Man IC ICS 5000+ Operators Manual Nov2012 Doc065446 01
Man IC ICS 5000+ Operators Manual Nov2012 Doc065446 01
Man IC ICS 5000+ Operators Manual Nov2012 Doc065446 01
Operator's Manual
Contents
1 Introduction
1.1
1.1.2
1.2
1.3
1.4
1.5
1.4.1
1.4.2
Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
1.4.3
Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . 19
2 Description
DP/SP Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.1
2.2
Pump Heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
2.2.2
Pressure Transducer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.2.3
2.2.4
2.2.5
2.3
2.2.6
2.2.7
2.2.8
2.3.2
2.4
2.5
Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
2.5.1
EO (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
2.5.2
2.5.3
Filtering Eluent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
EG Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
2.6
EG Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
2.7
EG Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
2.8
EG Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
2.9
EG Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
DC Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
2.10 DC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
2.11 DC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
2.11.1 DC Interior Components for Capillary IC . . . . . . . . . . . . . . 58
2.11.2 IC Cube for Capillary IC . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
2.11.3 DC Interior Components for Analytical IC . . . . . . . . . . . . . 64
2.12 DC Temperature Control Zones . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
2.13 High-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
ii
Contents
iii
TC Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
2.20 TC Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
2.21 TC Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 121
2.22 TC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
2.23 Injection Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
2.23.1 Injection Valve Operation . . . . . . . . . . . . . . . . . . . . . . . . . . 126
2.23.2 Injection Valve Plumbing . . . . . . . . . . . . . . . . . . . . . . . . . . 128
2.24 Column Identification (ID) System . . . . . . . . . . . . . . . . . . . . . . . . . 129
2.25 Gas and Humidity Sensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
2.26 TC Theory of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
2.26.1 Predictive Performance . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
3 Configurations
3.1
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135
4 Startup
4.1
4.2
iv
4.1.2
Contents
4.3
4.4
4.5
4.3.2
4.3.3
4.3.4
4.4.2
4.5.2
4.7
4.8
EG Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
4.9
DC Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.11 Starting the DC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
4.12 Equilibrating the System and Verifying Operational Readiness . . . 170
TC Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
4.13 Starting the TC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
5 Operation
5.1
5.2
5.3
5.4
5.2.1
5.2.2
5.2.3
5.3.2
5.3.3
6 Shutdown
DP/SP Shutdown. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
EG Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 189
6.1
6.2
DC Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 191
6.3
6.4
vi
Contents
6.4.2
TC Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 193
6.5
6.6
6.7
7 Maintenance
7.1
7.1.2
7.1.3
7.1.4
7.3
7.4
7.5
7.7
7.8
vii
8 Troubleshooting
8.1
8.1.2
8.1.3
8.1.4
8.2
8.3
8.4
8.5
8.6
No Peaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 225
8.7
8.8
8.9
viii
Contents
EG Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 245
8.19 Troubleshooting EG Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 245
8.20 EG ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257
8.21 EG POWER LED Fails to Light . . . . . . . . . . . . . . . . . . . . . . . . . . . 258
8.22 Liquid Leaks in the EG . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 258
8.23 No Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259
8.24 EG Stops Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 260
DC Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263
8.25 Troubleshooting DC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 263
8.26 Liquid Leaks from DC Components . . . . . . . . . . . . . . . . . . . . . . . . 274
8.27 VALVE Button Not Working . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275
8.28 ED Cell Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275
8.28.1 ED Cell pH Readout Always 7.0 . . . . . . . . . . . . . . . . . . . . 275
8.28.2 Cannot Set ED Cell pH Readout to 7.0 . . . . . . . . . . . . . . . . 276
8.28.3 Shift in ED Cell pH Readout . . . . . . . . . . . . . . . . . . . . . . . 276
ix
TC Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 279
8.29 Troubleshooting TC Error Messages . . . . . . . . . . . . . . . . . . . . . . . . 279
8.30 TC ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 303
8.31 Liquid Leaks from TC Components . . . . . . . . . . . . . . . . . . . . . . . . 304
8.32 TC Temperature Does Not Increase . . . . . . . . . . . . . . . . . . . . . . . . . 305
8.33 TC Temperature Stabilizer Not Operating Properly . . . . . . . . . . . . 305
9 Service
9.1
9.2
9.4
9.5
9.6
9.7
9.5.1
9.5.2
9.6.2
Contents
9.8
9.9
9.7.2
9.7.3
9.7.4
9.7.5
9.7.6
9.8.2
9.8.3
EG Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 335
9.12 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 335
9.12.1 Tubing and Fittings for Capillary IC EG Channels . . . . . . 335
9.12.2 Tubing and Fittings for Analytical IC EG Channels . . . . . 337
9.13 Isolating a Restriction in the Liquid Lines . . . . . . . . . . . . . . . . . . . . 338
9.14 Replacing the EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 338
9.14.1 Removing the Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . 339
9.14.2 Disposing of the Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . 341
9.14.3 Storing the Old EGC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 342
9.14.4 Installing and Conditioning a New Capillary EGC . . . . . . 343
9.14.5 Installing and Conditioning a New Analytical EGC . . . . . . 347
xi
DC Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 365
9.19 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 365
9.19.1 Tubing and Fittings for Capillary IC Systems . . . . . . . . . . 365
9.19.2 Tubing and Fittings for Analytical IC Systems . . . . . . . . . 368
9.20 Connecting a Sample Loading Port to the Injection Valve . . . . . . . 369
9.21 Replacing the Leak Sensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 370
9.22 Rebuilding a High-Pressure (Injection) Valve . . . . . . . . . . . . . . . . . 372
9.23 Replacing a High-Pressure (Injection) Valve Pod . . . . . . . . . . . . . . 373
9.24 Installing or Replacing an I/O Option Board . . . . . . . . . . . . . . . . . . 376
9.25 Changing the DC Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . 377
9.26 IC Cube Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 379
9.26.1 Replacing an IC Cube Cartridge . . . . . . . . . . . . . . . . . . . . . 379
9.26.2 Replacing Capillary Columns . . . . . . . . . . . . . . . . . . . . . . . 380
9.27 CD Service Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 386
9.27.1 Calibrating the CD Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . 386
9.27.2 Replacing an Analytical Suppressor . . . . . . . . . . . . . . . . . . 387
9.27.3 Replacing a CD . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 389
xii
Contents
TC Service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 413
9.29 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 413
9.30 Setting Up the Column ID System . . . . . . . . . . . . . . . . . . . . . . . . . . 414
9.31 Rebuilding an Injection Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 416
9.32 Replacing an Injection Valve Pod . . . . . . . . . . . . . . . . . . . . . . . . . . 417
9.33 Changing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . 419
A Specifications
DP/SP Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 421
EG Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 425
DC Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 429
xiii
TC Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 439
B Reordering Information
DP/SP Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . 441
EG Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 445
DC Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 447
TC Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 451
xiv
1 Introduction
1.1
ICS-5000+ Conductivity
Dionex
Detector (EG)
the Dionex ICS-5000+ system can be used for long periods of continuous
operation and minimal eluent consumption.
The dual-analysis capabilities (both simultaneous and sequential) of the
Dionex ICS-5000+ system let you maximize efficiency and throughput and
minimize downtime. The modular system design lets you quickly configure
and customize hardware.
The single-channel Dionex ICS-5000+ can be configured to run either
capillary IC applications or analytical (microbore or standard bore) IC
applications.
1 Introduction
1.1.1
Eluent Generator
Eluent Organizer
Detector/Chromatography
Compartment
IC Cube (inside DC)
Detector (inside DC)
Product Name
Page
+
page 4
page 4
Dionex
ICS-5000+
Eluent Generator
page 4
Dionex
ICS-5000+
Eluent Organizer
page 6
Dionex ICS-5000
Detector/Chromatography Module
page 6
page 7
ICS-5000+
page 7
Dionex
Detector
Conductivity
page 7
page 7
page 9
page 9
Thermal Compartment
page 8
Autosampler
page 8
page 9
page 10
Mass Spectrometer
Dionex ICS-5000+ Dual Pump (DP) and Dionex ICS-5000+ Single Pump
(SP)
The DP contains two pumps in any combination of the three types listed
above (for example, two isocratic capillary IC pumps, or two isocratic
analytical IC pumps, or one isocratic capillary IC pump and one gradient
analytical IC pump).
The second pump in the DP can be operated as a second-channel
chromatography pump, an auxiliary dependent pump, or an auxiliary
independent pump.
Capillary
IC
Capillary IC pumps operate at flow rates ranging from 0.001 to 3.0 mL/min
and operating pressures up to 41 MPa (6000 psi).
Analytical IC pumps operate at flow rates ranging from 0.00 to 10.0 mL/min
and operating pressures up to 41 MPa (6000 psi). Both microbore and
standard bore IC applications are supported.
Dionex ICS-5000+ Eluent Generator (EG)
The EG generates high purity acid or base eluents online from deionized
water. The EG can be configured for single- or dual-channel operation. Each
channel includes:
1 Introduction
For each channel, the following options must be ordered separately for
installation inside the EG:
The EO holds eluent reservoirs in a liner that contains spills and leaks. Up to
two EOs can be installed on top of the DC. Each EO accommodates up to four
1-liter or 2-liter reservoirs or up to two 4-liter reservoirs. The EO is typically
ordered configured with four 2-liter reservoirs (P/N 072058).
All eluent reservoirs available for use with the DP/SP can be pressurized. If
you plan to pressurize the eluent reservoirs, the optional EO Regulator
Accessory and Stand (P/N AAA-074423) is required.
The Regulator Accessory includes a pressure regulator and gauge assembly
with four outputs (for connections to four eluent reservoirs), as well as the
tubing and connection fitting required. If more reservoirs are required, order a
second regulator (P/N 074422).
Reagent-Free IC with Electrolytic Sample Preparation (RFIC-ESP)
The DC provides a temperature-controlled environment for Dionex ICS5000+ chromatography components. The DC can accommodate components
for two channels, plumbed either serially or in parallel.
The following components may be installed in the DC:
Conductivity detectors
Electrochemical detectors
Injection valves
1 Introduction
Switching valves
Suppressors
The TC provides a temperature-controlled environment for Dionex ICS5000+ chromatography components. The TC is intended for applications that
do not require conductivity or electrochemical detection.
The TC is available in four configurations:
With one 2-position, 6-port high-pressure injection valve and one 2position, 10-port high-pressure injection valve
1 Introduction
1.1.2
10
1 Introduction
a panel tabset. In both the ePanel Set and the panel tabset, a convenient Home
panel shows the overall system status and provides basic module control
functions. Individual tabs provide quick access to additional functions for
each module and detailed status and diagnostics functions. Figure 1-2 shows
the Home panel in Chromeleon 7 and Figure 1-3 shows the Home panel in
Chromeleon 6.8.
11
Figure 1-3. Chromeleon 6.8 Panel Tabset (Dionex ICS-5000+ Home Panel
Shown)
12
1 Introduction
1.2
Part
Number
PDF
File
Printed
Manual
065446
Yes
No
065447
Yes
Yes
065361
Yes
No
065147
Yes
No
065141
Yes
No
071686
Yes
Yes
071679
Yes
Yes
N/A
N/A
N/A
4829.5060
Yes
No
031883
Yes
No
N/A
N/A
N/A
All Adobe PDF files listed above are shipped on the Thermo Scientific
Reference Library DVD (P/N 053891), which is included in the ship kit of
each Dionex ICS-5000+ system module. In addition, the software manuals are
provided as PDF files on the Chromeleon DVD. A printed copy of the
software installation instructions is provided in the software ship kit.
Consumables documentation: For complete information about Dionex
columns, suppressors, eluent generator cartridges, etc., refer to the appropriate
13
1.3
Index entries
If you are not familiar with how to navigate PDF files, refer to the Help
system for Adobe Acrobat or Adobe Reader for assistance.
14
Chapter 1
Introduction
Chapter 2
Description
Chapter 3
System
Configurations
Chapter 4
Getting Started
Chapter 5
Operation
Chapter 6
Shutdown
1 Introduction
1.4
Chapter 7
Maintenance
Chapter 8
Troubleshooting
Chapter 9
Service
Appendix A
Specifications
Appendix B
Reordering
Information
1.4.1
15
properly followed. Safety messages appear in bold type and are accompanied
by icons, as shown below.
Indicates an imminently hazardous situation which, if not avoided, will
result in death or serious injury.
Indicates a potentially hazardous situation which, if not avoided, could
result in death or serious injury.
Indicates a potentially hazardous situation which, if not avoided, may
result in minor or moderate injury. Also used to identify a situation or
practice that may seriously damage the instrument, but will not cause
injury.
Indicates that the function or process of the instrument may be
impaired. Operation does not constitute a hazard.
Signale une situation de danger potentiel qui, si elle n'est pas vite,
pourrait entraner des blessures graves mortelles.
Signale une situation de danger potentiel qui, si elle n'est pas vite,
pourrait entraner des blessures mineures modres. galement
utilis pour signaler une situation ou une pratique qui pourrait
gravement endommager l'instrument mais qui n'entranera pas de
blessures.
Warnhinweise in Deutsch
Bedeutet unmittelbare Gefahr. Miachtung kann zum Tod oder
schwerwiegenden Verletzungen fhren.
16
1 Introduction
Notes
Informational messages also appear throughout this manual. These are labeled
NOTE and are in bold type:
NOTE
Capillary
IC
Sections preceded with the Capillary IC flag indicate that the information in
the section applies to capillary IC systems only.
Sections preceded with the Analytical IC flag indicate that the information in
the section applies to analytical IC systems only.
If a section is not flagged, the information in the section applies to both
capillary IC and analytical IC systems.
1.4.2
Safety Symbols
These symbols appear on the Dionex ICS-5000+ modules or on labels affixed
to the modules:
Alternating current
Primary protective conductor terminal
Secondary protective conductor terminal
Power supply is on
Power supply is off
17
18
1 Introduction
1.4.3
Declaration of Conformity
The cETLus or cTUVus and CE marks on the model/data labels on each
Dionex ICS-5000+ module indicate that the modules are in compliance with
the following standards.
19
1.5
Specification
IonsResistivity
>18.0 (megohm-cm)
OrganicsTOC
<10 ppb
Iron/Transition Metals*
<1 ppb
Pyrogens
<0.03 (Eu/mL)
<1 (units/mL)
ColloidsSilica
<10 ppb
Bacteria
<1 (cfu/mL)
20
2 Description
ICS-5000+
DP/SP
2.1
DP/SP Description
DP/SP Front Features
A status bar on the front of the DP and SP includes buttons for controlling
certain pump functions, as well as LEDs (light emitting diodes) that indicate
the status of several pump functions (see Figure 2-1 and Figure 2-2).
FLOW
CONNECTED
ALARM
PRIME
PUMP 1
FLOW
PRIME
PUMP 2
FLOW
CONNECTED
ALARM
PRIME
PUMP 1
21
Button/LED
Label
If the LED Is On
CONNECTED
ALARM
A DP/SP-related problem
has occurred (for example,
a pressure limit was
activated). Check the
Chromeleon audit trail for
the cause.
PUMP 1 FLOW*
PUMP 2 FLOW**
PUMP 1 PRIME*
PUMP 2 PRIME**
POWER
22
2 Description
2.2
Status Bar
Priming Valve
Pressure Transducer
9
10
11
12
Handle (2)
13
14
Leak Sensor
9
6
9
10
11
12
13
9
10
12
14
23
Vacuum Degas
Chambers (four
channels)
Proportioning
Valve Fittings
Proportioning
Valve Outlet to
Primary Pump
Head
Static Mixer
Pump Outlet to
EG or Injection
Valve
3
5
4
2.2.1
For easier access to pump components when performing service procedures, the pump panel can be pulled forward to the
front of the pump compartment. First, check that the five red
Phillips screws installed on the component mounting panel
before shipment from the factory have been removed. Then,
use the handles to pull the panel forward. The upper and
lower component panels slide forward together.
Pump Heads
The DP/SP is a low-pulsation, serial dual-piston pump with electronic
compressibility compensation. Two pump headsa primary head and a
secondary headare connected in series. Eluent passes through both pump
heads in succession.
The primary pump head delivers eluent at the selected flow rate, while
simultaneously filling the secondary pump head. The latter serves as a
reservoir and delivers eluent while the primary head carries out the refill
stroke.
The characteristic feature of the patented isokinetic pre-compression phase is
the programmed overlapping of the delivery strokes of the two pump heads.
When delivering compressible liquids without controlled pre-compression,
24
2 Description
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.
2.2.2
Pressure Transducer
The secondary pump head contains a built-in pressure transducer to measure
the system pressure. The instrument control firmware installed in the DP/SP
precisely controls the pump motor speed to ensure flow rate accuracy and to
maintain constant flow and constant pressure.
2.2.3
2.2.4
25
Make sure the run time is long enough to ensure that the vacuum degassing module delivers the optimal degassing performance.
2.2.5
The piston seal wash system is designed for use with only one of the two
pumps in a DP module. When the DP is shipped from the factory, the seal
wash system is connected to pump 1 (the bottom pump). If necessary, connect
26
2 Description
the seal wash system to pump 2 (the top pump), instead. For instructions on
how to replumb the system, see Section 4.7.
NOTE
2.2.6
2.2.7
27
For details about a column, refer to the column manual. Column manuals are
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
High-Pressure Trap Column
Part Number
079017
079018
079019
075976
075977
075978
075979
2.2.8
28
2 Description
2.3
2.3.1
OUTLET
CHECK VALVE
SECONDARY
PUMP
HEAD
PRIMARY
PUMP
HEAD
DI WATER
OR
ELUENT
INLET
CHECK VALVE
VACUUM
DEGAS
PULSE
DAMPER*
TO ELUENT GENERATOR
OR INJECTION VALVE
ELUENT SUPPLY
ON/OFF VALVE
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.
29
2.3.2
OUTLET
CHECK VALVE
SECONDARY
PUMP
HEAD
ELUENT
A
ELUENT
C
ELUENT
B
ELUENT
D
PRIMARY
PUMP
HEAD
INLET
CHECK VALVE
VACUUM
DEGAS
STATIC
MIXER
A
PROPORTIONING
VALVE D
TO ELUENT GENERATOR
OR INJECTION VALVE
30
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 Description
2.4
4
3
5
6
USB Receptacle
(B Connectors)
Drain Port
7
8
The tubing chases route tubing from the front of the DP/SP, through the
interior of the module, and to the rear panel.
Main Power Switch, Fuse Holder, and Power Receptacle
The rear panel power switch is the main power switch for the DP/SP. Turn on
the main power switch before initial operation and leave it on unless
instructed to turn it off (for example, before performing a service procedure).
31
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.
Le cordon d'alimentation principal est utilis comme dispositif principal
de dbranchement. Veillez ce que la prise de base soit situe/installe
prs du module et facilement accessible.
Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen
Sie sicher, da sich die Steckdose nahe am Gert befindet und leicht
zugnglich ist.
The digital I/O port provides a connection to auxiliary devices. The connector
includes three TTL inputs and four relay outputs. Table 2-2 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.
Pin Number
Signal Name
Signal Level
Description
-----
-----
Not used
-----
-----
Not used
Relay 3 Out
Potential-free
Normally open
Relay 1 Out
Potential-free
Normally closed
Relay 2 Out
Potential-free
Normally closed
Relay 3 Out
Potential-free
Normally closed
32
2 Description
Pin Number
Signal Name
Signal Level
Description
Relay 1 Out
Potential-free
Common
Relay 2 Out
Potential-free
Common
Gnd
Ground
Ground
10
Gnd
Ground
Ground
11
Gnd
Ground
Ground
12
Gnd
Ground
Ground
13
-----
-----
Not used
14
Relay 4 Out
Potential-free
Normally open
15
Relay 4 Out
Potential-free
Common
16
Relay 4 Out
Potential-free
Normally closed
17
-----
-----
Not used
18
Relay 3 Out
Potential-free
Common
19
Relay 1 Out
Potential-free
Normally open
20
Relay 2 Out
Potential-free
Normally open
21
Vcc Out
+5V
+5V, 500 mA
22
TTL Input 1
TTL
Hold/Run
23
TTL Input 2
TTL
Stop
24
TTL Input 3
TTL
Start
25
-----
-----
Not used
The analog pressure output indicates the operating pressure of the pump. The
pressure output is set to 50 mV/MPa (5 mV/14.51 psi). To monitor the
pressure, connect the pressure output to a recorder or an A/D converter. These
are the pin assignments for the 2-pin Cinch connector (P/N 8005.9001A):
Signal Level
Function
Inner ring:
Signal (pressure)
Outer ring:
Ground
33
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 Command window (Chromeleon 7) or the
Commands dialog box (Chromeleon 6.8).
3. Select the pump name.
4. Select the AnalogOut property and select PumpTop.
5. For Chromeleon 6.8, click Execute.
USB Connections
One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the pump ship kit:
Pump Ship Kit
Part Number
072112
062463
072111
063342
34
One waste line is connected to the secondary pump head on each pump
and is routed through the tubing chase to the rear of the DP/SP.
The drain port removes any liquid that collects in the drip tray in the
bottom of the DP/SP. A clear corrugated drain hose (P/N 055075) is
connected to this port during installation.
2 Description
Place the free ends of the waste lines and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
pump.
For correct drainage, make sure the waste lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.
2.5
Eluent Reservoirs
The following reservoirs are available for use with the DP/SP:
2.5.1
EO (Optional)
The Dionex ICS-5000+ Eluent Organizer (EO) holds eluent reservoirs in a
liner that contains spills and leaks. Up to two EOs can be installed on top of
the DC. Each EO accommodates up to four 1-liter or 2-liter reservoirs or up to
two 4-liter reservoirs. The EO is typically ordered configured with four 2-liter
reservoirs (P/N 072058).
2.5.2
35
Setzen Sie den Eluentbehlter auf keinen Fall einem Druck ber
0,07 MPa aus.
36
2 Description
2.5.3
Filtering Eluent
37
38
ICS-5000+
EG
2.6
EG Description
EG Front Features
The status bar on the front of the Dionex ICS-5000+ Eluent Generator (EG)
includes buttons that provide control of certain EG functions, as well as LEDs
that indicate the status of several EG functions (see Figure 2-8).
1
CONNECTED
ALARM
EGC
CR-TC
If the LED Is On
Comment
CONNECTED
The EG is connected to a
Chromeleon 7 instrument or
a Chromeleon 6.8 timebase.
-----
ALARM
EGC 1
EGC 2
39
Button/LED
Label
If the LED Is On
Comment
CR-TC 1
CR-TC 2
POWER
2.7
EG Interior Components
The EG component compartment, which is located directly behind the front
door, accommodates the components required for generating eluent in a single
system or in both channels of a dual system. A component mounting panel
divides the compartment into two sections:
40
2 EG Description
EGC (Capillary)
CR-TC (Capillary)
Leak Sensor
Drip Tray
2
Note:
For a capillary IC
system, the eluent
degasser is installed in
the IC Cube.
3
4
41
RFIC+ Eluent
Degasser (for
Analytical IC only)
Electrical Cables
CR-TC (Analytical)
Drip Tray
Figure 2-10. Example EG Interior Components for an Analytical (StandardPressure) IC System (System 2 of a Dual-Channel EG Shown)
42
2 EG Description
Electrical Cables
CR-TC (Analytical)
Drip Tray
Figure 2-11. Example EG Interior Components for an Analytical (HighPressure) IC System (System 1 Shown)
Eluent Generator Cartridge (EGC)
Table 2-3 lists the versions of eluent generator cartridges available for use
with the EG. Each Dionex EGC contains an electrolyte concentrate solution
appropriate for the particular eluent generation. Each Dionex EGC is designed
to be used in either a capillary IC system or an analytical IC system. A Dionex
EGC designed for a capillary IC system cannot be used in an analytical IC
system, and vice versa.
Analytical IC systems typically include Dionex EGC 500 cartridges.
Although it is possible to operate high-pressure analytical systems with
Dionex EGC 300 cartridges and (if required for the application) the Thermo
Scientific Dionex EPM 300 Electrolytic pH Modifier, this will limit the
43
operating pressure to 21 MPa (3000 psi). Thermo Fisher Scientific does not
currently offer a Dionex EPM for high-pressure systems.
Dionex EGC Version
Part
Number
Function
072076
072077
074536
080135
074532
074534
074535
074533
075778
075779
For more information, refer to the Dionex EGC manual. The manual is
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
44
2 EG Description
The Dionex CR-TC is a high-pressure, electrolyticallyregenerated trap column. The Dionex CR-TC is designed
to remove anionic or cationic contaminants in the eluent
or deionized water and to reduce drift during gradient
separations. The following versions of the Dionex CR-TC
can be used with the EG:
Dionex CR-TC Version
IC System
Type
Part
Number
Capillary
072078
Capillary
072079
Analytical
(All)
075550
Analytical
(All)
075551
For more information, refer to the Dionex CR-TC manual. The manual is
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
NOTE
NOTE
The Thermo Scientific Dionex IonPac ATC-HC Trap Column (P/N 059604) or IonPac CTC-1 Trap Column
(P/N 040192) may be used with Dionex EGC 300 cartridges.
The Thermo Scientific Dionex ATC-HC 500 Trap Column
(P/N 075958) or IonPac CTC 500 Trap Column
(P/N 075977) can be used with Dionex EGC 500 cartridges.
However, all of these IonPac trap columns require off-line
chemical regeneration. Contact Technical Support for Dionex
products for more information.
45
The Dionex EGC 300 K2CO3 can be used with a Dionex EPM 300
Electrolytic pH Modifier (P/N 080135) and a carbonate mixer (2 mm,
P/N 063443; 4 mm, P/N 079943) to produce a carbonate/bicarbonate
mixture for use with anion exchange separations on carbonate-based IonPac
columns.
After the cartridge generates potassium carbonate eluent, the Dionex 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 Dionex EGC manual.
Dionex EGC manuals are provided on the Thermo Scientific Reference
Library DVD (P/N 053891).
NOTE
46
2 EG Description
Leak Sensor
If liquid collects in the drip tray in the bottom of the EG, a leak sensor reports
the leak to Chromeleon and an error message is displayed in the audit trail. In
addition, the Alarm LED on the EG front panel lights.
Electrical Connections
Two CR-TCs
When operating with a Dionex EGC 300 K2CO3 and the Dionex EPM 300,
the Dionex EGC is connected to the Dionex EGC power supply for one
channel and the Dionex EPM is connected to the Dionex EGC power supply
for the second channel. Thus, the EG can accommodate only one such
configuration.
47
2.8
EG Rear Panel
Figure 2-13 illustrates the rear panel of the EG.
1
Exhaust Fan
USB Receptacle
(B Connector)
Tubing Chase
Drain Port
3
4
6
5
7
8
The exhaust fan cools the interior of the EG and exhausts any oxygen and
hydrogen gases that escape during operation.
USB Connections
48
2 EG Description
One 1.8 m (6 ft) USB cable (P/N 960777) is provided in the EG Ship Kit
(P/N 075780).
Fuse Holder, Main Power Switch, and Power Receptacle
The fuse cartridge contains two 2-amp slow-blow fuses (P/N 954773). For
instructions on how to change the fuses, see Section 9.18.
The rear panel power switch is the main power switch for the EG. Turn on the
main power switch before initial operation and leave it on unless instructed to
turn it off (for example, before performing a service procedure).
NOTE
For routine on/off control, use the POWER button on the front
of the EG (see Figure 2-8). To turn off the EG, press and hold
the POWER button for 2 seconds.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the EG and is easily accessible.
Le cordon d'alimentation principal est utilis comme dispositif principal
de dbranchement. Veillez ce que la prise de base soit situe/installe
prs du module et facilement accessible.
Das Netzkabel ist das wichtigste Mittel zur Stromunterbrechung. Stellen
Sie sicher, da sich die Steckdose nahe am Gert befindet und leicht
zugnglich ist.
Tubing Chase
The tubing chase routes tubing from the front of the EG, through the interior
of the module, and to the rear panel.
Suppressor, Vent, and Drain Lines
The lines exiting the tubing chase (white tubing) are for connecting the
REGEN IN port on the Dionex RFIC+ Eluent Degasser or Dionex EPM 300
Electrolytic pH Modifier to the REGEN OUT port on the suppressor.
The gas vent lines (clear tubing) discharge the electrolysis gas (H2 or O2)
that is vented from the Dionex EGC electrolyte reservoir and the Dionex
RFIC+ Eluent Degasser.
49
The drain port removes any liquid that collects in the drip tray in the
bottom of the EG. A clear corrugated drain hose (P/N 055075) is
connected to this port during installation.
Place the free ends of the vent lines and drain hose into a waste container. To
maintain a positive siphon, position the waste container below the level of the
EG.
For correct drainage, make sure the vent lines and drain hose are not
bent, pinched, or elevated at any point. Do not allow the ends of the
lines to be submerged in waste liquid.
2.9
EG Flow Schematics
Liquid flows through the EG components in the following order:
The pump delivers deionized water to the Dionex EGC. Direct current is
applied to the Dionex EGC to produce eluent.
After exiting the degasser, the eluent flows through the backpressure coil
(if installed), through the injection valve to the separator column, and
finally to the detector cell.
The flow paths for a capillary IC and an analytical IC system are the same.
However, in a capillary IC system, a degasser cartridge is located in the IC
Cube inside the DC. In an analytical IC system, the degasser is located inside
the EG.
Capillary
IC
Figure 2-14 illustrates the liquid flow path through an EG configured for a
capillary IC system.
Figure 2-15 illustrates the liquid flow path through an EG configured for an
analytical IC system. Figure 2-16 illustrates the liquid flow path through an
EG configured for a high-pressure analytical IC system.
50
2 EG Description
Vent
EGC
(Capillary)
EGC
IN
EGC
OUT
TO PUMP/DAMPER
To Inject
Valve
ELUENT IN
To EG Degas
Regen Out
(blue label)
REGEN IN
ELUENT OUT
To CR-TC
Eluent In
(red label)
REGEN OUT
ELUENT OUT
WASTE, GAS
SEPARATOR
To CR-TC
Regen Out
(blue label)
EG
Degas
Cartridge
(inside DC)
To CR-TC
Eluent Out
(yellow label)
To CR-TC
Regen In
(orange label)
To EG Degas
Eluent In
(red label)
51
EGC VENT
EGC
RFIC+
Eluent
Degasser
To Waste
Vent
(via EG
rear wall)
Eluent
Out
Inlet
Outlet
EGC
IN
To
Waste
EGC
OUT
TO PUMP
Eluent
In
Coupler
(via EG
rear wall)
TO INJ VALVE - P
TO CR -TC
REGEN OUT
(blue label)
To CR-TC
Eluent In
(red label)
To CR-TC
Regen In
(orange label)
To CR-TC
Eluent Out
(yellow label)
REGEN IN
WASTE, GAS
SEPARATOR
Coupler
ELUENT OUT
TO SRS/AES
REGEN OUT
CR-TC
52
2 EG Description
EGC VENT
RFIC+
Eluent
Degasser
EGC
Vent
To Waste
Eluent
Out
(via EG
rear wall)
Inlet
Eluent
In
Outlet
To Waste
EGC
IN
TO PUMP
EGC
OUT
Coupler
(via EG
rear wall)
TO INJ VALVE - P
Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Eluent In
(red label)
To CR-TC
Eluent Out
(yellow label)
REGEN IN
TO CR -TC
REGEN OUT
(blue label)
ELUENT OUT
WASTE, GAS
SEPARATOR
To CR-TC
Regen In
(orange label)
CR-TC
Refer to the Dionex EGC-CO3 Mixer manual for a flow schematic showing the components required to generate a carbonate/bicarbonate mixture. The manual is provided on the
Thermo Scientific Reference Library DVD (P/N 053891).
53
54
ICS-5000+
DC
2.10
DC Description
DC Front Features
The status bar on the front of the Dionex ICS-5000+
Detector/Chromatography Module (DC) (see Figure 2-17) includes buttons
for controlling certain DC functions, as well as LEDs that indicate the status
of several DC components and functions.
1
CONNECTED
ALARM
SUPPRESSOR
UPPER
LOWER
OVEN
LOAD
INJECT
LOAD
VALVE 1
INJECT
VALVE 2
If the LED Is On
CONNECTED
The DC is connected to a
Chromeleon 7 instrument or a
Chromeleon 6.8 timebase.
ALARM
SUPPRESSOR 1
SUPPRESSOR 2
OVEN UPPER
OVEN LOWER
55
Button/LED
Label
If the LED Is On
VALVE 1 LOAD
VALVE 2 LOAD
VALVE 1 INJECT
VALVE 2 INJECT
POWER
NOTE
The two sample loading ports on the front of the DC (see Figure 2-18) can be
connected to injection valves installed inside the DC. A syringe can then be
used to manually load sample through the ports. For automated sample
56
2 DC Description
Sample
Loading Ports
2.11
DC Interior Components
The interior of the DC consists of two temperature-controlled compartments
(upper and lower). To access the upper compartment, lift up the top door. To
access the lower compartment, pull down the lower door.
The upper and lower compartments are isolated from each other in separate
temperature zones. There is no common air flow between the two
compartments. For details about DC temperature control, see Section 2.12.
The compartments can accommodate the components required for up to two
IC systems. The following configurations are possible:
57
Capillary
IC
58
The top section houses one or two Dionex ICS-5000+ IC Cubes (IC
Cubes). For details about the IC Cube, see Section 2.11.2. The tray slides
forward for easy access to components.
2 DC Description
Figure 2-19 shows the upper compartments of a DC that is configured for two
capillary IC systems. Both systems are configured for conductivity detection.
Conductivity Detector
(Capillary) (System #1)
Conductivity Detector
(Capillary) (System #2)
59
Suppressor Cartridge
or Suppressor Bypass
Cartridge
EG Degas Cartridge
Injection Valve
The Dionex CRD 200 (Capillary) cartridge (P/N 072054) contains a Dionex
CRD 200 Carbonate Removal Device (Capillary). The Dionex CRD 200
(Capillary) removes the carbonate peak contributed by the sample in
hydroxide eluent chemistries. Removal occurs immediately after suppression
of the eluent, before the sample reaches the detector. The Dionex CRD 200
(Capillary) is optimized for operation at the flow rate range typically used
with capillary columns.
The Dionex CRD and tubing connections inside the cartridge are not
accessible. Tubing exits the front of the cartridge to allow connection to other
capillary IC components.
60
2 DC Description
61
Capillary
IC
EG Degas Cartridge
The EG degas (capillary) cartridge contains a tubing assembly that purges the
electrolysis gas from eluent that has been generated by an EG. After passing
through the degas tubing, the eluent is directed to the injection valve and then
to the guard and separator columns.
The EG degas (capillary) cartridge also contains plumbing connections that
route the regenerant flow from the suppressor out of the IC Cube to the
regenerant inlet port of the Continuously Regenerated Trap Column
(Capillary) in the EG.
If the system does not include an EG, the eluent inlet line from the EG degas
cartridge is connected directly to the pump outlet. The regenerant outlet line is
directed to waste.
Capillary
IC
The numbers on the schematic shown in Figure 2-21 indicate the flow path of
eluent and regenerant through the plumbing connections on an IC Cube
configured for conductivity detection.
ELUENT IN
ELUENT IN
ELUENT IN
14
ELUENT OUT
CRD 200
CES 300
ELUENT OUT
REGEN IN
ELUENT OUT
To Waste
ELUENT OUT
From
Autosampler
REGEN OUT
ELUENT OUT
ELUENT IN
EG
DEGAS
SAMPLE IN
10
13
ELUENT IN
SAMPLE OUT
CELL IN
11
To CR-TC
Regen In Port
12
From CR-TC
Eluent Out Port
CELL OUT
Conductivity Detector
(Capillary)
62
2 DC Description
NOTE
The numbers on the schematic shown in Figure 2-22 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
ELUENT OUT
4
CRD
BYPASS
From
Autosampler
To Waste
10
SUPPRESSOR
BYPASS
ELUENT OUT
ELUENT IN
To CR-TC
Regen In Port
EG
DEGAS
REGEN IN
SAMPLE IN
SAMPLE OUT
1
ELUENT IN
From CR-TC
Eluent Out Port
EC CELL
OUT
IN
63
Automation
Manager
Components
Electrochemical
Detector and Cell
Conductivity
Detector and
Suppressor
Lower Compartment
Columns and
Injection
Valves
64
2 DC Description
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 electricallyactivated, two-position valves. See Section 2.13 for details about the injection
valves.
The compartment tray slides forward about 10 cm (4 in) for easy access to
columns and valves. To pull the tray forward, use the handle installed in the
center of the compartment (see Figure 2-24).
65
2.12
Capillary
IC
DC upper compartment
DC lower compartment
The temperatures achieved for a particular zone can vary from the control
range, depending on the ambient temperature (see Table 2-4).
Temperature
Zone
Control
Range
Upper
compartment
10 to
40 C
Lower
compartment
10 to
70 C
CD cell
15 to
60 C
IC Cube column
heater
15 to
80 C
RCH-1
20 to
80 C
66
2 DC Description
67
2.13
High-Pressure Valves
Up to four high-pressure valves can be installed in the DC. The following
valve models are available: 4-port (P/N 074525), 6-port (P/N 075917), and
10-port (P/N 075918).
Capillary
IC
68
2 DC Description
LOAD POSITION
Internal
Loop
Sample In
S
W 6
Internal
Loop
Sample In
To
Column
To
Waste
INJECT POSITION
To
Column
W 6
To
Waste
From Pump
= Sample
3
2
From Pump
= 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.
69
Sample In
S
W 6
To
Waste
INJECT POSITION
Sample
Loop
Sample In
S
To
Column
W 6
To
Waste
From Pump
From Pump
= Sample
To
Column
= 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.
70
2 DC Description
Other plumbing configurations for the 10-port valve are possible, depending on the components to be connected to the
valve and the application to be run. Refer to the appropriate
Dionex Application Note for more information.
LOAD POSITION
INJECT POSITION
(Loop Loading)
(Concentrator Loading)
Concentrator
Concentrator
To Column
Large
Loop
7
9
10
Sample
In
To Waste
To Waste
Carrier
Pump In
= Sample
Eluent
Pump In
Large
Loop
3
2
To Column
Eluent
Pump In
9
10
Sample
In
To Waste
= Eluent
To Waste
Carrier
Pump In
= Carrier
Liquid flows through either the Load or Inject path, depending on the valve
position. For the example shown in Figure 2-28, the flow occurs as follows:
In the Load position, sample flows from the syringe or autosampler line,
through the valve, and into the sample loop. Excess sample flows out to
waste. Eluent flows from the eluent pump, through the valve, through the
concentrator column, and to the separator column. If sample was
previously loaded onto the concentrator column, it is swept to the
separator column for analysis.
71
2.14
In the Inject position, carrier liquid flows through the sample loop and on
to the concentrator column, carrying the contents of the sample loop with
it. Excess flows out to waste. Eluent flows from the pump, through the
valve, and to the separator column, bypassing the concentrator column.
CD Conductivity Detector
Each Dionex ICS-5000+ Conductivity Detector (CD) consists of a heated
conductivity cell and the electronics required for collecting the conductivity
data and sending it to the computer and the analog output (if installed). The
CD is installed in the upper compartment of the DC (see Figure 2-23).
The CD is available in two versions:
The features and functions of the two CD versions are the same. However,
because the cell volumes of the two are different, the versions are not
interchangeable. The CD version must match the system type (capillary IC or
analytical IC). If the CD version and system type are mismatched,
chromatograms will be affected; for example, there may be broad peaks or
lowered sensitivity.
72
2 DC Description
When the operating temperature is different from the temperature at which the
cell was calibrated, built-in temperature compensation helps minimize
changes in the baseline or in peak heights. The default temperature
compensation is 1.7% per C. This can be reset to between 0% and 3.0% per
C, depending on the eluent. If you notice that the baseline shifts up when the
temperature increases, the compensation factor is too low and should be reset
to a higher value.
To change the temperature compensation factor:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Command window (Chromeleon 7) or the
Commands dialog box (Chromeleon 6.8).
3. Select the conductivity detector.
4. Select the Temperature_Compensation property and enter the value.
5. For Chromeleon 6.8, click Execute.
73
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:
CD Type
Capillary CD
Analytical CD
For details about any of the suppressors, including guidelines for selecting a
suppressor for your application, refer to the suppressor manuals. The manuals
are provided on the Thermo Scientific Reference Library DVD (P/N 053891).
Capillary
IC
Capillary IC Suppressor
Conductivity
Detector
Suppressor
(Optional)
(ASRS 300
model shown)
Suppressor
Cable
74
2 DC Description
NOTE
NOTE
To prevent accumulation of oxygen or hydrogen gases, connect a gas separator waste tube (P/N 045460) to the suppressor waste line during installation For details, refer to Dionex
ICS-5000+ Ion Chromatography System Installation Instructions (Document No. 065447).
The basic flow path is the same for both capillary IC and analytical IC systems. However, in capillary IC systems, connections to components installed inside IC Cube cartridges
(columns, suppressor, and Dionex CRD) are not visible.
75
COND CELL
7
REGEN
OUT
10
CRD
6
8
SUPPRESSOR
5
SEPARATOR COLUMN
GUARD
SAMPLE
= Eluent Flow
= Regenerant
TEMP
STABILIZER
L
Flow
5
W
6
L
2
VALVE
WASTE
For analytical
IC only
PUMP or
ELUENT
GENERATOR
76
After sample is loaded into the sample loop 3 and the injection valve is
toggled to the Inject position, eluent passes through the loop.
From the suppressor, the mixture flows through a Dionex CRD 6 (if
installed) to the cell 7 , where the analytes are detected. A digital signal is
sent to Chromeleon.
Finally, the mixture flows out of the cell and is recycled back into the
suppressor 8 , where it is used as the water source for the regenerant
2 DC Description
chamber. Flow is again routed through the Dionex CRD (if installed)
and then to waste 10 .
1
EGC
COND CELL
11
CRD
CR-TC
14
For anion
suppression only
2
13
WASTE
10
SUPPRESSOR
REGEN IN
EG
12
DEGAS
7
SEPARATOR COLUMN
GUARD
SAMPLE
= Eluent Flow
= Regenerant
VALVE
Flow
6
L
WASTE
5
W
1 TEMP
STABILIZER
5
1
3
2
4P
(Inject Position)
For analytical
IC only
ELUENT IN
Deionized water from the pump 1 enters the EGC, which generates the
eluent. Eluent exits the Dionex EGC and passes through the Dionex CRTC 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.
77
2.15
From the suppressor, the mixture flows through a Dionex CRD 8 (if
installed) to the cell 9 , where the analytes are detected. A digital signal is
sent to Chromeleon.
The mixture flows out of the cell and is recycled back into the
suppressor 10 , where it is used as the water source for the regenerant
chamber. Regenerant flow is routed through the Dionex CRD 11 (if
installed), through the EG degas tubing 12 , through the Dionex CRTC 13 , and then out to waste 14 .
ED Electrochemical Detector
One or two Dionex ICS-5000+ Electrochemical Detectors (EDs) can be
installed in the DC. Each complete ED assembly consists of an amperometric
detection cell and the detector electronics required to collect data and send it
to the computer and the analog output (if installed). The detector is installed in
the upper compartment of the DC (see Figure 2-23). The cell mounts on the
front of the detector. The detector electronics are not accessible to the user.
The ED can perform the following electrochemical detection modes:
78
2 DC Description
Working
Electrode
Cell Body
(counter
electrode)
pH-Ag/AgCl
Reference
Electrode
Titanium Inlet
Tubing (for
analytical IC)
79
substrate is used, the percentage of methanol should not exceed 30% and the
percentage of acetonitrile should not exceed 10%. In addition, prolonged
exposure (more than 8 hours) of disposable gold electrodes on polyester
substrate to eluents containing hydroxide concentrations greater than 100 mM
is not recommended. Shorter rinse periods of 10 to 20 minutes (for example,
the carbonate removal step during monosaccharide and disaccharide
chromatography) at high hydroxide concentrations do not affect the electrode
performance. If sustained highly alkaline eluent conditions are required, use a
disposable gold electrode on a PTFE substrate or a conventional gold
electrode. Refer to Product Manual for Disposable Electrode (Document No.
065040) for additional eluent compatibility information. The manual is
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
Because conventional working electrode blocks are made of Kel-F and use
a gasket made of Ultem, there is no restriction on the concentration of
organic solvents that can be used with them, providing the solvent is
compatible with PEEK tubing.
There is also no restriction on the use of organic solvents when using
disposable gold electrodes on a PTFE substrate and PTFE gaskets.
80
2 DC Description
81
82
2 DC Description
2.16
DC Rear Panel
Figure 2-33 illustrates the rear panel of the DC.
1
8
Switched AC Sockets
USB Receptacle
(B Connector)
9
8
Drain Port
5
6
2
4
7
3
9
The tubing chases route tubing from the front compartment, through the DC
interior, and to the rear panel. Foam inserts insulate the chases.
83
Switched AC Sockets
The two AC receptacles can be used to control the power to external devices.
Use Chromeleon to switch the power on and off. TTL inputs can also be used
to control the AC sockets (see Section 2.17.4).
Fuse Holder, Main Power Switch, and Power Receptacle
The fuse holder contains two 10-amp slow-blow fuses (P/N 954772). For
instructions on how to change the fuses, see Section 9.22.
The rear panel power switch is the main power switch for the DC. Turn on the
main power switch before initial operation and leave the switch on unless
instructed to turn it off (for example, before performing a service procedure).
NOTE
For routine on/off control, use the POWER button on the front
of the DC (see Figure 2-18). To turn off the DC, press and
hold the POWER button for 2 seconds.
The power cord plugs into the IEC 320 three-prong receptacle.
The power supply cord is used as the main disconnect device. Make
sure the socket-outlet is located near the DC and is easily accessible.
USB Connections
84
2 DC Description
If the I/O option (P/N 062201) is installed, the following connections are
provided:
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.
85
2.17
I/O Option
When the I/O option (P/N 062201) is installed, two 12-pin connector strips
are on the DC rear panel. Figure 2-34 describes the functions assigned to each
connector pin.
86
2 DC Description
Position 1
Locking
Screws
Position 12
Figure 2-35.
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. See Figure 2-34 or the label on the DC rear panel for the
connector pin assignments.
To attach a wire to the plug, strip the end of the wire, insert it into the
plug, and use a screwdriver to tighten the locking screw. If necessary,
multiple ground wires can be attached to a single ground pin.
When attaching wires to the connector plug, be careful not to allow
stray strands of wire to short to an adjoining position on the connector.
3. Plug the connector into the appropriate 12-pin connector on the DC rear
panel.
4. Connect the wires from the DC connector plug to the appropriate
connector pins on the other modules. Additional connector plugs are
provided with other Dionex modules.
NOTE
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 Manager or
the Chromeleon 6.8 Server Configuration program (see Section 2.17.4).
87
Values
Description
Full-scale voltage
Range
Conductivity:
0.01 to 15,000 S
DC Amperometry:
50 pA to 300 A
Integrated
Amperometry:
50 pC to 200 C
88
2 DC Description
Analog Output
Setting
Values
Description
Recorder
calibration
Offset level
0 to 100%
Polarity
Positive, Negative
Mark
89
90
A normally open relay is open when the relay is switched off and closed
when the relay is turned on.
A normally closed relay is closed when the relay is off and is open when
the relay is on.
2 DC Description
COM
N.C.
NOTES
Non-Energized Relay
N.O.
COM
N.C.
Energized Relay
91
You can control the power, relays, and TTL outputs from the DC ePanel in
Chromeleon 7 (see Figure 2-38) or the DC Control panel in Chromeleon 6.8.
92
2 DC Description
93
4. Select the name of the input and press the F2 key (or double-click the
name).
94
2 DC Description
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.
TTL Input Control Types
95
controlling device and the information below to determine the correct type.
Select the input control type in the Device Configuration dialog box for each
TTL input (see Figure 2-40).
+0 V
Action On
The action of the positive (rising)
edge depends on the function: For on/off or other functions that have two
options, the rising edge turns off the function. However, for functions with
only one option, the rising edge has no effect.
For example, for the injection valve position, the falling edge switches the
valve to Load and the rising edge switches the valve to Inject. Similarly,
for the detector start/stop, the falling edge starts the detector and the rising
edge stops it. For the detector mark and offset functions, the falling edge
turns on the function and the rising edge has no effect.
Action On
TTL +5 V
INVERTED
EDGE
+0 V
Action Off or No Effect
TTL +5 V
NORMAL
PULSE +0 V
Action On
Action Off
96
Action On
Action Off
TTL +5 V
INVERTED
PULSE +0 V
2 DC Description
2.18
Automation Manager
The Dionex ICS-5000+ Automation Manager (AM) provides a mounting
location for various components used for performing matrix elimination, large
volume pre-concentration, post-column reagent addition, and other functions.
Each AM consists of a tray on which valves and other components are
installed (see Figure 2-41). The tray is installed in the upper compartment of
the DC (see Figure 2-23). Connections to other components in the system
(pump, injection valve, reagent reservoirs, etc.) depend on the application.
See Chapter 3 for the configuration schematic for your application.
Low-Pressure
Valve #1
Low-Pressure
Valve #2
Temperature
Stabilizer
RCH-1
Reaction Coil
High-Pressure High-Pressure
Valve #1
Valve #2
Because the AM requires the full width of the DC upper compartment, an IC Cube cannot be installed in the DC when an
AM is installed.
97
Part Number
075950
075951
075952
AutoPrep configuration:
10-port high-pressure valve
AutoPrep sample loop
AutoPrep standard loops
075953
079833
In addition to the configurations described above, you can order the following
components separately for installation on an AM:
AM Component
Part Number
075917
075918
061971
079848
079849
062561
062562
98
2 DC Description
POSITION B
6
1
6
1
POSITION A
POSITION B
9
10
4
3
8
9
1
2
10
3
1
99
COM
(N.O.)
ON POSITION
COM
(N.O.)
(N.C.)
(N.C.)
N.C. = normally closed
N.O. = normally open
COM = common flow
Note:
When the valve is
off (i.e., it is not
energized), port 0 is
open (N.O.) and port
1 is closed (N.C.).
Conversely, when
the valve is on, port
1 is open and port 0
is closed.
100
2 DC Description
101
102
2 DC Description
103
For direct control of the heater, use the controls on the DC ePanel in
Chromeleon 7 or the Control panel in Chromeleon 6.8.
104
2 DC Description
2.19
105
The applied voltage can be changed up to 10 times during a run. The actual
number of potential changes allowed depends on the available data storage
capacity, which is determined by the length of the run and the data sampling
rate.
For direct control, enter the potentials on the DC ePanel in Chromeleon 7 or
the Control panel in Chromeleon 6.8.
106
2 DC Description
+0.7
Integration
Delay
Potential
(Volts)
+0.1
t1
-0.1
t3
0.0
0.2
E1
0.4
Time (Seconds)
0.6
E2
E3
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.
107
+0.60
+0.35
Potential
(Volts)
-0.10
Integration
-0.60
0.0
0.2
0.4
Time (Seconds)
E1, E2
0.6
0.8
E3
E4
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
analytes 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.
108
2 DC Description
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
NOTE
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.
109
(14.0, 0.60)
0.60
0.40
0.20
Volts
0.00
0.00
-0.20
5.00
10.00
15.00
20.00
25.00
30.00
-0.40
-0.60
-0.80
(0.00, -0.80
(28.0, -0.80)
Seconds
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
2------------------- 1.4 V = 0.1 V
--s
28s
110
2 DC Description
The duration of one waveform period can be between 0.05 and 2.0 s, with
a step resolution of 10 ms. A waveform can have no more than 100 steps.
Multiple waveforms can be defined for a single run, provided they all
have the same cycle duration. Up to 15 waveform changes per run are
allowed.
The integration interval generates one integrated data point per waveform.
111
To view the Waveform Editor, click Edit on the ED Options page in the
Instrument Method Wizard (Chromeleon 7) or Program Wizard (Chromeleon
6.8).
Analytical vs. Scanning Waveforms
112
2 DC Description
1.0
E2
Potential
(Volts)
0.0
E1
-1.0
E1
Integration
E3
-2.5
0.0
0.5
1.0
Time (Seconds)
1.5
2.0
113
time (in minutes) is on the x-axis and the detector response (in
nanoCoulombs) is on the y-axis.
40
Peaks:
1.
2.
3.
4.
5.
6.
3
4
Response
(nC)
L-Fucose
D-Galactosamine
D-Glucosamine
D-Galactose
D-Glucose
D-Mannose
0
0
10
114
2 DC Description
Sample
Injection Data
I-t Plot
(current vs.
waveform
time)
Chromatogram
Plot*
3D Amperometry
Data Plot
Waveform
Plot
Chromatogram plot
Waveform/I-t plot
115
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.
res
po
ns
e(
nA
)
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).
The 3D data shown in Figure 2-58 and Figure 2-59 was collected using an analytical waveform (see Analytical vs.
Scanning Waveforms on page 112).
To switch to the 3D plot view, right-click on the Iso plot, select Decoration,
and click the Iso/3D Plot tab. The 3D view projects the response values in the
third dimension, which allows you to see the height of responses as well as the
colors representing different magnitudes of detection signal along the z-axis
116
2 DC Description
(see Figure 2-59). For this view, imagine you are standing in front and slightly
to the left of the plot.
or
m
ti m
(m
s)
w
av
ef
response (nA)
Based on the peak recognition algorithm or by peaks obtained with a userdrawn baseline, Chromeleon can calculate a baseline I-t plot for each data
point of a peak. Each I-t plot measured at a given retention time can be
corrected by subtracting the calculated baseline I-t plot from the 3D
amperometry data. By definition, if baseline correction is enabled, 3D
amperometry data is zero unless a peak is present.
To enable baseline correction, select Baseline correction on the General tab
page of the 3D Amperometry Decoration dialog box.
117
118
ICS-5000+
TC
2.20
TC Description
TC Front Features
A status bar on the front of the Dionex ICS-5000+ Thermal Compartment
(TC) includes LEDs (light emitting diodes) that indicate the status of several
TC components and functions (see Figure 2-60).
LOAD
CONNECTED
ALARM
INJECT
VALVE 1
LOAD
INJECT
VALVE 2
OVEN
POWER
If the LED Is On
CONNECTED
The TC is connected to a
Chromeleon 7 instrument
or a Chromeleon 6.8
timebase.
ALARM
VALVE 1 LOAD
VALVE 2 LOAD
VALVE 1 INJECT
VALVE 2 INJECT
119
LED Label
If the LED Is On
OVEN
The TC is transitioning to
the set temperature. The
TC is not ready for
operation.
If the LED is flashing and
the ALARM LED is
lighted, an oven error was
detected. See
Section 8.30 for
troubleshooting.
POWER
NOTE
120
2 TC Description
2.21
TC Interior Components
Figure 2-61 illustrates the interior of the TC. The components installed in
your TC may vary, depending on your application.
3
4
5
6
Guard Column
Injection Valves
Column Brackets
Separator Column
Temperature Stabilizer
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).
121
122
2 TC Description
2.22
TC Rear Panel
Figure 2-62 illustrates the rear panel of the TC.
Main Power
2
Switch, Fuse
Holder, and Power
Receptacle
Digital I/O
Connectors (2)
USB Receptacle 4
(B Connector)
Drain Port
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.
123
The two 6-pin mini-DIN connectors can be used to exchange digital signals
with any external device capable of being controlled through a relay or TTL
input. The two connectors are identical in function.
Relay_Com
Relay_N.O.*
Digital Input
Digital_GND
Not Used
Not Used
When the relay is activated, the connection is between Com and N.O.
124
Connection
Description
0 to +5 V
2 TC Description
Use the 6-pin mini-DIN signal cable (P/N 6000.1004) provided in the TC
Ship Kit (P/N 064789) to connect the TC to an external device. For details
about the pin assignments, see Table 2-8.
Pin
Signal Name
Signal Level
Core
Color
Core Label
Not occupied
----
Pink
Analog High
Not occupied
----
Gray
Analog Low
Digital_GND
0V
Green
Digital GND
Digital Input
0 to +5 V
Yellow
Digital Input
Relay_N.O.
Brown
Digital Output
Relay_Com
White
Dig./Out (GND)
Black
Shield
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.
125
2.23
Injection Valves
The TC is available in the following configurations:
TC Description
Part Number
075960
075961
075962
075963
INJECT POSITION
Sample In
To Waste
W (6)
W (6)
From Pump
Sample In
S (5)
S (5)
L (4)
L (4)
To Column
= Sample
From Pump
To Column
= Eluent
126
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
2 TC Description
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.
10_1 POSITION
(Loop Loading)
1_2 POSITION
(Concentrator Loading)
Concentrator
Concentrator
6
7
Large
Loop
Sample In
5
3
9
10
To Column
Eluent
Pump In
6
7
To Waste
Large
Loop
Carrier Pump In
To Waste
10
Sample In
5
3
To Column
Eluent
Pump In
To Waste
Carrier Pump In
To Waste
= 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.
127
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.
TO INJECT
VALVE -W
W (6)
S (5)
25 L SAMPLE LOOP
(Orange)
TO INJECT
VALVE -P
L (4)
TO INJ
VALVE -C
(Red - microbore)
(Black - standard bore)
128
2 TC Description
2.24
Secondary column properties are entered by the user and can be changed
whenever required by any Chromeleon user with Expert privileges.
Secondary properties include the column manufacturer, diameter, length,
particle size, maximum number of injections, pH limits, and upper
pressure limit. For a complete list of secondary properties, refer to the
Chromeleon Help.
129
2.25
The ALARM LED on the front of the TC lights (red), and remains red as
long as the sensor is exposed to gases or humidity.
A beep sounds.
Follow the steps below 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 Command window (Chromeleon 7) or the
Commands dialog box (Chromeleon 6.8).
3. Select the TC.
4. If you are using Chromeleon 7: Click the Parameters tab page for the TC
and click the GasLeakSensor or HumidityLeakSensor parameter.
Select the new sensitivity setting (or select Off to disable the sensor).
If you are using Chromeleon 6.8: Click the plus sign beside TC to display
130
2 TC Description
2.26
TC Theory of Operation
The fundamental requirement for a thermal compartment intended for
chromatography applications is the ability to maintain the preset temperature
as precisely as possible. The TC contains advanced electronic circuitry that
maintains the selected temperature with a precision of 0.1 C.
The TC can be heated from 5 to 85 C in 0.1 C increments. An increase in
temperature from 20 to 50 C (or a decrease from 50 to 20 C) is typically
realized in less than 20 minutes. Columns can be warmed up to 85 C. If the
ambient temperature changes during the analysis, increased heating or cooling
ensures that the column temperature remains constant.
Operating IC columns at temperatures above 70 C (158 F) may affect
column performance. Before selecting the TC temperature, refer to the
column manual for the recommended operating conditions. Column
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
The stationary phase temperature remains constant over the total column
length.
The column and the eluent have the same temperature during the analysis.
131
The temperature achieved may vary from the control range, depending on the
ambient temperature (see the table below).
Control Range
5 to 85 C
For example, if the ambient air temperature in the lab is 30 C and you set the
temperature to 5 C, the actual temperature achieved will be about 12 C.
Do not touch any metal parts inside the TC while it is heating up or after
it reaches the set point temperature. Wait for the compartment to cool
down before servicing any parts.
Ne touchez aucune des pices mtalliques l'intrieur du TC pendant
qu'il chauffe ou aprs qu'il ait atteint la temprature de consigne.
Attendez que le compartiment soit refroidi avant de rparer les pices.
Berhren Sie im TC keine metallischen Teile, whrend dieses
aufgeheizt wird oder nachdem die Solltemperatur erreicht ist. Warten
Sie, bis die Kammer abgekhlt ist, ehe Sie Wartungsarbeiten
durchfhren.
132
2 TC Description
133
134
3 Configurations
3.1
Overview
This chapter provides example component and plumbing drawings for the
following Dionex ICS-5000+ system configurations:
Dionex ICS-5000+ IC System Configuration
See
page 136
page 137
page 138
page 139
page 140
page 141
page 142
page 143
page 144
page 145
page 146
135
Seal
Wash
Pump
System #2
To waste
Piston
Seal
Wash
System #1
Deionized
Water
Deionized
Water
To waste
To EGC
#1 In
DC (front view)
ELUENT IN
ELUENT IN
ELUENT IN
ELUENT OUT
CES 300
ELUENT OUT
REGEN IN
EG
DEGAS
ELUENT IN
SUPPRESSOR
BYPASS
EG
DEGAS
EG
(right side view)
System #2
EGC
(capillary)
REGEN IN
SAMPLE IN
CELL IN
System #1
ELUENT OUT
CRD
BYPASS
SAMPLE IN
ELUENT IN
SAMPLE OUT
CELL OUT
Conductivity Detector
(Capillary)
SAMPLE OUT
ELUENT IN
EGC
(capillary)
L
EC CEL
OUT
IN
System #1
System #2
From
autosampler
To waste
EG
(left side view)
ELUENT OUT
ELUENT IN
CRD 200
REGEN OUT
ELUENT OUT
ELUENT OUT
ELUENT OUT
From
autosampler
ELUENT IN
REGEN OUT
ELUENT OUT
To waste
From IC Cube #1
EG Degas
Regen Out
Regen Out
Regen Out
Regen In
To IC Cube #1
EG Degas
Eluent In
Regen In
Eluent In
Eluent In
Eluent Out
Eluent Out
To waste
To waste
3 Configurations
Seal
Wash
Pump
System #2
To waste
Piston
Seal
Wash
System #1
Deionized
Water
Deionized
Water
To waste
To EGC
#1 In
DC (front view)
ELUENT IN
ELUENT IN
ELUENT IN
ELUENT OUT
CES 300
ELUENT OUT
REGEN IN
EG
(left side view)
EG
DEGAS
ELUENT IN
SUPPRESSOR
BYPASS
EG
DEGAS
EGC
(capillary)
REGEN IN
SAMPLE IN
CELL IN
ELUENT IN
CELL OUT
Conductivity Detector
(Capillary)
SAMPLE OUT
ELUENT IN
EGC
(capillary)
EC CELL
OUT
IN
System #1
System #2
From
autosampler
To waste
EG
(right side view)
System #2
ELUENT OUT
CRD
BYPASS
SAMPLE IN
SAMPLE OUT
System #1
ELUENT OUT
ELUENT IN
CRD 200
REGEN OUT
ELUENT OUT
ELUENT OUT
ELUENT OUT
From
autosampler
ELUENT IN
REGEN OUT
ELUENT OUT
To waste
From IC Cube #1
EG Degas
Regen Out
Regen Out
Regen Out
Regen In
To IC Cube #1
EG Degas
Eluent In
Regen In
Eluent In
Eluent In
Eluent Out
Eluent Out
To waste
To waste
137
Seal
Wash
Pump
System #2
To EGC
#2 In
To waste
A
Piston
Seal
Wash
System #1
Deionized
Water
Deionized
Water
Mixer
To EGC #1 In
B
C
D
To waste
DC (front view)
ELUENT IN
ELUENT IN
REGEN OUT
ELUENT OUT
ELUENT IN
CES 300
REGEN IN
EG
DEGAS
ELUENT IN
SAMPLE OUT
Cell In
Cell Out
CELL IN
Eluent Out
CELL OUT
EGC
(capillary)
EGC
(standardpressure)
SAMPLE IN
Regen Out
EG
(right side view)
System #2
ELUENT OUT
ELUENT IN
CRD 200
ELUENT OUT
System #1
ELUENT OUT
ELUENT OUT
From autosampler
To waste
EG
(left side view)
Conductivity Detector
(Capillary)
System #2
Vent
Eluent
Out
In
Out
System #1
Separator
(5) S
Temp .
Stabilizer W
(6)
From autosampler
(1) L
(3)
Regen
Out
Eluent
In
Regen Out
Eluent
Out
Regen In
Regen In
CR-TC
Guard
L (4)
P (2)
Eluent
In
To
Waste
REGEN IN
Regen In
ELUENT OUT
Eluent In
Backpressure
Device
Eluent In
Eluent
Out
To waste
To waste
To waste
Figure 3-3. Hybrid System: Dual RFIC-EG System (CD Analytical/CD Capillary)
138
3 Configurations
Eluent
DC (front view)
Seal
Wash
Pump
Cell In
Regen Out
Cell Out
Eluent Out
Eluent In
Regen In
Piston
Seal
Wash
Pump inlet
Separator
(5) S
Temp .
Stabilizer W
(6)
From AS-AP
(1) L
L (4)
Guard
(3)
Mixer
On/Off Valve
P (2)
To waste
To AS-AP/Waste
139
Seal
Wash
Pump
Pump inlet
Piston
Seal
Wash
Deionized
Water
On/Off
Valve
Mixer
To waste
DC (front view)
EG
(left side view)
EGC
(high-pressure)
Vent
Eluent
Out
Regen In
Out
In
Separator
Eluent
In
To
Waste
Regen
Out
Eluent
In
REGEN IN
Eluent In
Cell Out
Eluent Out
ELUENT OUT
Cell In
Regen Out
Eluent
Out
Regen In
(5) S
Temp .
Stabilizer W
(6)
From AS-AP
To AS-AP/Waste
(1) L
(3)
P (2)
CR-TC
Guard
L (4)
Backpressure
Device
To Waste
3 Configurations
Seal
Wash
Pump
B
C
D
System #2
Mixer
To waste
Piston
Seal
Wash
System #1
Deionized
Water
Deionized
Water
Mixer
B
C
D
To waste
EG
(left side view)
System #1
Regen In
Eluent In
Cell Out
Vent
Eluent Out
(6)
From AS-AP
To AS-AP/Waste
Guard #1
L (4)
(5) S
(3)
W
From AS-AP
(6)
L (4)
Temp.
Stabilizer
C
(3)
P (2)
To AS-AP/Waste (1)
L
P (2)
Backpressure Device
System #1
System #2
(1) L
Out
Eluent
In
Eluent
Out
Eluent
Out
Out
CR-TC
Eluent
To
In
Waste
Regen
Out
In
Regen In
Backpressure Device
Temp.
Stabilizer
(5) S
In
To AS-AP/Waste
Guard #2
Eluent
In
To
Regen Waste
Regen In
Out
Separator #2
Separator #1
Vent
Eluent
Out
Eluent
In
REGEN IN
Eluent In
Cell In
Regen Out
REGEN IN
Cell Out
Eluent Out
ELUENT OUT
Cell In
EGC
(high-pressure)
Eluent
Out
To inject valve
#2 port P (2)
EGC
(high-pressure)
Regen Out
EG
(right side view)
System #2
ELUENT OUT
DC (front view)
Regen In
CR-TC
To waste
To waste
141
A
Seal
Wash
Pump
B
C
D
System #2
Mixer
Mixing
Chamber
To waste
System #1
Deionized
Water
Eluent
Piston
Seal
Wash
Mixing
Mixer
Chamber
B
C
D
To waste
From pump #2
DC (front view)
EG
(left side view)
System #1
Cell Out
Vent
In
Guard #2
(5) S
Temp .
Stabilizer
From AS-AP
To AS-AP/Waste
(6)
(1) L
Guard #1
L (4)
(5) S
(3)
P (2)
W
From AS-AP
To AS-AP/Waste
(6)
(1) L
L (4)
C
(3)
P (2)
Temp .
Stabilizer
Backpressure Device
Separator #2
Separator #1
To inject
valve #1
port P (2)
Out
To the CR-TC #1
Regen
Out
Eluent
In
Regen In
CR-TC
Eluent
Out
In
Eluent
Out
Out
Eluent
In
To
Waste
To inject valve
#2 port P (2)
Regen
Out
Eluent
In
REGEN IN
To the degasser #2
To
Waste
REGEN IN
Regen In
Vent
Eluent
In
Regen In
CR-TC
ELUENT OUT
Eluent
Out
ELUENT OUT
Eluent Out
Eluent In
Cell In
EGC
(standardpressure)
EGC
(standardpressure)
Regen Out
EG
(right side view)
System #2
Eluent
Out
To waste
Backpressure Device
System #1
System #2
To waste
3 Configurations
Pump inlet
Seal
Wash
Pump
Pump #2
On/Off
Valve
Mixer
To waste
Piston
Seal
Wash
Deionized
Water
(carrier)
B
C
D
Pump #1
Deionized
Water
Mixer
To waste
DC (front view)
From AS-AP
EG
(left side view)
To AS-AP/Waste
From AS-AP
Large Loop
EGC
(standardpressure)
Regen In
In
Out
Separator
(5) S
Temp .
Stabilizer W
(6)
(1) L
L (4)
Regen
Out
Eluent
In
Regen In
CR-TC
Guard
Eluent
In
To
Waste
REGEN IN
Eluent In
Cell Out
Eluent Out
ELUENT OUT
Cell In
Regen Out
Eluent
Out
(3)
P (2)
Backpressure
Device
To Waste
Figure 3-8. Analytical IC: Single RFIC-EG System with Matrix Elimination Using a DP and a 6-Port Valve
Doc. 065446-01 11/12
143
Injection Valve
Connections Key
To column
Pump inlet
Seal
Wash
Pump
Concentrator
Pump #2
Eluent in
On/Off
Valve
Mixer
8
10
7 5
9
1 3
To waste
To waste
Piston
Seal
Wash
2
Carrier pump in
To waste
Deionized
Water
(carrier)
B
C
D
Pump #1
Deionized
Water
Mixer
To waste
DC (front view)
EG
(left side view)
EGC
(standardpressure)
Cell In
Regen Out
Cell Out
Vent
Eluent Out
In
Out
Separator
6
From AS-AP
9
10
Eluent
Out
Concentrator
3
1
Regen
Out
Eluent
In
Regen In
CR-TC
Guard
7 5
8
Eluent
In
To
Waste
Regen In
REGEN IN
Eluent In
Eluent
Out
ELUENT OUT
Sample in
Backpressure Device
Large Loop
To AS-AP/Waste
To Waste
Figure 3-9. Analytical IC: Single RFIC-EG System with Matrix Elimination Using an SP and a 10-Port Valve
144
3 Configurations
Pump inlet
Seal
Wash
Pump
Pump #2
On/Off
Valve
Mixer
To waste
Deionized
Water
(Regen)
Deionized
Water
Reagent
To the
absorbance
or PDA
detector
Piston
Seal
Wash
To waste
DC (front view)
EG
(left side view)
plug
M N.O.
CO
N.C.
Pump #1
Mixer
Reagent in
from pump #2
B
C
M
CO N.O.
N.C.
RCH-1
To waste
Vent
Eluent
Out
Regen In
In
Out
Separator
(5) S
Temp.
Stabilizer W
(6)
From AS-AP
To AS-AP/Waste
(1) L
L (4)
Eluent
In
To
Waste
Regen
Out
Eluent
In
REGEN IN
Eluent In
Cell Out
Eluent Out
Regen In
CR-TC
ELUENT OUT
Cell In
Regen Out
EGC
(standardpressure)
Eluent
Out
Guard
(3)
P (2)
Backpressure
Device
To Waste
Figure 3-10. Analytical IC: Single RFIC-EG System with Post-Column Reagent Addition (Bromate)
Doc. 065446-01 11/12
145
Seal
Wash
Pump
Piston
Seal
Wash
Deionized
Water
VP
Ballast
Bottle
To the
VP
DC (front view)
Mixer
B
C
D
To waste
EG
(left side view)
EGC
(standardpressure)
Vent
Eluent
Out
Out
CarboPac PA20
(5) S
Temp.
Stabilizer W
(6)
From AS-AP
To AS-AP/Waste
(1) L
(3)
P (2)
Eluent
In
Eluent
Out
Regen In
CR-TC
L (4)
C
Regen
Out
Eluent
In
REGEN IN
In
To
Waste
ELUENT OUT
VP
Vacuum
Pump
Figure 3-11. Analytical IC: Single RFIC-EG System with ED and VP (for Carbohydrate Analysis)
146
4 Startup
This section is an overview of the steps required to start up the Dionex ICS5000+ system components and prepare the system to run samples. The
operating parameters (flow rate, compartment temperature, suppressor
current, etc.) depend on the application you plan to run. Refer to the column
manual, as well as the schematics in Chapter 3 of this manual, for the required
operating parameters.
NOTE
4.1
Operating Precautions
4.1.1
EG Operating Precautions
In an analytical IC system, the Dionex EGC requires at least 14 MPa (2000
psi) of system backpressure. This ensures optimal removal of electrolysis gas
from the eluent produced by the cartridge.
During system equilibration, monitor the Current Pressure reading on the
Pump panel in Chromeleon. The pressure should remain between 14 and
35 MPa (2000 and 5000 psi) if a Dionex EGC 500 is installed or between 14
and 21 MPa (2000 and 3000 psi) if a Dionex EGC 300 is installed. If
necessary, increase the system backpressure by installing a backpressure coil
between the injection valve and the ELUENT OUT port on the Dionex EGC.
For instructions, see Section 9.17.
The recommended maximum operating pressure for the EG in an
analytical IC system is 35 MPa (5000 psi) if a Dionex EGC 500 is
installed or 21 MPa (3000 psi) if a Dionex EGC 300 is installed.
Excessive backpressure may rupture the tubing inside the Dionex
RFIC+ Eluent Degasser.
147
If you select a low flow rate that allows the system pressure to drop below
14 MPa (2000 psi) and you do not turn off the EG, the EG will continue to
generate eluent at the concentration set for the last step of the last Chromeleon
7 instrument method or Chromeleon 6.8 program.
If this occurs, the eluent concentration will increase in proportion to the
decrease in the flow rate. In extreme cases, excessive heat buildup can occur
and damage the Dionex EGC.
For a complete list of operating precautions for Dionex EGCs and CR-TC trap
columns, refer to the product manuals. The manuals are provided on the
Thermo Scientific Reference Library DVD (P/N 053891).
148
4 Startup
4.1.2
Prepare all eluents with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
Be careful to keep the polished surface of the ED cell body clean and dry
when not in use. The gold, spring-loaded (pogo) contact must also remain
clean and dry. If a salt bridge forms, it can cause an electrical short
between the working electrode contact and the cell body.
Over the lifetime of the conventional working electrode, the surface may
gradually become pitted or receded. Receded electrodes can be repaired
by sanding with 600 grit sandpaper. Continue sanding until the metal
surface is again flush with the Kel-F electrode block surface. Then, polish
the electrode (see Section 9.28.4).
149
150
4 Startup
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. If the
limits are exceeded, the audit trail displays an alarm.
To disable the alarm, set the upper limit to 14 and the lower
limit to 0.
151
4.2
4.3
You can use the Smart Startup feature in Chromeleon to automate system startup and equilibration. Refer to the Chromeleon Help for details.
Preparing Samples
This section provides basic information about collecting, storing, and
preparing samples for analysis.
NOTE
4.3.1
152
4 Startup
these can leave traces of ions on the container walls. The ions may interfere
with the analysis.
If samples will not be analyzed on the day they are collected, filter them
through clean 0.45 micron filters immediately after collection; otherwise,
bacteria in the samples may cause the ionic concentrations to change over
time. Refrigerating the samples at 4C (39 F) will reduce, but not eliminate,
bacterial growth.
Analyze samples containing nitrite or sulfite as soon as possible. Nitrite
oxidizes to nitrate, and sulfite to sulfate, thus increasing the measured
concentrations of these ions in the sample. In general, samples that do not
contain nitrite or sulfite can be refrigerated for at least one week with no
significant change in anion concentration.
4.3.2
Pretreating Samples
Analyze rainwater, drinking water, and air particulate leach solutions directly
with no sample preparation (other than filtering and if required, diluting).
Filter groundwater and wastewater samples through 0.45 micron filters before
injection, unless samples were filtered after collection.
A Dionex Low-Volume High-Pressure Inline Filter (P/N 074505) is available
for removing particulates down to 0.45 micron from samples. Connect the
inline filter between the autosampler outlet and the sample inlet port on the
injection valve. For details, see the instructions provided with the inline filter.
Before injection, pretreat samples that may contain high concentrations of
interfering substances by putting them through Thermo Scientific Dionex
OnGuard cartridges. Refer to the installation and troubleshooting guide for
the OnGuard cartridge for instructions. The guide is provided on the Thermo
Scientific Reference Library DVD (P/N 053891).
4.3.3
Diluting Samples
Because the concentrations of ionic species in different samples can vary
widely from sample to sample, no single dilution factor can be recommended
for all samples of one type. In some cases (for example, many water samples),
concentrations are so low that dilution is not necessary.
To dilute the sample, use eluent or ASTM Type I (18 megohm-cm) filtered
and deionized water that meets the specifications listed in Section 1.5. When
153
using carbonate eluents, diluting with eluent minimizes the effect of the water
dip at the beginning of the chromatogram. If you dilute the sample with
eluent, also use eluent from the same lot to prepare the calibration standards.
This is most important for fluoride and chloride, which elute near the water
dip.
To improve the accuracy of early eluting peak determinations, such as
fluoride, at concentrations below 50 ppb, dilute samples in eluent or spike the
samples with concentrated eluent to minimize the water dip. For example,
spike a 100 mL sample with 1.0 mL of a 100 X eluent concentrate.
4.3.4
Fill the vials to the vial shoulder or lower. Do not fill to the top.
During sampling, make sure the needle vent is not immersed in liquid.
For 10 mL vials only: If necessary, raise the needle height inside the vial
to position the vent above the liquid. Set the needle height in a
Chromeleon 7 instrument method or a Chromeleon 6.8 program.
Install a cap on each vial. Make sure the septum is pushed fully into the
cap and the cap is securely tightened.
154
Put on powder-free latex gloves before handling well plates and covers to
minimize sample contamination.
Rinse well plates and covers thoroughly with deionized water before use
to remove any contaminants.
4 Startup
4.4
Fill the vials until the level in the vial reaches the top of the vial tray.
Install a cap on each vial. Use the cap insertion tool (P/N 037987) to
prevent contamination and ensure the cap is inserted to the proper depth.
Starting Chromeleon 7
NOTE
4.4.1
4.4.2
155
156
4 Startup
4.5
4.5.1
4.5.2
157
number of device functions can be controlled directly from this panel and
the audit trail can be accessed from here.
158
ICS-5000+
DP/SP
4.6
DP/SP Startup
Setting Up the Eluent Reservoirs
1. Rinse the eluent reservoirs with ASTM Type I (18 megohm-cm) filtered
and deionized water.
NOTE
Part Number
072112
062463
072111
063342
Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water to remove any loose
particles.
5. Install an end-line filter on the end of each reservoirs 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.
159
NOTE
4.7
The standard piston seal wash system is designed for use with only one of the
two pumps in a DP module. When the DP is shipped from the factory, the seal
wash system is connected to pump 1 (the bottom pump). If you want to
connect the seal wash system to pump 2 (the top pump), follow the
instructions in this section.
NOTE
160
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).
4 DP/SP Startup
1. Note the tubing connected from the peristaltic pump to the seal wash tube
on the secondary pump head on pump 1 (see Figure 4-5, item 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
secondary pump
head
Connection between
pump heads
3
2
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.
161
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
162
4 DP/SP Startup
d. For Chromeleon 7, click the Properties tab in the right pane of the
window. For Chromeleon 6.8, scroll through the list of commands
and properties under the pump name.
e. Select the RearSealWashSystem property and select the Interval
option.
f.
4.8
3. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the Pump tab to display the Pump panel (see Figure 4-7).
Enter a new
flow rate or
click the
switch to start
the pump at
the selected
flow rate.
Figure 4-7. Setting the Pump Flow Rate and Pressure Limits
(Chromeleon 7 Version Shown)
163
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
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.
If your system includes a capillary pump linked to a Dionex EGC using
the standard EG degas (capillary) cartridge (P/N AAA-074459), the high
pressure limit must be changed to 21 MPa (3000 psi).
Pump Configuration
Default Low
Pressure Limit
Default High
Pressure Limit
164
ICS-5000+
EG
4.9
EG Startup
Entering the Eluent Concentration
1. Press the POWER button on the front of the EG.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the Eluent Generator tab to display the Eluent Generator panel (see
Figure 4-8).
165
5. If the CR-TC switch is off, click the switch to turn on the power to the
Dionex CR-TC.
4.10
KOH (Capillary)
MSA (Capillary)
K2CO3
KOH
LiOH
166
4 EG Startup
Dionex EGC
MSA
NaOH
Comment
K2CO3/EPM
Electrolytic pH
Modifier
KOH/KOH
KOH/MSA
KOH/NaOH
MSA/MSA
MSA/NaOH
NaOH/NaOH
The eluent
concentration range
for each cartridge is
50% of the range for
an independent
cartridge.
167
Dionex EGCs
Comment
LiOH/LiOH
The eluent
concentration range
for each cartridge is
50% of the range for a
single-independent
cartridge.
KOH (Capillary)/
MSA (Capillary)
The eluent
concentration range
for each cartridge is
50% of the range for
an independent
cartridge.
168
ICS-5000+
DC
4.11
DC Startup
Starting the DC
1. Press the POWER button on the front of the DC.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the DC tab to display the DC panel (see Figure 4-9).
169
4.12
Pump
EGC
CR-TC
EPM
Suppressor
170
4 DC Startup
3. View the detector signal and monitor the background. Refer to the column
manual for the appropriate background for your application. The column
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
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. If the reading is too high, see Section 8.11 for
troubleshooting information. If the baseline is drifting or is excessively
noisy (there are large fluctuations in readings), see Section 8.2 for
troubleshooting information.
6. Monitor the DP/SP pressure to make sure it is at the expected reading for
the installed column and 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
IC
Because capillary IC systems use low flow rates and consume very little
eluent, you can leave a capillary IC system on at all times, allowing it to
remain equilibrated and always ready to run the next sample.
171
172
ICS-5000+
TC
4.13
TC Startup
Starting the TC
1. Press the POWER button on the front of the TC.
2. On the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset, click
the TC tab to display the TC panel (see Figure 4-10).
173
4.14
174
5 Operation
5.1
toolbar button.
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 Command window (Chromeleon 7) or the
Commands dialog box (Chromeleon 6.8). You can access all commands
available for the system from here.
175
5.2
Analyzing Samples
Figure 5-1 shows the basic steps used to
analyze a sample in a chromatography
system.
To analyze a sample with a Dionex ICS5000+ system, you add sample injections to
a Chromeleon sequence. The sequence
determines how the group of injections will
be analyzed and the order in which they will
be run. A sequence typically includes the
following elements:
Autozero
Start data
acquisition
Stop data
acquisition
Evaluate
sample data
176
5 Operation
5.2.1
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
.
177
4. After you finish the eWorkflow Wizard, the sequence is displayed in the
Console Data view (see Figure 5-3).
3. After you finish the wizard, the new sequence is displayed in the Console
Data view (see Figure 5-3).
5.2.2
178
If the program and quantification method have already been created, use
the Sequence Wizard.
5 Operation
1. On the Sequence Control panel in the Chromeleon 6.8 panel tabset, click
Create Sequence (see Figure 5-4).
3. After you finish the Sequence Wizard, the new sequence is displayed in
the Chromeleon 6.8 Browser.
179
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.
5.2.3
Starting a Sequence
Starting a Sequence in Chromeleon 7
180
5 Operation
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).
181
5.3
5.3.1
Loading samples with a syringe through the sample loading ports on the
DC front door (see Section 5.3.2)
5.3.2
182
Loading sample with a syringe through the sample loading port on the
front of the DC (push method)
Loading sample with a vacuum syringe through the sample loading port
on the front of the DC (pull method)
5 Operation
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, see 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.
5.3.3
183
g
Syrin
(5) S
(6)
(1) L
L (4)
Sample Port
Guard
(3)
P (2)
Valve
Sample
5.4
184
5 Operation
Figure 5-9 shows the basic Chromeleon commands for controlling sample
injection with a Dionex AS-AP.
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.
Figure 5-10. Commands for Loading and Injecting Sample with a Dionex
AS-DV (Chromeleon 7 Script Editor Shown)
185
186
6 Shutdown
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
Disconnect the tubing from the peristaltic pump on the component panel:
press the lever to the right, remove the tubing, and release the lever (see
Figure 6-1).
187
188
ICS-5000+
EG
6.1
EG Shutdown
Short-term Shutdown
If the shutdown is for 3 months or less, follow the instructions below.
To prepare the EG for the shutdown:
1. Turn off the EG, including all consumables installed in the EG (the
Dionex CR-TC, suppressor, etc.).
2. Verify that the current to the Dionex EGC and the suppressor is off.
ICS-5000
EG
Supplying power to the Dionex EGC when there is no eluent flow can
severely damage the cartridge.
6.2
Long-term Shutdown
If the shutdown is for 3 months or more, follow the instructions below.
To prepare the EG for the shutdown:
1. Turn off the EG, including all consumables installed in the EG (the
Dionex CR-TC, suppressor, etc.).
189
2. Verify that the current to the Dionex EGC and the suppressor is off.
Supplying power to the Dionex EGC when there is no eluent flow can
severely damage the cartridge.
3. If you plan to store the Dionex EGC in the EG, no further action is
required.
If you plan to store the cartridge outside the EG (for example, in the
original shipping container), follow the instructions in Section 9.14.1 to
remove the Dionex EGC from the EG, and the instructions in
Section 9.14.3 to store the Dionex EGC.
To restart the EG:
1. 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 Dionex EGC. For instructions, see Conditioning the
Capillary EGC on page 346 or Conditioning the Analytical EGC on
page 352.
3. Hydrate the Dionex CR-TC (see Installing and Flushing the New CRTC on page 355).
4. Hydrate the suppressor as instructed in the product manual. Suppressor
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
5. Let the system equilibrate before collecting data.
Before shipping the EG:
1. Follow the instructions in Section 9.14.1 to remove the Dionex EGC from
the EG.
2. Plug all fittings. Tighten the vent fitting (capillary Dionex EGC or highpressure analytical Dionex EGC) or cap the vent port (standard-pressure
analytical Dionex EGC). This will prevent the evaporation of water in the
electrolyte reservoir.
Make sure the Dionex EGC packaging conforms to hazardous material
shipping requirements. Refer to the Material Safety Data Sheet (MSDS)
shipped with the Dionex EGC for the chemical description.
190
ICS-5000+
DC
6.3
DC Shutdown
Consumables Storage
The columns, suppressors, and other consumable items used with a Dionex
ICS-5000+ system have various short- and long-term storage requirements.
Refer to the manuals for the individual products for instructions. These
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
6.4
ED Cell Storage
6.4.1
6.4.2
191
5. Make sure there is no air bubble in the cap. Add more KCl solution if
needed.
Storage
Cap
192
ICS-5000+
TC
6.5
TC Shutdown
Consumables Storage
The columns and other consumable items used with a Dionex ICS-5000+
system have various short- and long-term storage requirements. Refer to the
manuals for the individual products for instructions. These manuals are
provided on the Thermo Scientific Reference Library DVD (P/N 053891).
6.6
Short-term Shutdown
Before a TC shutdown of less than one week, no special procedure is
required.
6.7
Long-term Shutdown
Before interrupting TC operation for more than one week, or before shipping
the TC, rinse the fluid connections with deionized water.
193
194
7 Maintenance
This section describes routine maintenance procedures for the Dionex ICS5000+ system that users may perform. All other maintenance procedures must
be performed by a Technical Support Representative for Dionex products.
For information about maintenance procedures for the Dionex EGC, CR-TC
trap column, or suppressor, refer to the appropriate product manual. These
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
7.1
7.1.1
Daily Maintenance
Check for leaks.
Wipe up liquid spills.
Check eluent reservoirs for microbial growth; clean reservoirs and replace
eluent as needed.
7.1.2
DP/SP
page 199
EG
page 201
DC
page 203
TC
page 205
Weekly Maintenance
Check end-line filters on eluent lines. When end-line filters are new, they
are pure white. Replace filters if they become discolored, if bacterial
195
7.1.3
page 199
EG
page 201
DC
page 203
TC
page 205
Periodic Maintenance
Clean eluent reservoirs (when making fresh eluent or as needed) (see
Section 9.4).
page 200
DC
page 203
TC
page 205
NOTE
7.1.4
Annual Maintenance
Thermo Fisher Scientific recommends performing preventive
maintenance on each module annually. Preventive Maintenance Kits
contain all the required parts for these procedures.
196
7 Maintenance
NOTE
197
198
ICS-5000+
DP/SP
7.2
7.3
Check for leaks at the following locations: the eluent proportioning valves
(gradient pump only), vacuum degas chambers, and eluent reservoirs.
Tighten or replace any leaking fittings.
Wipe up liquid spills and rinse dried reagents off pump components with
deionized water. Dry the leak sensor thoroughly; if the sensor is not dry, it
will remain activated and continue to report a leak to the audit trail.
Check the liquid level in the seal wash reservoir. The liquid level should
remain between the Min. and Max. markers on the reservoir label.
Check eluent reservoirs for microbial growth; clean reservoirs and replace
eluent as needed. Rinse each eluent reservoir thoroughly (inside and out)
with ASTM filtered, Type I (18 megohm-cm) deionized water that meets
the specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, clean the reservoir as instructed in Section 9.4.
Check the liquid level in each eluent reservoir and refill as required.
The end-line filters (P/N 045987) on the eluent lines may need to be
replaced weekly, depending on water quality and eluent conditions. For
example, replace the filters weekly when using a Dionex EGC to generate
carbonate/bicarbonate eluent.
When the end-line filters are new, they are pure white. Replace the filters
whenever they become discolored, if bacterial buildup is evident, or if
eluent flow is blocked.
199
NOTE
Part Number
072112
062463
072111
063342
Before installation, thoroughly rinse the end-line filter with ASTM Type I
(18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5 to remove any loose particles.
Capillary
IC
7.4
Capillary
IC
7.5
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 liquid level in each eluent reservoir and refill as required.
200
ICS-5000+
EG
EG Routine Maintenance
This section describes routine maintenance procedures for the Dionex ICS5000+ Eluent Generator (EG) that users may perform. All other maintenance
procedures must be performed by a Technical Support Representative for
Dionex products.
For information about maintenance procedures for the Dionex EGC, trap
column, or suppressor, refer to the appropriate product manual. These
manuals are provided on the Thermo Scientific Reference Library DVD
(P/N 053891).
7.6
7.7
EG Daily Maintenance
Locate and repair leaks inside the EG (see Section 9.13) and wipe up
liquid. Rinse dried eluents off components with deionized water.
Rinse the EG drip tray with deionized water (to prevent formation of salt
crystals) and dry the drip tray thoroughly. Rinse and dry the leak sensor,
also; if the sensor is not dry, it will remain activated and continue to report
a leak to the audit trail.
EG Weekly Maintenance
Check all lines for crimping. Move (or reroute) pinched lines and replace
damaged lines (see Section 9.12). For help in isolating the cause of a
tubing restriction, see Section 9.13.
201
7.8
EG Annual Maintenance
202
Check the expiration date and remaining lifetime of the Dionex EGC on
the Eluent Generator ePanel in Chromeleon 7 or the Control panel in
Chromeleon 6.8.
ICS-5000+
DC
DC Routine Maintenance
This section describes routine maintenance procedures for the Dionex ICS5000+ Detector/Chromatography Module (DC) that users may perform. All
other maintenance procedures must be performed by a Technical Support
Representative for Dionex products.
7.9
DC Daily Maintenance
Check the DC components for leaks or spills. Wipe up spills. Isolate and
repair leaks (see Section 8.26). Rinse off any dried eluent with ASTM
filtered, Type I (18 megohm-cm) deionized water that meets the
specifications listed in Section 1.5.
NOTE
7.10
7.11
If you are using an electrochemical detector, also see the special maintenance considerations that are described in
Section 4.1.2.
DC Weekly Maintenance
Check for excess condensation inside the DC. Condensation may build up
when the DC is operated in a highly humid environment and the majority
of the applications are run at cold temperatures. To remove condensation,
run the DC at its maximum temperature for at least 48 hours.
DC Periodic Maintenance
Inspect the door seal for signs of damage. A defective seal impairs the
performance of the instrument. If the seal is defective, contact Technical
Support for Dionex products.
203
7.12
DC Annual Maintenance
Thermo Fisher Scientific recommends performing preventive maintenance
annually. The DC preventive maintenance procedure consists of rebuilding
each high-pressure valve installed in the module. The following kits are
available:
204
ICS-5000+
TC
TC Routine Maintenance
This section describes routine maintenance procedures for the Dionex ICS5000+ Thermal Compartment (TC) that users may perform. All other
maintenance procedures must be performed by a Technical Support
Representative for Dionex products.
7.13
TC Daily Maintenance
Check the TC components for leaks or spills. Wipe up spills. Isolate and
repair leaks (see Section 8.31). Rinse off any dried eluent with ASTM
filtered, Type I (18 megohm-cm) deionized water that meets the
specifications listed in Section 1.5.
Check the liquid level in the waste container and empty as needed.
Neutralize acidic and caustic wastes before disposal. Dispose of all
wastes in accordance with local regulations.
7.14
TC Weekly Maintenance
7.15
TC Periodic Maintenance
Clean the interior of the TC, using a lint-free cloth. Use paper to absorb
any liquid inside the module. The cleaner the module, the more effective
the sensors are at detecting excessive gas or humidity.
205
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.
7.16
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.
TC Annual Maintenance
Thermo Fisher Scientific recommends performing preventive maintenance
annually. The TC preventive maintenance procedure consists of rebuilding
each high-pressure valve installed in the module. The following kits are
available:
206
8 Troubleshooting
This chapter is a guide to troubleshooting minor issues that may arise during
operation of the Dionex ICS-5000+ system. Turn to the section of this chapter
that best describes the operating problem or symptom that has been observed.
Each section lists possible causes of the problem or symptom in order of
probability. A systematic troubleshooting approach is the most effective way
to determine the root cause.
If you are unable to resolve a problem by following the instructions here,
contact Technical Support for Dionex products. In the U.S. and Canada, call
1-800-346-6390. Outside the U.S. and Canada, call the nearest Thermo Fisher
Scientific office. Please have this chapter at hand when talking with Technical
Support personnel.
8.1
Default
Severity Level
Description
Warning
Error
Abort
207
8.1.1
Default
Severity
Level
See
Abort
page 231
Warning
page 231
Abort
page 232
Abort
page 232
Abort
page 232
Abort
page 232
Degasser malfunction.
Warning
page 232
Abort
page 233
Abort
page 233
Abort
page 233
Abort
page 234
Motor malfunction.
Abort
page 234
Abort
page 234
Abort
page 235
Abort
page 236
Abort
page 234
Abort
page 236
Abort
page 237
Abort
page 237
208
8 Troubleshooting
Default
Severity
Level
See
Abort
page 237
Abort
page 238
Abort
page 238
8.1.2
EG Error Messages
Table 8-2 lists the EG-related error messages and their default severity levels.
For troubleshooting assistance, see the page indicated in the table.
EG-Related Audit Trail Error Message
Default
Severity
Level
See
Error
page 245
Error
page 245
Abort
page 245
Abort
page 246
Abort
page 246
Abort
page 247
Abort
page 247
Abort
page 247
Abort
page 248
209
Default
Severity
Level
See
Abort
page 248
Abort
page 248
Abort
page 249
Abort
page 249
Abort
page 249
Abort
page 250
Abort
page 250
Abort
page 251
Abort
page 251
Abort
page 252
Abort
page 252
Abort
page 253
Abort
page 253
Warning
page 253
Warning
page 254
210
8 Troubleshooting
Default
Severity
Level
See
Abort
page 254
Warning
page 255
Abort
page 255
Abort
page 255
Abort
page 256
Abort
page 256
Warning
page 256
Error
page 257
Warning
page 257
8.1.3
DC Error Messages
Table 8-3 lists the DC-related error messages and their default severity levels.
For troubleshooting assistance, see the page indicated in the table.
DC-Related Audit Trail Error Message
Default
Severity
Level
See
Abort
page 263
Abort
page 264
Abort
page 264
Abort
page 264
Warning
page 265
211
Default
Severity
Level
See
Abort
page 265
Abort
page 265
Warning
page 265
Warning
page 265
Abort
page 266
Abort
page 267
Warning
page 267
Warning
page 268
Warning
page 268
Abort
page 269
Error
page 270
Warning
page 271
Warning
page 271
Abort
page 271
Abort
page 272
Suppressor over-current.
Abort
page 272
Suppressor over-power.
Abort
page 272
Suppressor over-voltage.
Abort
page 273
Warning
page 273
Warning
page 273
212
8 Troubleshooting
8.1.4
TC Error Messages
Table 8-4 lists the TC-related error messages and their default severity levels.
For troubleshooting assistance, see the page indicated in the table.
TC-Related Audit Trail Error Message
Default
Severity
Level
See
Error
page 279
Error
page 279
Error
page 279
Error
page 279
Error
page 280
Warning
page 280
Warning
page 280
Abort
page 280
Error
page 281
Abort
page 281
Abort
page 281
Error
page 282
213
Default
Severity
Level
See
Error
page 282
Error
page 283
Abort
page 283
Communication error: x.
Abort
page 283
Communication time-out.
Abort
page 284
Warning
page 284
Abort
page 284
Warning
page 284
Warning
page 285
Warning
page 285
Abort
page 285
Abort
page 286
Abort
page 286
Abort
page 287
Warning
page 287
Abort
page 287
Error
page 288
214
8 Troubleshooting
Default
Severity
Level
See
Abort
page 281
Abort
page 288
Warning
page 288
Abort
page 289
Error
page 289
Error
page 289
Error
page 289
Illegal parameter.
Abort
page 290
Error
page 290
Warning
page 290
Warning
page 291
Warning
page 291
Error
page 291
Warning
page 291
Warning
page 291
Warning
page 291
Error
page 292
Warning
page 292
Abort
page 292
215
Default
Severity
Level
See
Warning
page 293
Warning
page 293
Error
page 294
Error
page 294
Error
page 294
Error
page 295
Warning
page 295
Warning
page 295
Warning
page 295
Warning
page 295
Warning
page 296
Abort
page 281
TC is not remote.
Abort
page 286
Error
page 296
Error
page 296
Warning
page 297
216
8 Troubleshooting
Default
Severity
Level
See
Warning
page 297
Error
page 297
Warning
page 298
Warning
page 298
Error
page 298
Error
page 298
Error
page 298
Warning
page 299
Error
page 299
Error
page 300
Error
page 300
Warning
page 300
Warning
page 300
Abort
page 301
Warning
page 301
217
Default
Severity
Level
See
Error
page 300
Warning
page 301
Error
page 301
Abort
page 287
Warning
page 293
Warning
page 293
X position error.
Abort
page 302
Error
page 302
Error
page 302
Error
page 302
8.2
Noisy Baseline
Eluent is contaminated
1. Clean all eluent reservoirs thoroughly (inside and out) with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, follow the cleaning instructions in Section 9.4.
2. Flush the system with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
3. Replace all end-line filters (P/N 045987). See Section 4.6 for
instructions.
4. Prepare new stock solution.
218
8 Troubleshooting
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.
219
220
8 Troubleshooting
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
221
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.
8.3
Liquid leaks
1. Check for leaks from the piston seals. Replace the piston seal on any
head with a leak (see Section 9.7).
2. Check for leaks throughout the remainder of the system, including the
check valves, injection valve, and columns. Tighten or replace fittings
as needed.
222
8 Troubleshooting
Eluent is contaminated
1. Clean all eluent reservoirs thoroughly (inside and out) with ASTM
Type I (18 megohm-cm) filtered and deionized water that meets the
specifications listed in Section 1.5. Dry with clean, particulate-free
air. If a reservoir still appears dirty, or if there is a slimy film on the
interior, follow the cleaning instructions in Section 9.4.
2. Flush the system with ASTM Type I (18 megohm-cm) filtered and
deionized water that meets the specifications listed in Section 1.5.
3. Replace all end-line filters (P/N 045987). See Section 4.6 for
instructions.
4. Prepare new stock solution.
5. Prepare fresh eluent. To ensure eluent purity, prepare all eluents with
electrochemical-grade chemicals, and ASTM Type I (18 megohmcm) filtered and deionized water that meets the specifications listed in
Section 1.5.
223
2. The column may be the source of the problem. Refer to the column
manual for troubleshooting assistance. Column manuals are provided
on the Thermo Scientific Reference Library DVD (P/N 053891).
3. The injection valve may be the source of the problem. Rebuild the
injection valve (see Section 9.22).
8.4
8.5
224
8 Troubleshooting
8.6
No Peaks
ED: Verify that the signal cables from the cell are connected to the
detector block. In addition, an electronics connector on the back of the
detector plugs into a receptacle on the detector compartment. Push on the
detector to make certain the connector is securely connected (see
Figure 8-1).
Push here to ensure that the
detectors electrical
connection is secure.
225
ED Only
Cell is off
Turn on the cell from the detector ePanel (in Chromeleon 7) or Control
panel (in Chromeleon 6.8).
8.7
Tailing Peaks
226
8 Troubleshooting
Capillary
IC
8.8
Loose fitting
Make sure there are no liquid leaks in the flow system. Check tubing
connections throughout the system (including the check valves, injection
valves, and columns) and tighten or replace fittings as needed.
227
NOTE
8.9
8.10
228
8 Troubleshooting
ED Only
8.11
High Background
Wrong eluent
Check that you are using the correct eluent for your application. For ED
detectors, verify that the pH readout is correct for your eluent.
229
CD Only
ED Only
230
ICS-5000+
DP/SP
8.12
DP/SP Troubleshooting
Troubleshooting DP/SP Error Messages
If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon audit trail.
A program with this name already exists.
This error occurs if you attempt to save a modified Chromeleon 7 instrument
method or Chromeleon 6.8 program under the name of an existing instrument
method or program.
To troubleshoot:
Enter a new name for the modified instrument method or program or select
Save to save your changes under the existing instrument method or program
name.
Abnormal drive current for x.x seconds.
If this error occurs, the tubing between the pump heads may be blocked or the
fitting may be overtightened.
To troubleshoot:
Inspect the tubing for blockage or crimping, and replace it as needed (see
Section 9.3). Be careful not to overtighten fittings. If the message appears
again, contact Technical Support for Dionex products for assistance.
231
232
8 DP/SP Troubleshooting
233
234
8 DP/SP Troubleshooting
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).
235
236
8 DP/SP Troubleshooting
237
4. Observe a run to see whether the high pressure limit is triggered when
injection occurs; if it is, the injection valve may be the source of the
blockage (i.e., the rotor seal or stator may need to be replaced). Contact
Technical Support for Dionex products for assistance.
This function cannot be adjusted by the user.
This error occurs if you attempt to change a parameter that users are not
allowed to adjust.
To troubleshoot:
Only qualified personnel can change this parameter. For assistance, contact
Technical Support for Dionex products.
Upper pressure limit exceeded.
This error occurs if the upper pressure limit specified in the Chromeleon 7
instrument method or Chromeleon 6.8 program is exceeded. The running
batch is aborted (default) and this message appears.
To troubleshoot:
1. Inspect the tubing for blockage or crimping, and replace it as needed (see
Section 9.3). Be careful not to overtighten fittings.
2. To determine the source of the high backpressure, isolate segments of the
flow path:
a. Remove the pump outlet tubing at the injection valve.
b. Press the POWER button on the front of the DP/SP to turn on the
pump.
c. 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. Record the backpressure.
d. Disconnect all components after the injection valve.
e. One at a time, reconnect each component of the flow path. If
reconnecting a component causes an abnormal increase in
backpressure, replace the component. Replace as many components
238
8 DP/SP Troubleshooting
8.13
Power is off
Check that the main power switch on the DP/SP rear panel is turned on.
Press the POWER button on the front of the DP/SP to turn on the pump.
239
8.14
240
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
8 DP/SP Troubleshooting
8.15
241
8.16
8.17
242
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
8 DP/SP Troubleshooting
8.18
243
244
ICS-5000+
EG
8.19
EG Troubleshooting
Troubleshooting EG Error Messages
If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon audit trail.
Concentration out of range! The maximum value is %1.
-or-
245
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
246
8 EG Troubleshooting
247
248
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
8 EG Troubleshooting
The Dionex ICS-5000+ IC system electronics components and instrument control firmware cannot be serviced by the user.
249
250
8 EG Troubleshooting
251
252
8 EG Troubleshooting
253
254
8 EG Troubleshooting
255
2. Verify that the Dionex EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
EGC is either not installed or invalid cartridge number. Please
install an analytical EGC.
This error occurs if no Dionex EGC cartridge is connected to the EG or if a
capillary Dionex EGC is connected to an analytical IC system.
To troubleshoot:
1. Verify that an analytical Dionex EGC is installed.
2. Verify that the Dionex EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
EGC is either not installed or invalid cartridge number. Please
install an EGC.
This error occurs if no Dionex EGC cartridge is connected to the EG or if the
cartridge serial number is not valid for the type of IC system.
To troubleshoot:
1. Verify that a Dionex EGC of the correct type (capillary or analytical) is
installed.
2. Verify that the Dionex EGC cable is securely plugged into the EG (see
Figure 2-10) and the locking ring is tightened.
Leak sensor wet.
This error occurs when liquid accumulates in the drip tray in the bottom of the
EG.
To troubleshoot:
1. Locate the source of the leak by visually inspecting the tubing, fittings,
and components in the EG.
256
8 EG Troubleshooting
8.20
Leaking fitting
Locate the source of the leak. Tighten or replace liquid line connections as
needed (see Section 9.12).
EGC leaks
Replace the Dionex EGC (see Section 9.14).
257
Electrical error
The EG current and/or voltage may have become unstable. Contact
Technical Support for Dionex products for assistance.
NOTE
8.21
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
No power
Check that the POWER button on the front of the EG is turned on.
Check that the EG main power switch (on the rear panel) is turned on.
Check that the main power cord is plugged into both the EG rear panel
connector and the power source. Check that the wall outlet has power.
If the POWER LED still fails to light, contact Technical Support for
Dionex products for assistance.
8.22
Leaking fitting
Locate the source of the leak. Tighten or replace liquid line connections as
needed (see Section 9.12).
258
8 EG Troubleshooting
EGC leaks
Replace the Dionex EGC (see Section 9.14).
8.23
No Flow
259
8.24
EG Stops Operation
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
EGC is expended
Replace the cartridge (see Section 9.14).
260
8 EG Troubleshooting
261
262
ICS-5000+
DC
8.25
DC Troubleshooting
Troubleshooting DC Error Messages
If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon audit trail.
CD cell option disconnected.
To troubleshoot:
1. Check the detector connection: An electronics connector on the back of
the detector plugs into a receptacle on the detector compartment. Push on
the upper part of the detector (see Figure 8-3) to make sure the connector
is securely connected.
2. If the error persists, there may be a problem in the detector electronics.
Contact Technical Support for Dionex products for assistance.
NOTE
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
Push here to
ensure the
detectors
electrical
connection is
secure.
263
264
8 DC Troubleshooting
265
266
8 DC Troubleshooting
ED Cell Cable
If the error appears again, contact Technical Support for Dionex products
for assistance. The detector electronics may have malfunctioned.
NOTE
The Dionex ICS-5000+ IC system electronics components cannot be serviced by the user.
267
268
8 DC Troubleshooting
High-Pressure
Valve #2 (not
installed in this
system)
HighPressure
Valve #3
HighPressure
Valve #4
269
HighPressure
Valve #3
HighPressure
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 Dionex ICS-5000+ IC system power briefly by pressing the
POWER button on the front of each module. Then press each button again
to restart the system.
3. Try to toggle the valve from Load to Inject by pressing the Load and
Inject buttons on the front of the DC.
If the problem persists, contact Technical Support for Dionex products for
assistance.
IC Cube 1 heater over safe temperature.
-or-
270
8 DC Troubleshooting
271
Suppressor over-power.
This error appears when, in order to maintain the selected current, the Dionex
ICS-5000+ IC system is required to apply a higher voltage than the suppressor
can support.
To troubleshoot:
1. Reduce the flow rate.
272
8 DC Troubleshooting
273
8.26
Leaking fitting
Locate the source of the leak. Tighten or, if necessary, replace the liquid
line connection (see Section 9.19).
Leaking cell
1. Check the waste lines for blockage; trapped particles can plug the
lines and cause a restriction and/or leak. If necessary, clear the waste
lines by reversing the direction of flow.
2. Make sure the plumbing downstream from the cell is clear; a
blockage may overpressurize the cell and cause it to leak. If the
problem continues, contact Technical Support for Dionex products
for assistance.
Leaking suppressor
Refer to the suppressor manual for troubleshooting procedures.
Suppressor manuals are provided on the Thermo Scientific Reference
Library DVD (P/N 053891).
274
8 DC Troubleshooting
8.27
8.28
ED Cell Troubleshooting
Check the
cable
connection
275
276
8 DC Troubleshooting
3. If soaking does not fix the problem, replace the electrode (see
Section 9.28.5).
To prevent a pH-Ag/AgCl reference electrode from drying out, make sure that
eluent is being pumped continuously through the cell. If the cell will not be
used for a short time (less than 2 days), disconnect the tubing from the inlet
and outlet fittings and all fitting plugs. For longer shutdowns, remove the
electrode from the cell and store it in a storage cap filled with saturated KCl
solution. See Section 4.1.2 for detailed instructions.
277
278
ICS-5000+
TC
8.29
TC Troubleshooting
Troubleshooting TC Error Messages
If any of the following alarm conditions occurs, a message is displayed in the
Chromeleon audit trail.
279
280
8 TC Troubleshooting
281
282
8 TC Troubleshooting
283
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.
Configuration doesnt match. X not installed.
-or-
284
8 TC Troubleshooting
285
For Chromeleon 6.8, the license features you purchased are listed on the
About Chromeleon screen and labeled On.
TC is not remote.
If you try to issue certain commands (for example, Column_x and
InjectValve_x commands) when the TC is not under Chromeleon control, the
appropriate message (shown above) is displayed.
To troubleshoot:
Select the Connect command to connect the TC to the Chromeleon server.
Check the audit trail for messages indicating whether the module was
successfully connected.
286
8 TC Troubleshooting
287
288
8 TC Troubleshooting
289
If you are using Chromeleon 6.8: On the TC Control panel, click the
Clear Alarm button.
3. Ventilate the interior of the TC thoroughly before closing the door and
resuming operation.
Illegal parameter.
This error occurs if you enter a parameter that is not valid for the TC.
To troubleshoot:
Select a valid parameter.
Invalid date/time format. Either use DD MMM YYYY or current [
+ [Nyear[s]] [Nmonth[s]] [Nday[s]]]. Examples: 31 Dec 1999,
current + 1 year 6 months.
This error occurs if you enter the date associated with an event in an invalid
format.
To troubleshoot:
Enter the date in the format specified in the message.
Invalid enumerated value.
This error occurs if you attempt to enter an invalid value for a property, rather
than selecting a value from the drop-down list box in the Command window
(Chromeleon 7) or the Commands dialog box (Chromeleon 6.8).
To troubleshoot:
Select a valid option from the drop-down list box available for this property.
290
8 TC Troubleshooting
291
To troubleshoot:
Contact Technical Support for Dionex products for information about
performing annual preventive maintenance. Thermo Fisher Scientific
recommends performing preventive maintenance annually. The DC/TC
preventive maintenance procedure consists of rebuilding each high-pressure
valve installed in the module. The following kits are available:
292
8 TC Troubleshooting
Value for [name] parameter is not within valid range. Value passed
(x) will be substituted by y.
-or-
293
294
8 TC Troubleshooting
3. If the door is fully closed but the error persists, contact Technical Support
for Dionex products for assistance.
Properties cannot be changedthere is no card in the card
reader.
This error occurs if you attempt to change column ID properties for a column
for which no chip card is installed.
To troubleshoot:
Insert a column ID chip card into the appropriate slot (see Section 9.30).
Raw data file x cannot be created.
-or-
295
296
8 TC Troubleshooting
297
298
8 TC Troubleshooting
To troubleshoot:
1. Open the Chromeleon 7 ePanel Set or the Chromeleon 6.8 panel tabset.
2. Press the F8 key to open the Command window (Chromeleon 7) or the
Commands dialog box (Chromeleon 6.8).
3. Check the status of each property listed in the error message. The table
below indicates the status required for operation.
Command
Status
CardState
OK
Door
Closed
Ready
Ready
Standby
NoStandby
4. When you identify the component that is not ready for operation, find and
eliminate the cause of the problem.
The primary column ID property x will be changed. The property
can't be changed in the future.
This error occurs when you modify a primary column property (batch or lot
number, date of manufacture, etc.). To prevent any unintended changes,
Chromeleon requests confirmation before saving the new property.
To troubleshoot:
If you are sure that the proposed change is correct, go ahead and save it.
The upper limit must be higher than the lower limit.
This error occurs if the value entered for a parameters 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.
299
300
8 TC Troubleshooting
301
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.
You do not have the privilege to approve the module's
qualification.
-or-
302
8 TC Troubleshooting
To troubleshoot:
The Chromeleon administrator is responsible for assigning privileges to
individual users or to user groups. Contact the administrator if you need one
or more of the above privileges assigned to you.
8.30
303
8.31
Leaking fitting
Locate the source of the leak. Tighten or, if necessary, replace the liquid
line connection (see Section 9.29).
304
8 TC Troubleshooting
8.32
8.33
TC calibration is incorrect
The TC cannot be calibrated by the user. Contact Technical Support for
Dionex products for assistance.
305
306
9 Service
This chapter describes Dionex ICS-5000+ IC system service and repair
procedures that users may perform. All procedures not included here,
including electronics-related repair procedures, must be performed by
Thermo Fisher Scientific personnel. For assistance, contact Technical Support
for Dionex products. In the U.S. and Canada, call 1-800-346-6390. Outside
the U.S. and Canada, call the nearest Thermo Fisher Scientific office.
Before replacing any part, see the troubleshooting information in Chapter 8 to
correctly identify the cause of the problem.
Substituting non-Dionex/Thermo Scientific parts may impair a modules
performance, thereby voiding the product warranty. Refer to the
warranty statement in the Dionex Terms and Conditions for more
information.
9.1
Connecting Tubing
High-pressure 10-32 fitting bolts (P/N 074449) and high-pressure 10-32
double-cone ferrules (P/N 074373) are used for most ICS-5000+ tubing
connections, even in low-pressure systems. When connecting tubing to a port,
make sure the 10-32 ferrule and fitting bolt are at least 2 mm (0.1 in) from the
end of the tubing before you insert the tubing into the port. Do not position the
ferrule and fitting bolt flush with the end of the tubing. Figure 9-1 shows the
correct and incorrect placement of the ferrule and fitting bolt on the tubing.
Correct
Incorrect
2 mm
Figure 9-1. Correct and Incorrect Ferrule and Fitting Bolt Placement for
Tubing Connections (High-Pressure Fitting and Ferrule Shown)
307
9.2
308
ICS-5000+
DP/SP
9.3
DP/SP Service
Replacing Tubing and Fittings
The DP/SP is plumbed with the tubing and fittings listed below.
Tubing Size and Type
Color
P/N
Used to connect
Black
068658
Red
044221
(1 in)
Black
042690
(1 in)
Orange
042855
(1 in)
Tan
054410
(1 in)
Yellow
063268
(1 in)
Colorless
064079
(1 in)
014157
(1 in)
Eluent reservoirs
047203
(1 in)
Colorless
Colorless
Vacuum degassing
assembly
309
Color
P/N
Used to connect
10 mm (0.39 in) ID
polyethylene
Colorless
055075
Tan
Tan
052230
062511
Tan
Yellow
052267
048949
High-pressure 10-32
fitting bolt
Blue
074449
High-pressure 10-32
ferrule, double-cone
Blue
074373
Blue
Blue
074449
074373
310
Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing, and that there are no nicks or
burrs on the end. A tubing cutter (P/N 049584) is included in the DC Ship
Kit (P/N 072011). Refer to the instructions provided with the cutter for
details.
9 DP/SP Service
9.4
Capillary
IC
9.5
To prime the pump with the PUMP PRIME button, see Section 9.5.1.
311
9.5.1
5. Open the priming valve on the secondary pump head (see Figure 9-2) by
turning it one-half turn counterclockwise.
NOTE
Priming Valve
312
9 DP/SP Service
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.
9.5.2
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. Select the priming flow rate. The default rate for a capillary IC pump is
3.0 mL/min. The default rate for an analytical IC pump is 6.0 mL/min.
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.
313
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.
NOTE
Priming will stop automatically after the time specified (in seconds) in the Duration box has elapsed. You
can set the duration to a preferred value.
314
9 DP/SP Service
9.6
Part Number
Capillary IC
Inlet
044541
Outlet
044540
Inlet
045722
Outlet
045721
Analytical IC
Additional items:
9.6.1
Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
315
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. Using a 1/2-inch open-end wrench, loosen both check valve assemblies.
10. Remove both check valve assemblies from the pump head.
316
9 DP/SP Service
9.6.2
Double-hole
Inlet Check Valve
Assembly
Flow
Single-hole
Outlet Check
Valve Assembly
Flow
317
NOTE
The pump cannot operate properly unless the cartridges are installed in their respective housings in the
correct orientation. Liquid enters the check valve
through the large single hole and exits through the
small double holes.
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.
318
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.
9 DP/SP Service
9.7
NOTE
Before beginning, locate the following items in your pump ship kit:
Part Number
072112
062463
072111
063342
319
Additional items:
9.7.1
Small beaker
ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5
Methanol (optional)
Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
320
9 DP/SP Service
7. Disconnect all tubing connections to the pump head with the defective
piston seal.
8. The primary and secondary pump heads have different components.
When disassembling a pump head, see Figure 9-6 for a primary pump
head or Figure 9-7 for a secondary pump head.
B
8
3
2
1
10
1 Piston
2 Seal Retainer
6 Backup Ring
321
5
6
10
12
11
4
3
2
1
9 Priming Valve
P/N 063968
(Capillary and Analytical)
1 Piston
2 Seal Retainer
6 Backup Ring
11 Membrane
12 Pressure Transducer
P/N 063382
(Capillary and Analytical)
P/N 062081
(Capillary and Analytical)
Assembly; P/N 062057
(Capillary and Analytical)
9. Using the 3.0 mm hex key (P/N 062338), loosen the two screws on the
pump head with the defective seal. Remove the screws, and then carefully
remove the head and place it on a clean surface.
10. Remove the seal wash body from the pump head. Or, if the seal wash
body was not removed with the pump head in Step 9, pull it straight out of
the pump mechanism now.
11. Pull the piston out of the pump mechanism.
NOTE
322
9 DP/SP Service
9.7.2
9.7.3
4. If the piston seal was not removed in Step 3, follow these steps:
a. Verify that the 10-32 fitting plugs in the inlet and outlet holes are
tightened enough to prevent any leaks from the pump head.
b. Fill the piston cavity with water and check for bubbles.
c. If there are no bubbles, repeat Step 3.
323
9.7.4
9.7.5
Figure 9-8. Piston Seal Wash Seal and Seal Insertion Tool
c. Insert this end of the tool partway into the seal wash body. Make sure
the tool is centered and does not rock back and forth. Then, press
firmly on the tool and the seal wash body until they snap together.
d. Remove the seal insertion tool from the seal wash body.
324
9 DP/SP Service
e. The seal wash seal is now partially installed. To complete the seal
installation, place the retainer in the seal wash body and use the large
flat-blade screwdriver to tighten the retainer.
f.
Place the new O-ring (P/N 040695) on the seal wash body.
NOTE
When replacing a piston seal, always replace the Oring, also. This will prevent leaks.
g. Place the new backup ring (capillary pump: P/N 074371; analytical
pump: P/N 074370) on the seal wash body.
2. Rinse the new main piston seal (capillary pump: P/N 075493; analytical
pump: P/N 075768) with isopropyl alcohol (IPA) or dip it into a container
of IPA. (The seal is easier to install when it is moist.)
3. Insert the piston through the seal wash assembly, and then through the
new main piston seal.
4. Make sure the piston seal is centered.
If the piston seal is not centered, applying pressure to it in Step 7 will
damage the seal and make it unusable.
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.
325
9.7.6
9.8
Removing the pump head and the old piston (see Section 9.8.1)
NOTE
326
9 DP/SP Service
Before beginning, locate the 3.0 mm hex key (P/N 062338) in your pump ship
kit:
Pump Ship Kit
Part Number
072112
062463
072111
063342
Additional items:
9.8.1
ASTM Type I (18 megohm-cm) filtered and deionized water that meets
the specifications listed in Section 1.5
Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
327
7. Disconnect all tubing connections to the pump head with the damaged
piston.
8. Using the 3.0 mm hex key (P/N 062338), loosen the Allen screws on the
pump head with the damaged piston. Remove the Allen screws, and then
carefully remove the head and place it on a clean surface.
9. If the piston was not removed with the pump head in Step 8, remove the
piston now by pulling it straight out of the pump mechanism.
NOTE
10. If the piston is broken, be sure to remove all broken pieces. If necessary,
flush the pump head with ASTM Type I (18 megohm-cm) filtered and
deionized water.
9.8.2
9.8.3
328
9 DP/SP Service
9.9
329
d. Pull on the fitting slightly to remove the PharMed tubing from the
upper notch on the pump mounting plate.
1
2
3
4
PharMed Tubing
(P/N 063268)
Rotor
Lever
Mounting Plate
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:
330
Part Number
072112
062463
072111
063342
9 DP/SP Service
PharMed
Tubing
Tygon 2075
Tubing
Seal
Wash
Reservoir
Secondary
Head
Primary
Head
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.
331
9.10
Press the POWER button on the front of the DP/SP for 2 seconds to
turn off the pump.
Priming Valve
Secondary
Pump Head
332
9 DP/SP Service
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.
9.11
333
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 VOLTAGEDisconnect the main power cord from its source and
also from the rear panel of the pump.
Fuse
Cartridge
334
ICS-5000+
EG
9.12
Capillary
IC
EG Service
Replacing Tubing and Fittings
Color
P/N
Use to connect
Tubing assembly,
precision cut,
0.062 mm (0.0025 in)
ID PEEK, 61 cm (24 in)
Blue
072203
Tubing assembly,
precision cut,
0.062 mm (0.0025 in)
ID PEEK, 18 cm (7 in)
Blue
072204
Tubing assembly,
0.25 m (0.010 in) ID
PEEK, 64 cm (25 in)
Black
072224
Tubing assembly,
1.58 mm (0.062 in) ID
ETFE (ethylene
tetrafluoroethylene),
2.1 m (7 ft)
Clear
072225
10 mm (0.39 in) ID
polyethylene
Colorless
055075
335
Tubing/Fitting Size
and Type
Color
P/N
Use to connect
High-pressure 10-32
fitting bolt
Blue
074449
High-pressure 10-32
ferrule, double-cone
Blue
074373
336
Do not cut the 0.062 mm (0.0025 in) ID blue PEEK tubing used for
capillary IC connections. To ensure good chromatographic results, this
tubing must be cut at the factory, using a specialized precision cutter. If
you need to replace any tubing of this type, order the appropriate
precision cut tubing assembly listed in Table 9-3.
When replacing capillary tubing, make sure the 10-32 fitting bolt
(P/N 074449) and 10-32 double-cone ferrule (P/N 074373) are at least
2 mm (0.1 in) from the end of the tubing before you insert the tubing into
the port. Do not position the ferrule and fitting bolt flush with the end of
the tubing. For detailed connection instructions, see Section 9.1.
For tightening requirements for the 10-32 fitting bolt (P/N 074449) and
10-32 double-cone ferrule (P/N 074373), see Section 9.2.
9 EG Service
Color
P/N
Used to connect
Black
042690
(1 in)
Colorless
047203
10 mm (0.39 in) ID
polyethylene tubing
Colorless
055075
Tan
Yellow
052267
048949
For tightening requirements for the 10-32 fitting bolt (P/N 074449) and
10-32 double-cone ferrule (P/N 074373), see Section 9.2.
Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing, and that there are no nicks or
burrs on the end. A tubing cutter (P/N 049584) is included in the DC Ship
Kit (P/N 072011). Refer to the instructions provided with the cutter for
details.
337
9.13
9.14
338
9 EG Service
EGC
Cables
339
5. Close or cap the Dionex EGC vent opening to prevent leakage when you
turn over the cartridge in Step 7.
Capillary
IC
Capillary EGC
Vent Fitting
Vent Fitting
EGC
Vent Line
Luer
Adapter
If necessary, use a
wrench to hold the
luer adapter in place
while unscrewing the
vent line.
Figure 9-16. Analytical Dionex EGC Vent Line
(Standard-Pressure Cartridge Shown)
b. Locate the 10-32 plug (P/N 053981) removed from the Dionex EGC
vent opening during installation. Install the plug in the vent opening.
If you are removing a high-pressure analytical Dionex EGC, tighten the
vent fitting in the top of the Dionex EGC.
6. Lift the Dionex EGC straight up and off the cartridge holder.
340
9 EG Service
7. Turn the Dionex EGC upside down and place it on the EG drip tray (see
Figure 9-17). This is the service position for the cartridge.
EGC (Standard-Pressure Analytical)
Generation
Chamber
Electrolyte
Reservoir
Drip Tray
8. Disconnect the EGC IN and EGC OUT lines from the INLET and OUTLET
ports on the Dionex 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
341
342
9 EG Service
Vent
EGC
(Capillary)
EGC
IN
EGC
OUT
To EG Degas
Regen Out
(blue label)
REGEN IN
To CR-TC
Eluent In
(red label)
REGEN OUT
To CR-TC
Eluent Out
(yellow label)
To CR-TC
Regen In
(orange label)
4
To Inject
Valve
ELUENT IN
WASTE, GAS
SEPARATOR
To CR-TC
Regen Out
(blue label)
EG
Degas
Cartridge
(inside DC)
ELUENT OUT
TO PUMP/DAMPER
ELUENT OUT
Capillary
IC
To EG Degas
Eluent In
(red label)
343
2. Verify that the vent fitting on top of the Dionex EGC is tightened.
3. Turn the cartridge upside down and place it on the EG drip tray.
4. Remove the plugs from the INLET and OUTLET fittings on the eluent
generation chamber.
5. Locate the 38 cm (15 in) piece of 0.025 mm (0.001 in) ID tan PEEK
tubing (P/N 074582) in the IC Cube Ship Kit (P/N 072003).
6. Connect one end of this line to the Dionex EGC INLET port; connect the
other end to the EGC IN line from the pump pulse damper (see
Figure 9-19). (This is a temporary connection, to provide backpressure
during the Dionex EGC setup procedure.)
7. Connect a piece of 0.25 mm (0.010 in) ID black PEEK tubing to the
Dionex EGC OUTLET port. Direct the other end of the tubing to waste.
(This is a temporary connection.)
Capillary EGC Flushing:
Pump at 0.02 mL/min for 20 min
EGC
(Capillary)
Electrolyte Reservoir
EGC
IN
Electrolyte Generation
Chamber
EGC
OUT
Figure 9-19. Flow Schematic for Flushing the Capillary Dionex EGC
344
9 EG Service
9. Push the Dionex EGC electrical cable firmly into the EGC 1 (or EGC 2)
bulkhead connector (see Figure 9-14). Twist the ring on the cable
connector fingertight to secure it.
10. Unscrew the fitting on the top of the Dionex EGC a few turns to vent the
Dionex EGC.
To ensure proper ventilation, always loosen the fitting on the top of the
capillary Dionex 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. Eluent Generator panel: Verify that the Dionex CR-TC is off.
To avoid damaging the suppressor and Dionex CR-TC, always turn
them off before flushing the Dionex EGC. The pump flow is on during
flushing; however, no flow reaches the suppressor or Dionex CR-TC.
c. Pump panel: Set the flow rate to 0.02 mL/min. This turns on the pump
flow, also.
12. Flush the capillary Dionex EGC for 20 minutes and then turn off the
pump flow.
13. Disconnect the temporary tubing from the Dionex EGC OUTLET port.
345
Capillary
IC
1. Use a high-pressure (blue) fitting bolt and ferrule to connect the EGC OUT
line from the ELUENT IN port of the Dionex CR-TC to the Dionex EGC
OUTLET port (see Figure 9-21).
2. Disconnect the lines from the ELUENT OUT and REGEN IN port of the
Dionex CR-TC.
3. Connect a piece of 0.25 mm (0.010 in) ID PEEK tubing between the
ports. (This is a temporary connection.)
Capillary EGC Conditioning:
Pump at 0.02 mL/min for 15 min
EGC concentration at 50 mM
EGC
(Capillary)
EGC
IN
0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly
(P/N 072204)
EGC
OUT
ELUENT
IN
TO PUMP/DAMPER
ELUENT OUT
To CR-TC
Eluent In
(red label)
REGEN IN
To CR-TC
Regen Out
(blue label)
To CR-TC
Eluent Out
(yellow label)
To CR-TC
Regen In
(orange label)
Figure 9-21. Flow Schematic for Conditioning the Capillary Dionex EGC
346
9 EG Service
347
the appropriate figure when performing Dionex EGC and CR-TC service
procedures for an analytical IC system.
EGC VENT
EGC
RFIC+
Eluent
Degasser
To Waste
Vent
(via EG
rear wall)
Eluent
Out
Inlet
Outlet
EGC
IN
To
Waste
EGC
OUT
TO PUMP
Eluent
In
Coupler
(via EG
rear wall)
TO INJ VALVE - P
TO CR -TC
REGEN OUT
(blue label)
To CR-TC
Eluent In
(red label)
To CR-TC
Regen In
(orange label)
To CR-TC
Eluent Out
(yellow label)
REGEN IN
WASTE, GAS
SEPARATOR
Coupler
ELUENT OUT
TO SRS/AES
REGEN OUT
CR-TC
348
9 EG Service
EGC VENT
RFIC+
Eluent
Degasser
EGC
Vent
To Waste
Eluent
Out
(via EG
rear wall)
Inlet
Eluent
In
Outlet
To Waste
EGC
IN
TO PUMP
EGC
OUT
Coupler
(via EG
rear wall)
TO INJ VALVE - P
Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Eluent In
(red label)
To CR-TC
Eluent Out
(yellow label)
REGEN IN
TO CR -TC
REGEN OUT
(blue label)
ELUENT OUT
WASTE, GAS
SEPARATOR
To CR-TC
Regen In
(orange label)
CR-TC
349
3. Turn the cartridge upside down and place it on the EG drip tray in the
service position (see Figure 9-16).
4. Remove the plugs from the INLET and OUTLET fittings on the eluent
generation chamber.
5. Connect the EGC IN line from the pump to the Dionex EGC INLET port.
6. Locate the yellow 0.5 mL/min, 7 MPa (1000 psi) backpressure coil
(P/N 053765) in the EG Ship Kit (P/N 075780).
7. Connect one end of the
backpressure coil to the Dionex
EGC OUTLET port; leave the
other end of the coil unconnected
(see Figure 9-24). (This is a
temporary connection.)
Backpressure Coil
EGC
Outlet
Port
350
9 EG Service
9. Slide the Dionex EGC (with the electrolyte reservoir on top) into the
holder in the EG (see Figure 9-25).
EGC (Standard-Pressure Analytical)
11. Push the Dionex EGC electrical cable firmly into the EGC 1 (or EGC 2)
bulkhead connector (see Figure 9-14). Twist the ring on the cable
connector fingertight to secure it.
12. Connect the VENT line removed from the old cartridge to the vent opening
in the new cartridge (see Figure 9-16).
351
EGC VENT
EGC
To Waste
(via EG
rear wall)
Inlet
Outlet
EGC
IN
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 Dionex EGC OUTLET
port to the waste container. The backpressure must be at least 1.4 MPa
(200 psi).
2. On the Chromeleon 7 ePanel Set or Chromeleon 6.8 panel tabset, select
the following settings:
a. DC panel: Verify that the suppressor Mode is off.
b. Eluent Generator panel: Verify that the Dionex CR-TC is off.
To avoid damaging the suppressor and Dionex CR-TC, always turn
them off before conditioning the Dionex EGC. The pump flow is on
during conditioning; however, no flow reaches the suppressor or
Dionex CR-TC.
352
9 EG Service
c. Pump panel:
All pumps: Set the flow rate to 1.0 mL/min. This turns on the
pump flow, also.
353
9.15
Installing and hydrating the new Dionex CR-TC (see Section 9.15.2)
Completing the plumbing for the new Dionex CR-TC (see Section 9.15.3)
See Figure 9-18 for a flow schematic of the EG and Dionex CR-TC for
capillary IC. See Figure 9-22 or Figure 9-23 for a flow schematic for
standard-pressure or high-pressure analytical IC, respectively.
354
9 EG Service
355
d. Connect the EGC OUT line to the Dionex CR-TC ELUENT IN port and
connect the waste line to the Dionex CR-TC REGEN OUT port.
EGC
(Capillary)
EGC
IN
0.062 mm
(0.0025 in) ID
PEEK Tubing
Assembly
(P/N 072204)
EGC
OUT
ELUENT
IN
TO PUMP/DAMPER
REGEN IN
To CR-TC
Eluent In
(red label)
ELUENT OUT
To CR-TC
Regen Out
(blue label)
To CR-TC
Regen In
(orange label)
To CR-TC
Eluent Out
(yellow label)
356
9 EG Service
TO CR -TC
REGEN OUT
(blue label)
REGEN IN
To CR-TC
Eluent In
(red label)
ELUENT OUT
Eluent Out
(yellow label)
Regen In
(orange label)
b. Pump panel:
357
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.
358
9 EG Service
To EG Degas
Cartridge
Regen Out
ELUENT OUT
To CR-TC
Eluent In
(red label)
REGEN IN
To CR-TC
Regen Out
(blue label)
To CR-TC
Eluent Out
(yellow label)
To CR-TC
Regen In
(orange label)
To EG Degas
Cartridge
Eluent In
359
To RFIC+ Eluent
Degasser
ELUENT IN Port
To EGC
OUTLET Port
Coupler
TO SRS/AES
REGEN OUT
To CR-TC
Eluent In
(red label)
To CR-TC
Eluent Out
(yellow label)
REGEN IN
TO CR -TC
REGEN OUT
(blue label)
ELUENT OUT
WASTE, GAS
SEPARATOR
To CR-TC
Regen In
(orange label)
CR-TC
8. Check that no liquid lines are caught under the Dionex CR-TC. Align the
two mounting holes on the Dionex CR-TC back plate with the ball studs
on the mounting plate, and then push the Dionex CR-TC firmly onto the
mounting ball studs. The Dionex CR-TC clicks into place when properly
installed.
9. Push the Dionex CR-TC electrical cable firmly into the CR-TC 1 (or CR-TC
2) bulkhead connector. Twist the ring on the cable connector fingertight to
secure it.
10. Push the tray into the module until it locks into place. Close the EG door.
360
9 EG Service
9.16
9.17
If the backpressure is too low, install a backpressure coil (see Table 9-5)
between the injection valve and the OUTLET port on the Dionex EGC.
361
Connect one end of the backpressure coil to port P (2) on the injection valve;
connect the other end to the TO INJ VALVE IN - P line.
The EG Ship Kit (P/N 075780) includes four backpressure coils (see
Table 9-5).
Part
Number
Backpressure
Coil Description
Flow Rate
Approximate
Backpressure Added
AAA-053762
4 mm ID
2.0 mL/min
1.0 mL/min
2.0 mL/min
1.0 mL/min
0.50 mL/min
0.25 mL/min
0.50 mL/min
0.25 mL/min
AAA-053763
053764
053765
4 mm ID
2 mm ID
2 mm ID
362
9 EG Service
9.18
HIGH VOLTAGEDisconnect the main power cord from its source and
also from the rear panel of the EG.
Fuse
Drawer
Tab
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.
363
364
ICS-5000+
DC
9.19
Capillary
IC
DC Service
Replacing Tubing and Fittings
Color
P/N
Used to connect
N/A
072186
Blue
049714
(1 in)
N/A
074221
High-pressure 10-32
fitting bolt
High-pressure 10-32
ferrule, double-cone
Blue
074449
Blue
074373
Black
Black
062980
062978
Tan
052230
Clear
cone, tan
flat
062511
High-pressure 10-32
fitting bolt
High-pressure 10-32
ferrule, double-cone
Blue
074449
Blue
074373
365
Capillary
IC
Table 9-7 lists the tubing and fittings in the IC Cube Tubing Kit (P/N 072186).
Part
Length/
Quantity
Part
Number
Used to Connect
65 mm
(2.56 in)
072188
50 mm guard column
outlet to 250 mm
separator column inlet
115 mm
(4.53 in)
072189
75 mm
(2.93 in)
074603
35 mm guard column
outlet to 150 mm
separator column inlet
210 mm
(8.27 in)
072187
610 mm
(24 in)
042690
EG degas cartridge
REGEN OUT to waste (if
an EG is not present)
914 mm
(36 in)
042696
High-pressure 10-32
fitting bolt, blue
074449
EG degas cartridge
ELUENT OUT to
injection valve
Guard column to
separator column
Separator column to
suppressor
High-pressure 10-32
ferrule, double-cone
074373
366
9 DC Service
Capillary
IC
The 0.062 mm (0.0025 in) ID blue PEEK tubing (capillary tubing) used
for IC Cube connections is cut at the factory, using a specialized precision
cutter. If you need to replace any of this type of tubing, order an IC Cube
Tubing Kit (P/N 072186) or the individual tubing listed in Table 9-7.
When replacing capillary tubing, make sure the ferrule and fitting bolt are
at least 2 mm (0.1 in) from the end of the tubing before you insert the
tubing into the port. Do not position the ferrule and fitting bolt flush with
the end of the tubing. For detailed connection instructions, see
Section 9.1.
Except for capillary tubing, you can use a tubing cutter to cut tubing to the
required length. Make sure the cut is at a right angle to the length of the
tubing, and that there are no nicks or burrs on the end. A tubing cutter
(P/N 049584) is included in the DC Ship Kit (P/N 072011). Refer to the
instructions provided with the cutter for details.
For tightening requirements for the 10-32 fitting bolt (P/N 074449) and
10-32 double-cone ferrule (P/N 074373), see Section 9.2.
367
Color
P/N
Used to connect
Green
044777
(1 in)
Blue
049714
(1 in)
Blue
Blue
074449
074373
Black
Black
062980
062978
Tan
052230
Clear
cone, tan
flat
062511
Colorless
014157
(1 in)
Red
044221
(1 in)
Microbore systems:
Connections between
other system components
Black
042690
(1 in)
Tan
Yellow
052267
048949
Black
Tan
074449
043276
368
9 DC Service
9.20
Use a tubing cutter to cut tubing to the required length. Make sure the cut
is at a right angle to the length of the tubing, and that there are no nicks or
burrs on the end. A tubing cutter (P/N 049584) is included in the DC Ship
Kit (P/N 072011). Refer to the instructions provided with the cutter for
details.
For tightening requirements for the 10-32 fitting bolt (P/N 074449) and
10-32 double-cone ferrule (P/N 074373), see Section 9.2.
2. Locate the metal release tab under the sample loading port on the front of
the DC (see Figure 9-32). Press up on the tab to release the port and pull
the port out the front of the DC.
Sample Loading
Ports
Release Tabs
369
4. Attach the luer adapter fitting to the front of the port (see Figure 9-33).
4
3
2
1
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.
9.21
370
9 DC Service
Leak
Sensor
Loosen
this
screw
Disconnect
cables
371
10. Make sure the leak sensor does not touch the bottom of the drip tray.
9.22
NOTE
372
9 DC Service
9.23
NOTE
Electronics-related repair procedures must be performed by Technical Support for Dionex products.
373
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.
3. Open the DC door.
4. Disconnect each liquid line connected to the valve.
5. Unscrew the locking ring on the outside of the valve (see Figure 9-36)
and remove the ring.
Locking Ring
6. Grasp the front of the valve pod and pull out firmly to remove it from the
DC or AM.
7. Align the slots in the new pod with the runner in the valve holder on the
DC or AM (see Figure 9-37). Valve pods are keyed to fit only one way
(one slot is narrower than the other). Verify that the slots are aligned with
their matching runners.
374
9 DC Service
8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-37). If necessary, twist the end of the
pod to adjust the position of the splines.
Valve Pod
Valve Holder
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 power to the DC.
12. Turn on the pump flow. Check for leaks from the valve. Tighten fittings as
required. For tightening requirements for the 10-32 fitting bolt
(P/N 074449) and 10-32 double-cone ferrule (P/N 074373), see
Section 9.2.
13. Close the door.
375
9.24
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 9-38). Save the screws.
Remove two
screws
Figure 9-38. DC Rear Panel: Removing the I/O Option Cover Plate
376
9 DC Service
5. Slide the new I/O option board (P/N 062201) into the rear panel opening
and press firmly to connect the board to the DC motherboard.
6. Replace the two screws.
Figure 9-39 shows the I/O option installed.
I/O
Option
9.25
377
Fuse
Drawer
Tab
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.
378
9 DC Service
9.26
Cartridge
Thumbscrews
379
4. Loosen the two thumbscrews on the column cartridge and pull the
cartridge out of the IC Cube.
380
9 DC Service
5. Lift the lid of the column cartridge to open it. Figure 9-43 shows the
column cartridge when a capillary guard column and a capillary separator
column are installed.
Separator
1 Column Outlet
Separator
3 Column Inlet
Separator
2 Column
4 Precision Cut
Tubing
Guard Column
5 Outlet
5
6
6 Guard Column
7 Guard Column
Inlet
8 Precision Cut
Tubing
Figure 9-44 shows the column cartridge when only a capillary separator
column is installed.
3
2
Separator
Column Outlet
Separator
Column
Separator
Column Inlet
Precision Cut
Tubing
381
Do not cut the tubing that you removed from the columns 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 configuration), order an IC Cube Tubing Kit (P/N 072186).
9. Before installing the new separator column, tear off the column label and
slide it into the holder on the front of the cartridge (see Figure 9-49).
382
9 DC Service
10. If the new column configuration is the same as the previous one, connect
the precision cut tubing that you removed in Step 8 to the new columns.
If you are changing the column configuration, see the following figures
for the precision cut tubing required for your configuration:
3
2
250 mm Separator
Column
65 mm (2.5 in)
Precision Cut Tubing
(P/N 072188)
50 mm Guard
Column
150 mm Separator
1 Column
75 mm (3 in)
2 Precision Cut Tubing
(P/N 074603)
35 mm Guard
3 Column
383
Separator
1 Column
2
1
11. Remove the fitting plug from the outlet fitting on the separator column.
Orient the fitting with a flat side up and push the fitting into the opening at
the front of the column cartridge until it stops (see Figure 9-45).
12. Coil the separator column tubing inside the cartridge as shown in
Figure 9-43 or Figure 9-44. Secure the column and the inlet fitting in the
clips on 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 9-49).
NOTE
384
9 DC Service
Separator Column
Outlet
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 9-42).
22. Close the DC upper door.
385
9.27
CD Service Procedures
Items Needed
Description
Backpressure tubing to
provide at least 7 MPa
(1000 psi)
1. Click the CD tab on the Chromeleon 7 ePanel Set or the Cond. Detector
tab on the Chromeleon 6.8 panel tabset.
2. Under Detector Settings, click Calibration. The Wellness panel opens
(see Figure 9-50).
386
9 DC Service
387
2. Press the POWER button on the front of the DC for 2 seconds to turn off
the DC.
To avoid injury, wait for the DC to cool down before opening the door or
performing any maintenance or service procedures.
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 9-51). Press the suppressor against the back of the
detector and then slide it to the right to secure it onto the mounting tabs.
Pull out slightly on the center of the suppressor to verify that it is securely
fastened.
388
9 DC Service
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 9-52).
Disconnect tubing
Release Lever
4. For an analytical CD, remove the suppressor from the detector. For
instructions, see Section 9.27.2.
5. Press the release lever located below the detector (see Figure 9-52). The
detector pops out slightly from the DC compartment. Grasp the top of the
detector and pull outward to remove the detector from the compartment.
Do not pull from the CELL IN and CELL OUT fittings.
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.
389
Column
Format
Flow Rate
(mL/min)
Backpressure
Coils
AES
2 mm
0.25 to 0.50
2 red*
3 mm
0.50 to 1.00
2 red
4 mm
1.00 to 2.00
1 red
2 mm or 3 mm
<0.25
2 red
2 mm or 3 mm
0.25 to 0.50
1 red
SRS or MMS
*The red coil (P/N 045878) consists of 0.125 mm (0.005 in) ID PEEK tubing
with fittings.
Table 9-10 lists the correct pressure range for each type of suppressor.
Dionex Suppressor Type
Pressure Range
AES
SRS or MMS
390
9 DC Service
3. If a bubble is still trapped in the cell, try these techniques to remove it:
9.28
ED Service Procedures
391
NOTE
Inlet Line
Outlet line
4. Grasp the cell by the cell body and pull straight out to remove it from the
detector.
392
9 DC Service
Replace the gasket if there is a leak between the gasket and electrode, or
between the gasket and cell body.
Items Needed
Gloves
Blunt-end tweezers
393
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 9-54).
First, loosen the
yoke knob
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 then pull the block
and knob off the working electrode (see Figure 9-54).
NOTE
394
9 DC Service
5. Use tweezers to remove the old cell gasket from the cell body (see
Figure 9-56).
Alignment
Pins
Conventional
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.
395
NOTE
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 cells 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
396
Gloves
9 DC Service
Tweezers
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:
NOTE
NOTE
397
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 1 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 polishing compound from the pads. After initial use, add
only enough polishing compound to maintain the coating on the pad.
7. Replace the working electrode block and yoke knob. Fingertighten the
knob by turning it a full 360 degrees.
NOTE
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 cells inlet and outlet lines.
10. Reconnect the electrical cables.
11. Start the pump flow.
398
9 DC Service
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.
399
2. Unscrew the pH-Ag/AgCl reference electrode and remove it from the cell
body (see Figure 9-57).
Unscrew
the pH-Ag/AgCl
reference electrode
3. Unscrew the storage cap from the new pH-Ag/AgCl reference electrode
(see Figure 9-58). 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
400
9 DC Service
Items Needed
401
402
9 DC Service
Capillary
IC
pH-Ag/AgCl
Reference
Electrode
O-Ring
(Remove for
capillary IC)
Reference
Electrode Gasket
for Capillary IC
403
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 9-62).
Reference
Electrode Well
Inlet
Reference
Electrode Well
Outlet
Figure 9-62.
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.
404
9 DC Service
pH-Ag/AgCl
Reference
Electrode
O-Ring
3.
Orient the cell assembly with the yoke knob on the left (see Figure 9-53)
and push the cell onto its mounting location in the DC compartment.
4.
5.
6.
7.
Wait until the pump pressure has stabilized (30 to 60 seconds) and then
turn on the cell voltage.
405
Unscrew the
pH-Ag/AgCl
reference
electrode
pH-Ag/AgCl
Reference
Electrode
O-Ring
406
9 DC Service
Replace the PdH reference electrode if its sensing surface is damaged or if the
electrode no longer seals properly. Replace the PdH electrode if performance
has degraded; for example, you observe lower response, higher background,
or spikes.
The PdH reference electrode typically lasts several years, depending on use.
Items Needed
Tweezers
Wrench
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.
407
2. Use a wrench to unscrew the PdH reference electrode nut and then
remove the nut from the reference electrode well (see Figure 9-67).
Nut
3. Pull the reference electrode out of the well (see Figure 9-68).
PdH Reference
Electrode
408
9 DC Service
4. Using tweezers, remove the PdH reference electrode gasket from the well
(see Figure 9-69).
Notch in
well
PdH Reference
Electrode Gasket
PdH Reference
Electrode Gasket
6. Align the gasket so that the notched edge of the gasket aligns with the
corresponding notch in the reference electrode well, and then press the
gasket into the well.
409
Knobs
Grooves
Figure 9-71. 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 9-72). After fingertightening,
use a wrench to tighten the nut an additional 20 to 30 degrees.
Nut
410
9 DC Service
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 (see the instructions below).
Conditioning the PdH Reference Electrode
411
3. Open the DC upper door and disconnect the cell inlet and outlet lines.
4. Disconnect the reference electrode cable and the cell cable.
5. Grasp the cell body and pull straight out to remove the cell from the
detector.
6. Press the release lever located below the detector. The detector pops out
slightly from the DC compartment. Grasp the detector and pull outward to
remove the detector from the compartment.
7. Note the electrical plug on the back of the detector and the receptacle on
the inside of the DC.
8. Push the new detector into the opening in the DC and press firmly to
ensure the electrical connection is secure.
9. Reinstall the cell and reconnect the cell inlet and outlet lines and the
cables.
NOTE
412
If you are installing an ED detector in a system that previously was set up for conductivity detection, remove the suppressor cartridge from the IC Cube and replace it with a
suppressor bypass cartridge (P/N 072055). For IC Cube cartridge installation instructions, see Section 9.26.1.
ICS-5000+
TC
TC Service
To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.
9.29
Color
P/N
Used For
Black
052310
Standard bore
system connections
Red
052306
Microbore system
connections
Colorless
055075
Waste line
Use 10-32 fitting bolts (P/N 074449) and 10-32 double-cone ferrule
fittings (P/N 074373) for all tubing connections. For tightening
requirements, 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 that there are no nicks or
burrs on the end.
413
9.30
Close the TC door and select the column properties you want to monitor.
414
9 TC Service
4. Select the check box for the column to be monitored (A, B, C, or D) and
click OK.
To install a column ID chip card:
415
9.31
NOTE
416
9 TC Service
6. Reconnect all liquid lines to the injection valve (see Figure 9-76).
(Green)
SAMPLE IN
(from door
inject port or
autosampler)
TO INJECT
VALVE -W
W (6)
S (5)
25 L SAMPLE LOOP
(Orange)
TO INJECT
VALVE -P
L (4)
TO INJ
VALVE -C
(Red - microbore)
(Black - standard bore)
9.32
NOTE
417
1. Turn off the pump flow from the ePanel in Chromeleon 7 or the Control
panel inChromeleon 6.8, or press PUMP FLOW on the front of the pump.
To avoid injury, wait for the TC to cool down before opening the door or
performing any maintenance or service procedures.
Black
Locking
Ring
6. Check that the new pod has the correct number of ports for the injection
valve being serviced.
7. Align the slots in the new pod with the runner in the valve holder in the
TC (see Figure 9-78). Valve pods are keyed to fit only one way (one slot
is narrower than the other). Verify that the slots are aligned with their
matching runners.
418
9 TC Service
8. Also verify that the two splines on the pod align with the matching splines
inside the valve holder (see Figure 9-78). If necessary, twist the end of the
pod to adjust the position of the splines.
Valve Pod
Valve Holder
Slot (larger)
Runner (larger)
Splines
9.
Push the pod into the holder until it clicks into place. Replace the black
locking ring.
9.33
419
3. The fuse cartridge is located next to the main power switch (see
Figure 9-79). Use a small screwdriver to remove the fuse cartridge.
Fuse Cartridge
4. Replace the two fuses with new 2 A IEC 60127-2 time lag fuses
(P/N 954776). Thermo Fisher Scientific recommends always replacing
both fuses.
5. Reinstall the fuse cartridge.
6. Reconnect the main power cord and turn on the power.
420
A Specifications
ICS-5000+
DP/SP
DP/SP Specifications
Dionex ICS-5000+ Single Pump/Dual Pump Specifications
Type
Construction
Pressure Range
<0.1%
Pressure Ripple
Pressure
None required
Vacuum Degasser
Gradient Formation
RFIC-EG Gradients
Analytical: 0.1100 mM
Capillary: 0.1200 mM
Gradient Profiles
421
0.5% at 2 mL/min
Gradient Mixing
(Analytical only)
Eluent Generation
Electrically-actuated, standard
Leak Sensor
Optical, standard
System Software
422
Software
Automated Procedure
Wizards
Standard feature
Standard feature
Standard feature
Application Templates
Standard feature
Automation Support of
Third-Party Instruments
Customizable System
Control Panels
Standard feature
Signal Channels
Pump pressure
Standard feature
Standard feature
System Trigger
Commands and
Conditionals
Standard feature
Standard feature
A Specifications
Standard feature
System Calibration
Storage
Customized Reporting
GLP Compliance
Electrical
Main Power
Requirements
Fuse Requirements
Physical
Dimensions
(h w d)
Weight
Flow Path
Environmental
Operating Temperature
440 C (40104 F)
Operating Humidity
423
424
ICS-5000+
EG
EG Specifications
Dionex ICS-5000+ Eluent Generator Specifications
Minimum and Maximum
Eluent Concentrations
Analytical: 0.1100 mM
Capillary: 0.1200 mM
Flow Rates
Eluent Types
(Standard-Pressure
Analytical)
Eluent Types
(High-Pressure
Analytical)
KOH
MSA
Eluent Types
(Capillary)
KOH
MSA
Maximum Operating
Pressure
Maximum Solvent
Concentration (Analytical
and Capillary)
Cations: None
Anions: 25% methanol
Gradient Profiles
Number of Cartridges
Supported
System Software
Software
Automated Procedure
Wizards
Standard feature
425
Standard feature
Standard feature
Application Templates
Standard feature
Automation Support of
Third-Party Instruments
Customizable System
Control Panels
Standard feature
Signal Channels
Eluent concentration
Standard feature
Standard feature
System Trigger
Commands and
Conditionals
Standard feature
Standard feature
Standard feature
Eluent Cartridge
Information Storage
Customized Reporting
GLP Compliance
Electrical
426
Main Power
Requirements
Fuse Requirements
A EG Specifications
Weight
Flow Path
Environmental
Operating Temperature
440 C (40104 F)
Operating Humidity
Flow Rates
1.002.00 mL/min
Continuous Operation
with 4 L of Eluent
Standard feature
System Wellness
Maximum Operating
Pressure
Operating Temperature
Range
440 C (40104 F)
427
428
ICS-5000+
DC
DC Specifications
Dionex ICS-5000+ Detector/Chromatography Compartment
Specifications
Dual Temperature Zone
Model: Independent
Temperature Control of
Each Zone
Automation Manager
(Optional, Analytical
only)
429
Flow Path
Detectors
Leak Detection
Application Control
Automation
Suppression
430
Nonsuppressed
Conductivity
Supported
Chemical Suppression
Displacement Chemical
Suppression
A DC Specifications
Electrolytic Suppression,
Self-Regenerating,
External Water Mode
Salt Converter
Dionex AMMS-ICE
Suppression Capacities
(Dionex Suppressors)
431
System Software
432
Software
Automated Procedure
Wizards
Standard feature
Standard feature
Standard feature
Application Templates
Standard feature
Automation Support of
Third-Party Instruments
Customizable System
Control Panels
Standard feature
Signal Channels
Standard feature
Standard feature
A DC Specifications
Standard feature
Standard feature
Standard feature
System Calibration
Storage
Customized Reporting
GLP Compliance
Electrical
Main Power
Requirements
Fuse Requirements
Physical Specifications
Dimensions
(h w d)
Weight
38 kg (84 lb)
Flow Path
Environmental
Operating Temperature
440 C (40104 F)
Operating Humidity
433
Cell Drive
Linearity
1%
Resolution
0.00238 nS/cm
Output Range
Noise, Wet
Filter
Sampling Rate
Cell Temperature
Cell Temperature
Stability
<0.001 C
Cell Temperature
Compensation
Analytical: 0.7 L
Capillary: 0.02 L
Cell Electrodes
Cell Body
Heat Exchanger
System Software
434
Software
Automated Procedure
Wizards
Standard feature
A DC Specifications
Standard feature
Standard feature
Application Templates
Standard feature
Automation Support of
Third-Party Instruments
Customizable System
Control Panels
Standard feature
Signal Channels
Data Trending
Standard feature
Standard feature
System Trigger
Commands and
Conditionals
Standard feature
Standard feature
Standard feature
System Calibration
Storage
Customized Reporting
GLP Compliance
Physical
Dimensions
(h w d)
Weight
435
Potential Range
Filter
Control Mode
Cell Body
Working Electrodes
Reference Electrode
Autoranging
Yes
Analog Output
<0.2 L
System Software
Software
436
A DC Specifications
3-D Amperometry
(Chromeleon 6.8 only)
Automated Procedure
Wizards
Standard feature
Standard feature
Standard feature
Application Templates
Standard feature
Automation Support of
Third-Party Instruments
Customizable System
Control Panels
Standard feature
Signal Channels
Standard feature
Standard feature
437
Standard feature
Standard feature
Standard feature
System Calibration
Storage
Customized Reporting
GLP Compliance
Physical
438
Dimensions
(h x w x d)
Weight
ICS-5000+
TC
TC Specifications
Dionex ICS-5000+ Thermal Compartment Specifications
Temperature Range
Temperature
Performance
Accuracy: 0.5 C
Stability: 0.1 C
Precision: 0.1 C
Heat-up/Cool-down Time
Typically 15 min
2050 C and 5020 C
High-Pressure Valve
Types
Column Capacity
Maximum Column
Length
Precolumn Heat
Exchangers
Leak Detection
Control
Computer Connection
USB
Electrical
Main Power
Requirements
Fuse Requirements
Physical
Dimensions
(h w d)
439
Environmental
440
Operating Temperature
1035 C (5095 F)
Operating Humidity
B Reordering Information
ICS-5000+
DP/SP
Item
074444 (capillary)
075044 (analytical)
044541 (capillary)
045722 (analytical)
044540 (capillary)
045721 (analytical)
075493 (capillary)
075768 (analytical)
074371 (capillary)
074370 (analytical)
Backup ring
040695
074446 (capillary)
075767 (analytical)
068628 (capillary)
063382 (analytical)
068627 (capillary)
062092 (analytical)
068646 (capillary)
079857 (analytical)
Piston
063968
063382
441
Part Number
Item
063268
064079
063518
EO without reservoirs
072057
072058
063291
062510
063292
AAA-074423
064792
074422
Regulator
045987
Filter, end-line
044105
Miscellaneous
442
049135
074373
074449
062511
052230
042772
Plug
079803
Syringe, 10 cc
B Reordering Information
Part Number
Item
954773
063246
005.9001A
Maintenance Kits
075970
075039
443
444
ICS-5000+
EG
EG Reordering Information
Part Number
Item
072077
072078
CR-ATC (Capillary)
072079
CR-CTC (Capillary)
074532
074534
074535
074533
075550
CR-ATC 500
075551
CR-CTC 500
080135
079943
063443
075779
075550
CR-ATC 500
075551
CR-CTC 500
0.062 mm (0.0025 in) ID PEEK, 61 cm (24 in); Dionex CRTC ELUENT OUT to EG Degas ELUENT IN
072204
0.062 mm (0.0025 in) ID PEEK, 18 cm (7 in); Dionex CRTC ELUENT IN to Dionex EGC OUT
Backpressure Coils
AAA-053762
445
Part Number
Item
AAA-053763
053764
053765
Miscellaneous
446
AAA-074459
072133
075522
954773
063246
074373
074449
046985
Mini-screwdriver
ICS-5000+
DC
DC Reordering Information
Part Number
Item
075917
075918
061971
079848
042949
Sample loop, 10 L
042857
Sample loop, 25 L
044105
024305
016388
074698
075973
079054
072186
AAA-074459
072052
072053
072055
072054
072056
447
Part Number
Item
056116
056118
064555
064556
064557
045460
045877
045878
448
072042
072044
ED cell
061879
014067
072162
072075
072214
079850
079851
079854
B DC Reordering Information
Part Number
Item
079856
045972
063722
060082
060139
066480
064440
063003
069336
060141
069339
072117
062158
036313
Polishing kit
036319
036318
036321
Polishing pads
Automation Manager
075960
Dionex ICS-5000+ Automation Manager, two 10-port highpressure valves, two low-pressure 3-way valves
449
Part Number
Item
075951
Dionex ICS-5000+ Automation Manager, one 10-port highpressure valve, one low-pressure 3-way valve
075952
Dionex ICS-5000+ Automation Manager, one 6-port highpressure valve, one low-pressure 3-way valve
075953
079833
079849
062561
062562
Analog Output/Relay/TTL
062201
I/O option
923686
043598
Miscellaneous
954772
960777
062437
Leak sensor
074373
074449
044105
Maintenance Kits
450
075040
075974
079053
ICS-5000+
TC
TC Reordering Information
Part Number
Item
079054
075917
075918
042857
Sample loop, 25 L
Consumables
6710.1505
064786
064548
064650
Miscellaneous
954776
063246
6000.1004
064792
Maintenance Kits
075040
075974
079053
451
452
Index
Symbols
% Offset (analog out), 89
+5V output (DC), 86, 90
Numerics
10-port valve
AM, 99
DC, 68 70
TC, 127
See also High-pressure valves
2D data
Integrated amperometry, 111, 113
Pulsed amperometry, 113
3D amperometry data, 115 117
3D plot description, 116 117
Chromatogram, 115
Definition, 114
Displayed in Chromeleon, 114
Isoamperometric plot description, 116
I-t plot, 115
3-way low-pressure valve
See Low-pressure valves
4-port valve, 69
6-port valve
DC, 68, 99
TC, 126, 128
See also High-pressure valves
See also Injection valves
A
AAES, 74
AC sockets (DC), 84
ACES 300 (Capillary), 61, 74
Acetonitrile, 80
Ag/AgCl half-cell, 80
Index-1
Mark, 89
Offset level, 89
Polarity, 89
Range, 88
Recorder calibration, 89
Selecting settings, 88
Analog pressure output, 33
Directing output to different pump, 34
Analog-to-digital converter, 88
Analytical IC applications
Conductivity detector for, 72
CR-TC trap column for, 45
Eluent generator cartridges for, 44
Suppressors for, 74
System configurations, 135
Annual maintenance
DC, 197, 204, 292, 450
DP, 196, 200, 443
EG, 202
SP, 196, 200, 443
TC, 197, 206, 292, 451
Application Wizard, 180
Application Wizard (Chromeleon 6.8), 178,
180
Creating a new sequence, 180
Applications, 135 146
AS-AP Autosampler, 3, 8
Instrument method example, 185
Program example, 185
Vials, filling and loading, 154
Well plates, filling and loading, 154
AS-DV Autosampler, 3
Instrument method example, 185
Program example, 185
Vials, filling and loading, 155
ASRS 300, 74
Atlas Electrolytic Suppressor (AES), 65
Gas separator waste tube, 75
Audit trail, 22, 39
Error messages, 207
Icons, 207
Automation Manager (AM), 3, 97
Description, 7, 97
Index-2
High-pressure valves, 99
Low-pressure valves, 100
Ordering, 449
RCH-1 Reaction Coil Heater, 104
Autorecycle mode, 76 77
Autosampler
Chromeleon control, 182
Controlling with relays/TTLs, 90
Filling vials or well plates, 152, 154
155
Injecting samples, 182
Loading the tray, 152, 154
Sample loading, 182
Autozero, 171
B
Background conductivity
High, 230
Offsetting, 171
Backpressure coil (CD)
Reordering, 448
Requirements, 390
Backpressure coil (EG), 46, 50
Installation, 361
Reordering, 445
Backpressure, excessive
Causes of, 228
Problems caused by, 5, 147
Backpressure, low
Causes of, 227 228
How to increase, 46, 147, 219
Problems caused by, 219
Baseline
Noisy or drifting, 219
Oscillations, 390
Shift, 108
Spikes, 221
Stability, 72
Bottles
See Reservoirs, eluent
Index
Bromate
Post-column reagent addition, 145
Bubbles
Removing from the cell, 390
Bulkhead connectors (EG), 47
Button descriptions
DC, 55
DP/SP, 21 22
EG, 39 40
TC, 119 120
C
Cables
Power cord, 363, 376 377, 419
Signal cable, 6-pin mini-DIN, 125, 451
USB, 34, 49, 443, 446, 450 451
CAES, 74
Calibration
CD cell, 386 387
pH-Ag/AgCl reference electrode, 401
Recorder (analog) output, 89
Capillary IC applications, 2
Conductivity detector for, 72
CR-ATC trap column for, 45
CR-CTC trap column for, 45
DC components for, 58
Eluent generator cartridges for, 44
Injection valves for, 68
Replacing capillary columns, 380 385
Suppressors for, 74
System configurations, 135
Tube fitting installation, 307
Tubing and fittings (DC), 365
Carbohydrate analysis, 146
Carbonate mixer, 46
Carbonate/bicarbonate eluent, 44, 46, 168
CCES 300 (Capillary), 61, 74
CD cell disconnected error, 263
CD cell over safe temperature, 264
CE mark, 19
cETLus mark, 19
Index-3
Index-4
Index
D
Daily maintenance
DC, 203
DP/SP, 199
EG, 201
TC, 205
Data
Displaying 3D amperometry data, 114
Reprocessing amperometry data, 113
Data collection rate
Cyclic voltammetry, 109
Electrochemical detector, 114
Integrated amperometry, 111
Data compression
Cyclic voltammetry, 109
DC amperometry, 106
Entering the potential, 106
DC Temperature Calibration Kit, 67
Declaration of Conformity, 19
Degassing eluents, 25
Deionized water requirements, 20
Detector
See Conductivity Detector (CD)
See Electrochemical Detector (ED)
Detector output
Low, 228
Detector/Chromatography Module (DC), 3, 6
Alarm LED is lighted, 55
Index-5
E
EC cell
See Amperometry cell
ED cell
See Amperometry cell
ED cell disconnected error, 265 268
EGC
See Eluent generator cartridges
Electrochemical detection
DC amperometry, 106
Integrated amperometry, 106
Pulsed amperometry, 106
Electrochemical Detector (ED), 3, 7, 78, 436
3D data, 115 117
Amperometric cell description, 78
Data storage, 113
Description, 64, 78
Detection modes, 78, 105
Palladium hydrogen (PdH) reference
electrode, 82
pH-Ag/AgCl reference electrode, 80
Reordering information, 448
Replacement procedure, 411
Shutdown procedure, 191
Working electrodes, 78
See also Amperometry cell
Electrodes, 79
Reference, 78
Working, 78
Index-6
Electrolysis gases
Purging from eluent, 46, 62, 147
Venting from system, 49
Eluent concentration, 165 167
Eluent generation
Electrolysis gases, 46, 62
Eluent Generator (EG), 3 4
Alarm LED is lighted, 257, 260
Analytical IC system, 42 43
Backpressure, 46
Backpressure coil, 219
Capillary IC system, 41
Component description, 40, 43, 45 46
Degas cartridge (for IC Cube), 62
Electrical connections (for consumables),
47
Eluent concentration ranges, 165 167
Eluent generator cartridges, 5
Fuse cartridge, 49
Fuses, 49
Gas vent line, 49
Leak sensor, 47, 256
Liquid flow path, 50 53
Liquid leaks, 257 259
Main power switch, 49
Maintenance, 201
Operating precautions, 147
Power LED does not light, 258
Pump pressure limits, 260
Rear panel description, 48 49
Selecting the eluent concentration, 165
Shutdown procedures, 189
Spare parts, 445
Specifications, 425
Status bar buttons and LEDs, 39
System configuration, 135
USB connections, 48
Waste lines, 49 50
See also Error messages (EG)
Eluent generator cartridges, 5, 43
Backpressure requirement, 46, 147 148,
259 260
Conditioning procedure, 190
Index
Electrical connections, 47
Frit, outlet, 228, 338
Leaks, 228, 257, 259
Replacement procedure, 338 354
Selecting the eluent concentration, 165
Start-up procedures, 190
Storage, long-term, 190
Storage, short-term, 189
Eluent Organizer (EO), 3, 6, 35
Eluent proportioning valves, 25
Eluent reservoirs
See Reservoirs, eluent
Eluent, filtering, 37
Eluents
Aqueous, 200
Degassing, 25
Filtering, 159
Flushing lines after eluent change, 222
Monitoring pH, 80
Outgassing, 390
End-line filter
See Filter, end-line
EO Regulator Kit, 36
ePanel Set, 10, 155
Displaying, 175
Home panel, 11
EPM 300 Electrolytic pH Modifier, 43 44,
46 47, 361
Function, 44, 46
Troubleshooting, 257
Equilibration, system, 170, 174
Error messages
Audit trail description, 207
DC summary, 211
DP/SP summary, 208
EG summary, 209
TC summary, 213
Error messages (DC), 263 273
CD cell disconnected, 263
CD cell over safe temperature, 264
Column open circuit, 264
Column over safe temperature, 264, 270
Compartment open circuit, 265
Index-7
Index-8
Index
F
Filter, end-line
Bacterial contamination, 200
Installation
Maintenance, 199
Filter, inline, 37
Fittings (DC)
Replacing, 365
Requirements, 365
Fittings (DP/SP)
Replacing, 309
Requirements, 309
Fittings (EG)
Replacing, 335
Requirements, 335
Fittings (TC)
Replacing, 413
Requirements, 413
Flow restrictions, 200
Flow schematics
Conductivity detection (suppression
recycle mode), 76 77
High-pressure valves (AM), 99
IC Cube (for conductivity detection), 62
IC Cube (for electrochemical detection),
63
Injection valve (DC) (10-port valve), 71
Injection valve (DC) (4-port valve), 69
Injection valve (DC) (6-port valve), 70
Injection valve (TC) (10-port valve), 127
Injection valve (TC) (6-port valve), 126
Low-pressure valves (AM), 100
System configurations, 135 146
G
Gas leak in TC, 119, 130, 289
Gas sensor (TC), 130, 289
Adjusting sensor sensitivity, 130
Alarm troubleshooting, 130
Gas separator waste tube, 75
Installation, 148
Reordering, 448
Gas vent line
EG, 49
RFIC+ Eluent Degasser, 49
Glassy carbon electrodes, 79
GM-4 Static Mixer, 27, 223, 442
Gold electrodes, 79
Gradient proportioning valves, 25
H
Half-cells, 80
Heater
Conductivity cell, 72
Index-9
I
I/O option (DC), 85 86, 450
+5V output, 86
Analog outputs, 86
Connections, 87
Power output, 90
Relay outputs, 86
TTL inputs and outputs, 86
IC Cube, 59
Cartridge replacement procedure, 379
Column cartridge, 61
Column heater, 61
CRD bypass cartridge, 60
Index-10
CRD cartridge, 60
EG degas cartridge, 62
Flow schematic (for conductivity
detection), 62
Flow schematic (for electrochemical
detection), 63
Suppressor bypass cartridge, 60 61
Suppressor cartridge, 60 61
Tubing and fittings, 366
ICS-5000+ Automation Manager (AM)
See Automation Manager (AM)
ICS-5000+ Conductivity Detector (CD)
See Conductivity Detector (CD)
ICS-5000+ Detector/Chromatography Module
See Detector/Chromatography Module
(DC)
ICS-5000+ Dual Pump (DP)
See Dual Pump (DP)
ICS-5000+ Electrochemical Detector (ED)
See Electrochemical Detector (ED)
ICS-5000+ Eluent Generator (EG)
See Eluent Generator (EG)
ICS-5000+ Eluent Organizer (EO)
See Eluent Organizer (EO)
ICS-5000+ IC System
CE mark, 19
cETLus mark, 19
Declaration of Conformity, 19
Overview, 1, 3, 10
Software control, 7, 10
User manuals, 13 15
Warranty, 307
ICS-5000+ Single Pump (SP)
See Single Pump (SP)
ICS-5000+ Thermal Compartment (TC)
See Thermal Compartment (TC)
Inject command, 184
Injecting samples
Example commands, 184
Injection ports
Loading with a syringe, 183
Injection valve (TC) (10-port valve), 127
Index
L
Leak sensor (EG), 47, 256
Leak sensors (DC)
Lower leak sensor wet alarm, 271
Replacement, 370
Upper leak sensor wet alarm, 273
Leak sensors (TC)
Gas, 130, 289
Humidity, 130, 289
Leaks
Conductivity cell, 274
DC, 274
EG, 47, 256
Gas, 119, 130, 289, 303
Humidity, 119, 130, 289, 303
Injection valve (DC), 274
Injection valve (TC), 304
Reference electrode, 278
Suppressor, 274
Temperature stabilizer (TC), 304
LED descriptions (DC), 55 56, 119
LED descriptions (DP/SP), 21 22
LED descriptions (EG), 39 40
LED descriptions (TC), 119 120
Lithium hydroxide eluent, 44
Load command, 184
Loading samples, 182
Instrument method example, 184
Program example, 184
With a syringe, 183
With a vacuum syringe, 183
With an autosampler, 182
Loading the autosampler tray, 152
Low detector output, 228
Low pressure limit
Selecting, 164
Index-11
M
Main power receptacle
DC, 84
DP/SP, 31
EG, 49
TC, 123
Main power switch
DC, 84
DP/SP, 31
EG, 49
TC, 123
Maintenance, annual
DC, 204
DP, 200
EG, 202
SP, 200
TC, 206
Maintenance, daily
DC, 203, 205
DP/SP, 199
EG, 201
TC, 205
Maintenance, periodic
DP/SP, 200
TC, 205
Maintenance, weekly
DC, 203
DP/SP, 199
EG, 201
Index-12
TC, 205
Manuals for ICS-5000+ system, 13 15
Mark (analog output), 89
Matrix elimination, 64, 97
System configuration, 143 144
Methanesulfonic acid eluent, 44
Methanol, 80
Methods
See Instrument methods (Chromeleon 7)
Microbore IC applications, 2
MicroMembrane Suppressor (MMS), 65, 74
See also Suppressor
Mixer, static, 27
Mobile phases
See Eluents
Moduleware, 207
MSQ Plus Mass Spectrometer, 3, 10
N
Nitrite in samples, 153
Noisy baseline, 219
Normal edge TTL input control (DC), 96
Normal pulse TTL input control (DC), 96
O
Offset percentage (analog out), 89
Offsetting background conductivity, 171
Open circuit, 271
Operating temperature
DP/SP, 423
Operation, 176
Analyzing samples, 176
Creating a sequence (Chromeleon 6.8),
178
Creating a sequence (Chromeleon 7), 177
Direct control of modules, 175
Filling vials, 152, 154
Filling well plates, 152
Instrument method example, 184
Loading samples, 182
Index
P
PAD
See Pulsed amperometry
Palladium hydrogen (PdH) reference
electrode, 82
Replacement procedure, 407
Panel tabset, 11
Displaying, 175
Home panel, 11, 155, 157
How to display, 163, 169, 173, 259 260
Peak height
Reproducibility, 72
Peaks
Fronting, 122
Reversed, 89
Tailing, 122, 226
Periodic maintenance
DC, 203
DP/SP, 200
TC, 205
pH gradient, 80
pH half-cell, 80
pH limits, 151
pH modifier, 46
pH reading
Adjusting potentials for, 81
Always 7.0, 275
Cannot be set to 7.0, 276
Effect on potentials, 80
Monitoring, 81
Nonexistent, 277
pH-Ag/AgCl reference electrode, 78, 80
Long-term storage, 191
O-ring replacement procedure, 406
Replacement procedure, 399
See also Reference electrode
Photodiode Array Detector, 3, 9
Regulator Bracket Kit, 36
Piston seal wash solution, 26, 187
Piston seal wash system, 26, 160
Activating, 162
Dual pump seal wash option, 27, 160, 442
Replumbing the DP connections, 160
Setup, 162
Piston seals
Replacement procedure, 319
Pistons
Replacement procedure, 326
Platinum working electrodes, 79
Plot, I-t, 115
Plumbing
Replacing DC tubing and fittings, 365
Replacing DP/SP tubing and fittings, 309
Replacing EG tubing and fittings, 335
Replacing TC tubing and fittings, 413
Plumbing configuration drawings, 135 146
Polarity
Analog output, 89
Polishing kit (ED), 396
Polishing procedure, 396
Reordering, 449
Post-column reagent addition, 64, 97, 145
Potassium carbonate eluent, 44, 46
Potassium hydroxide eluent, 44
Potential shifting, 80, 278
Power cord, 363, 376 377, 419
Power LED (DC), 56
Power LED (DP/SP), 22
Power LED (EG), 40
Power LED (TC), 120
Power output (DC)
Index-13
Index-14
Q
Quantification methods (Chromeleon 6.8),
180
R
Raw data, 114
RCH-1 Reaction Coil Heater, 104
Controlling, 104
Installed in AM, 97
Open circuit error, 271
Over safe temperature, 272
Reordering, 450
Reagent-Free IC (RFIC), 1
System configurations, 135 146
Rear panel (DC), 85
AC sockets, 84
Analog outputs, 85
Description, 83
Fuses, 84
I/O option, 85, 450
Power switch, 84
TTL and relay connectors, 85
USB connections, 84
Rear panel (DP/SP)
Analog pressure output, 33
Digital I/O port, 32
Fuses, 32
Power receptacle, 32
Power switch, 31
USB connections, 34
Waste lines, 34
Rear panel (EG), 48
Exhaust fan, 48
Index
Fuse cartridge, 49
Gas vent line, 49 50
Power switch, 49
USB connections, 48
Waste lines, 49 50
Rear panel (TC)
Description, 123
Digital I/O connectors, 124
Fuses, 123
Power switch, 123
USB connections, 125
Waste line, 125
Rear-seal wash
See Piston seal wash system
Recorder
Analog output setting, 89
Calibrating, 89
Recycle mode, 76
Redox reactions, 80
Reference electrode, 78
Contaminated, 276
Faulty, 278
Leaking, 278
Preventing from drying out, 81
Reordering information, 448
Shutdown procedure, 191
Reference Library DVD, 13
Reference potential shift, 81, 278
Regulator Bracket Kit, TC/VWD/PDA, 36
Regulator Kit, EO, 36
Relay connectors (DC), 85 87
Configuring, 90
Relay outputs (DC), 85
Controlling, 92
Reordering information
DC, 447
DP/SP, 441
EG, 445
TC, 451
Reprocessing amperometry data, 113
Reproducibility
Affected by amperometry cell pH, 81
Affected by temperature changes, 73
S
Safety icons, 36
Safety messages, 15, 36
Salt crystals, preventing, 201
Sample analysis overview, 176
Sample loading
With a syringe, 183
With an autosampler, 182
Sample loop (DC)
Injecting, 69 70, 72
Loading, 71, 182 183
Reordering, 447
Sample loop (TC)
Injecting, 127
Injection valve connections, 128
Loading, 126 127
Reordering, 451
Sample processing, 176
Sample tray
Loading, 152, 154
Index-15
Samples
Collecting and storing, 152
Diluting, 153
Filtering, 153
Loading, 182 184
Pretreating, 153
See also High-pressure valves
See also Injection valves
Self-Regenerating Suppressor (SRS), 50, 65
Gas separator waste tube, 75
Hydrating, 189 190
Start-up procedure, 189 190
See also Suppressor
Sensor, gas (TC), 119, 130, 289
Sensor, humidity (TC), 119, 130, 289
Sequence Wizard (Chromeleon 6.8), 178
Creating a new sequence, 179
Sequence Wizard (Chromeleon 7), 177
Creating a new sequence, 178
Service procedures (DC)
Amperometry cell gasket replacement,
393
Capillary column replacement, 380 385
CD cell air removal, 390
CD cell calibration, 386
Conductivity detector replacement, 389
Electrochemical detector replacement,
411
Fuse replacement, 377
IC Cube cartridge replacement, 379
Injection valve pod replacement, 373
Injection valve rebuilding, 372, 416
Leak sensor replacement, 370
PdH reference electrode replacement, 407
pH-Ag/AgCl reference electrode O-ring
replacement, 406
pH-Ag/AgCl reference electrode
replacement, 399
Suppressor replacement, 387
Tubing and fitting replacement, 365
Working electrode polishing, 396
Service procedures (DP/SP)
Check valve cartridge replacement, 315
Index-16
Index
Index-17
136
Hybrid RFIC-EG dual CD analytical and
CD capillary system, 138
Matrix elimination, 143 144
System Wellness, 133
T
TC/VWD/PDA Regulator Bracket Kit, 36
Technical Support for Dionex products, 307
Temperature calibration (DC), 67
Temperature control (CD), 72
Minimizing the effect of variations, 73
Temperature compensation, 73
Temperature control (DC), 66
Cell heater, 73
Temperature control (TC), 122, 131
Temperature stabilizer (TC), 8, 122
Liquid leaks, 304
Operating problem, 305
Thermal Compartment (TC), 3, 8
See also Error messages (TC)
Alarm LED is lighted, 119
Column ID system, 129
Digital I/O connectors, 124
Front description, 119 120
Maintenance, 205 206
Moduleware update, 282
Oven LED is flashing, 120
Oven LED is lighted, 120
Predictive Performance functions, 133
Rebuilding the injection valve, 416
Regulator Bracket Kit, 36
Replacing the injection valve pod, 417
Service procedures, 413
Shutdown procedure, 193
Signal cable, 125, 451
Specifications, 439
Theory of operation, 131
Trap column, 5
Trap column, high-pressure, 27
Index-18
Tray, autosampler
Loading, 152, 154
Triangular waveform, 110
Troubleshooting (DC)
Amperometry cell, 275
Error messages (DC), 263
Liquid leaks (DC), 274
pH readout always at 7.0, 275
pH readout cannot be set to 7.0, 276
pH readout nonexistent, 277
Reference electrode leaks, 278
Reference potential shifts, 278
VALVE button not working, 275
Troubleshooting (DP/SP)
Chromatographic reproducibility, 222
Digital I/O port not operating, 243
Leak alarm, 241
Liquid leaks, 241
Pump does not start, 239
Pump stops unexpectedly, 240
Vacuum degas module low vacuum, 242
Troubleshooting (EG)
Alarm LED is lighted, 257
EG stops operation, 260
Leaking fittings, 257
Liquid leaks, 258
No flow, 259
Power LED does not light, 258
Troubleshooting (system-wide), 207
High background, 229
Low detector output, 228
Noisy baseline, 219
Retention times too early, 224
Retention times too late, 224
Tailing peaks, 226
Troubleshooting (TC)
Alarm LED is lighted, 303
Liquid leaks, 304
Temperature does not increase, 305
Temperature stabilizer not operating, 305
TTL and relay connectors (DC), 85 86
Installation instructions, 87
Index
U
Upper compartment (DC)
Description, 64
Upper oven LED, 55
USB cables
DC, 84
DP/SP, 34
EG, 49
Reordering (DC), 450
Reordering (DP/SP), 443
Reordering (EG), 446
Reordering (TC), 451
TC, 125
USB communication error
Troubleshooting, 261, 283 284, 287,
292, 296
USB connections
DC, 84
DP/SP, 34
EG, 261
TC, 125
V
Vacuum degassing module, 25
Daily maintenance, 199
On/off control, 26
Vacuum is low, 242
VALVE buttons (DC), 56
Enabling/disabling, 56
Troubleshooting, 275
Valve LEDs (DC)
LED is flashing, 56
LED is lighted, 56
Valve LEDs (TC)
LED is flashing, 119, 303
LED is lighted, 119
Valves
See High-pressure valves
See Injection valves
See Low-pressure valves
Variable Wavelength Detector, 3, 9
Regulator Bracket Kit, 36
Vials, 152
Filling, 152, 154
Virtual Column Separation Simulator, 176,
180
Voltammetry, 109
See also Cyclic voltammetry
VP Vacuum Pump, 146
W
Waste container (EG)
Preventing gas buildup, 148
Waste disposal, 205
Waste lines (CD)
Gas separator waste tube, 75
Waste lines (DC), 85
Blocked, 274
Waste lines (DP/SP), 34
Waste lines (EG), 49 50
Blocked or incorrectly installed, 257, 259
Waste lines (TC)
Blocked, 304
Index-19
Z
Zero position (analog out), 89
Index-20