
Peak height Replacing EG tubing and fittings, 333
Reproducibility, 69 Replacing TC tubing and fittings, 407
Peaks Plumbing configuration drawings, 129 – 139
Fronting, 118 Polarity
Reversed, 86 Analog output, 86
Tailing, 118, 222 Polishing kit (ED)
Periodic maintenance Reordering, 443
DC, 199 Polishing working electrodes, 389
DP/SP, 196 Post-column reagent addition, 61, 94, 139
TC, 201 Potassium carbonate eluent, 41, 43
pH gradient, 77 Potassium hydroxide eluent, 41
Waveforms, 105
Cyclic voltammetry, 105
Defining, 108
Integrated amperometry, 107
Integrated amperometry example, 104
Maximum length, 107
Pre-programmed, 108
Pulsed amperometry example, 103
Weekly maintenance
DC, 199
DP/SP, 195
EG, 197
TC, 201
Wellness, 128
Wireframe plot, 112
Working electrodes, 75
Maintenance, 143
Materials, 75
Polishing, 389
Z
Zero position (analog out), 86