Thermo Scientific Dionex ICS Series User manual

Dionex ICS Series VWD Variable Wavelength
Detector Operator’s Manual
Document No. 065377
Revision 01
January 2012

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The contents of this document are subject to change without notice. All technical
information in this document is for reference purposes only. System configurations and
specifications in this document supersede all previous information received by the
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accurate, or error-free and assumes no responsibility and will not be liable for any errors,
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information in the document is followed properly.
Revision history: Revision 01 released January 2012
For Research Use Only. Not for use in diagnostic procedures.

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Contents
1 • Introduction
1.1 Detector Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.2 Principles of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.3 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.4.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.4.2 Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.4.3 Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2•Description
2.1 Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
2.2 Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.2.1 Tubing Slots and Tubing Chase . . . . . . . . . . . . . . . . . . . . . . . . 11
2.2.2 Leak Sensor and Leak Drain . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.2.3 Flow Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.2.4 Lamps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.3 Optical System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.4 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.4.1 Main Power Switch, Fuse Cartridge, and Power Receptacle . . 16
2.4.2 Digital I/O Ports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.4.3 USB Connector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

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2.4.4 Analog Outputs (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . .17
2.4.5 Tubing Chase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .18
2.4.6 Drain Port and Drain Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
2.5 Operating Guidelines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
2.5.1 Wavelength Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
2.5.2 Mobile Phases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
2.5.3 Mobile Phase Delivery System . . . . . . . . . . . . . . . . . . . . . . . . .20
2.6 Chromatography Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .21
2.6.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .21
2.6.2 System Wellness and Predictive Performance . . . . . . . . . . . . .23
3 • Operation and Maintenance
3.1 Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25
3.1.1 Initial Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25
3.1.2 Connect to the Chromeleon 7 Client . . . . . . . . . . . . . . . . . . . . .26
3.1.3 Connect to the Chromeleon 6.8 Client . . . . . . . . . . . . . . . . . . .27
3.1.4 Turn On the Lamps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29
3.2 System Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .29
3.3 Direct Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .30
3.4 Automated Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
3.5 Optimizing Detector Performance . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
3.5.1 Time Constant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
3.5.2 Data Collection Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
3.5.3 Step (Chromeleon 6.8 only) . . . . . . . . . . . . . . . . . . . . . . . . . . .36

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3.5.4 Average (Chromeleon 6.8 only) . . . . . . . . . . . . . . . . . . . . . . . . 37
3.5.5 Sample Wavelength Selection . . . . . . . . . . . . . . . . . . . . . . . . . 37
3.6 Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
3.6.1 Short-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
3.6.2 Long-term Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
3.7 Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
3.7.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
3.7.2 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
4 • Troubleshooting
4.1 Audit Trail Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
4.2 ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
4.3 No Detector Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
4.4 Lamp Does Not Light . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
4.5 Noisy Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
4.6 Drifting Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
4.7 Peak Broadening . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
4.8 Poor Reproducibility . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
4.9 Faulty USB Communication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
5•Service
5.1 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
5.2 Wavelength Calibration and Verification . . . . . . . . . . . . . . . . . . . . . . . 64
5.3 Replacing a Deuterium Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

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5.4 Replacing a Tungsten Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .69
5.5 Cleaning the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .71
5.6 Replacing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .72
5.6.1 Remove the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .72
5.6.2 Install the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73
5.6.3 Perform Wavelength Verification . . . . . . . . . . . . . . . . . . . . . . .73
5.7 Replacing the Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .74
A • Specifications
A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
A.2 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
A.3 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .75
A.4 Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .76
A.5 Flow Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78
A.5.1 Standard Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78
A.5.2 Semi-Micro Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78
A.6 Digital I/O . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79
A.7 Analog Outputs (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79
B • Installation
B.1 Facilities Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .81
B.2 Positioning the Dionex VWD in the System . . . . . . . . . . . . . . . . . . . . .82
B.3 Unpacking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .82
B.4 Installing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .84

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B.5 Connecting the Drain Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
B.6 Connecting the Digital I/O . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
B.7 Installing the Analog Outputs (Optional) . . . . . . . . . . . . . . . . . . . . . . . 90
B.7.1 Installing the DAC Plug-In Module . . . . . . . . . . . . . . . . . . . . . 91
B.7.2 Connecting the Analog Outputs to the External Device . . . . . 92
B.8 Connecting the Dionex VWD to the Chromeleon PC . . . . . . . . . . . . . . 93
B.8.1 Before You Begin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
B.8.2 Connecting the USB Cable . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
B.9 Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
B.10 Turning On the Dionex VWD Power . . . . . . . . . . . . . . . . . . . . . . . . . . 98
B.11 Setting Up the Chromatography Software . . . . . . . . . . . . . . . . . . . . . . 99
B.11.1 Chromeleon 7: Assigning the Dionex VWD to
an Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
B.11.2 Chromeleon 6.8: Assigning the Dionex VWD to
a Timebase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
B.11.3 Selecting Configuration Properties . . . . . . . . . . . . . . . . . . . . 103
C • Reordering Information
D • UV Absorbances
D.1 UV Cutoff Wavelengths of Common Mobile Phases . . . . . . . . . . . . . 109
D.2 UV Absorbance Wavelengths of Chromophores . . . . . . . . . . . . . . . . 110

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1 • Introduction
1.1 Detector Overview
The Thermo Scientific Dionex™ICS Series Variable Wavelength Detector
(Dionex VWD) is a high-quality instrument designed for IC analysis applications
requiring a UV-Vis detector and for LC analysis applications requiring an inert
(PEEK™) flow path. The Dionex VWD can be used with the following Thermo
Scientific Dionex systems: the ICS-5000 (analytical systems only), ICS-2100,
ICS-1600, ICS-1100, and ICS-900 (as well as some legacy systems). The Dionex
VWD can be used in numerous laboratory environments for routine analysis, as
well as for sophisticated research tasks.
Two versions of the Dionex VWD are available: a single-channel version
(P/N 070220) and a four-channel version (P/N 070221).
•The detector is a dual-beam, variable-wavelength photometer with one
measurement and one internal reference beam. See Section 2.3 for details
about the optical system.
Figure 1-1. Thermo Scientific Dionex ICS Series Variable Wavelength Detector

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•Two light sources, a deuterium lamp for ultraviolet detection and a tungsten
lamp for visible and near-infrared wavelength detection, provide a
wavelength detection range from 190 to 900 nm. For details about the lamps
and wavelength detection ranges, see Section 2.2.4.
•The four-channel detector measures at up to four wavelengths, by indexing
between wavelengths several times per second.
•To suppress higher-order radiation, two optical filters are inserted
(automatically) into the light path (see Section 2.3).
•The wavelength accuracy can be verified via the built-in holmium oxide filter
(see Section 5.2).
•The detector is controlled with a PC (personal PC) running Microsoft®
Windows Vista® or Windows®XP and either the Thermo Scientific Dionex
Chromeleon®7 Chromatography Data System or Chromeleon®6.8
Chromatography Data System. Chromeleon 7 and Chromeleon 6.8 also
provide data acquisition and data processing functions.
NOTE Thermo Scientific Dionex Chromeleon® Xpress software
can provide real-time control and monitoring of the
detector, but does not include data management
capabilities.
•Various monitoring, diagnostic, and calibration features are provided for
system wellness and predictive performance (see Section 2.6.2).

1 • Introduction
Doc. 065377-01 1/12 3
1.2 Principles of Operation
Photometric detection is based upon the absorption of monochromatic light. The
degree of absorption depends on the sample molecule, its concentration, the light's
path length in the sample, and the measurement wavelength.
Absorbance is defined as:
and is related to concentration by the empirical Lambert-Beer's Law:
where:
UV-Vis spectroscopy allows you to detect the chromophores of analyte molecules
directly in the sample or to generate them indirectly by derivatization.
Appendix D provides a list of wavelengths for the absorption maxima of various
chromophores.
IrReference beam intensity
IsSample beam intensity
Iro Reference beam intensity with autozero
Iso Sample beam intensity with autozero

Molar absorptivity coefficient of the analyte (L •mol-1 •cm-1)
cConcentration (mol/L)
lCell path length (cm)
AIr
Is
----


 Iro
Iso
-------



log–log=
Acl=

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1.3 About This Manual
The electronic version (i.e., PDF file) of the Dionex VWD operator’s manual
contains numerous hypertext links that can take you to other locations within the
file. These links include:
•Table of contents entries
•Index entries
•Cross-references (underlined in blue) to sections, figures, tables, etc.
If you are not familiar with how to navigate PDF files, refer to the Help system for
Adobe®Acrobat®or Adobe Reader®for assistance.
Chapter 1
Introduction An overview of the Dionex VWD, including a brief
description of the detector, the principles of operation,
and the chromatography software (Chromeleon) required
for detector operation.
Chapter 2
Description Detailed descriptions of Dionex VWD components and
important operating features.
Chapter 3
Operation Instructions for routine operation of the Dionex VWD.
Includes routine preventive maintenance and shutdown
procedures.
Chapter 4
Troubleshooting Minor problems that may occur during operation of the
Dionex VWD, with step-by-step procedures for how to
isolate and eliminate the cause of each problem. Includes
a list of Chromeleon Audit Trail error messages, with an
explanation of the possible cause of each message and
the corrective action to take.
Chapter 5
Service Step-by-step instructions for routine service and parts
replacement procedures the user can perform for the
Dionex VWD.
Appendix A
Specifications Specifications and installation site requirements for the
Dionex VWD.
Appendix B
Installation Step-by-step instructions for unpacking and installing the
Dionex VWD.

1 • Introduction
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1.4 Safety and Regulatory Information
The Dionex VWD was manufactured by Thermo Fisher Scientific Corporation at
the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A.
The Dionex VWD is designed for use with IC (ion chromatography) and HPLC
(high-performance liquid chromatography) applications and should not be used
for any other purpose. Operation of a Dionex VWD in a manner not specified by
Dionex may result in personal injury.
If there is a question regarding appropriate usage, contact Technical Support for
Dionex products. In the U.S. and Canada, call 1-800-346-6390. Outside the U.S.
and Canada, call the nearest Thermo Fisher Scientific office.
1.4.1 Safety Messages and Notes
This manual contains warnings and precautionary statements that can
prevent personal injury and/or damage to the Dionex VWD when
properly followed. Safety messages appear in bold type and are
accompanied by icons, as shown below.
Appendix C
Reordering
Information
Spare parts for the Dionex VWD.
Appendix D
UV Absorbances UV cutoff wavelengths of common mobile phases and
wavelengths for the absorption maxima of various
chromophores.
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.

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Messages d'avertissement en français
Warnhinweise in Deutsch
Notes
Informational messages also appear throughout this manual. These are
labeled NOTE and are in bold type:
NOTE NOTES call attention to certain information. They alert
you to an unexpected result of an action, suggest how to
optimize instrument performance, etc.
Indicates that the function or process of the instrument may be
impaired. Operation does not constitute a hazard.
Signale une situation de danger immédiat qui, si elle n'est pas évitée,
entraînera des blessures graves à mortelles.
Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures graves à mortelles.
Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures mineures à modérées. Également
utilisé pour signaler une situation ou une pratique qui pourrait
gravement endommager l'instrument mais qui n'entraînera pas de
blessures.
Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder
schwerwiegenden Verletzungen führen.
Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder
schwerwiegenden Verletzungen führen.
Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren
oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn
eine Situation zu schweren Schäden am Gerät führen kann, jedoch
keine Verletzungsgefahr besteht.

1 • Introduction
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1.4.2 Safety Symbols
These symbols appear on the Dionex VWD or on labels affixed to the
Dionex VWD:
1.4.3 Declaration of Conformity
The cTUVus Mark safety label and the CE Mark label on the Dionex
VWD indicate that it is in compliance with the following standards: EN
61010-1:2001 (safety), CAN/CSA-C22.2 No. 1010.1-92 + A2:97
(safety), UL 61010C:2002 R8.02 (safety), and EN 61326:1997, including
A1:1998 and A2:2001 (EMC susceptibility and immunity).
Alternating current
Primary protective conductor terminal
Secondary protective conductor terminal
Power supply is on
Power supply is off
Indicates a potential hazard. Refer to this operator’s
manual for an explanation of the hazard and how to
proceed.

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2 • Description
2.1 Front Features
Figure 2-1 illustrates the features on the front of the Thermo Scientific Dionex
ICS Series Variable Wavelength Detector (Dionex VWD).
•Use the power button in the lower left corner of the detector for routine on/off
control of the Dionex VWD. To turn on the Dionex VWD, press the power
button. To turn off the Dionex VWD, press and hold the power button for
2 seconds.
NOTE The main power switch is on the Dionex VWD rear
panel (see Section 2.4.1).
Figure 2-1. Thermo Scientific Dionex ICS Series Variable Wavelength Detector Front
Features
Front Cover
Status Bar
Power Button

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•The front cover provides access to the interior components of the Dionex
VWD. To remove the cover, grasp the cover by the sides and pull it straight
off.
•The status bar provides LEDs (light emitting diodes) that indicate the status of
several detector functions (see Figure 2-2).
Figure 2-2. Dionex VWD Status Bar
Button/LED Label If the LED is on ...
CONNECTED The Dionex VWD is connected to a Chromeleon 7 instrument or
a Chromeleon 6.8 timebase.
ALARM A problem has occurred (for example, a leak). Check the
Chromeleon Audit Trail for the cause.
DEUTERIUM – UV The deuterium lamp is on.
TUNGSTEN – VIS The tungsten lamp is on.
POWER The Dionex VWD power is on.
CONNECTED ALARM
DEUTERIUM - UV POWERTUNGSTEN - VIS

2 • Description
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2.2 Interior Components
To access the interior components of the Dionex VWD, grasp the front cover by
the sides and pull it straight off.
2.2.1 Tubing Slots and Tubing Chase
The tubing slots route tubing (for example, the flow cell inlet tubing)
from the Dionex VWD interior to outside the detector.
The tubing chase routes tubing (for example, the waste line from the flow
cell outlet) from the interior of the Dionex VWD, through the body of the
module, and to the rear panel (see Figure 2-5).
2.2.2 Leak Sensor and Leak Drain
A leak sensor is installed inside the detector (see Figure 2-3). If the leak
sensor detects a leak, the ALARM LED on the status bar lights, and an
error message appears in the Chromeleon Audit Trail. The drip tray
collects the fluid and the leak drain routes the fluid from the drip tray to
the drain port on the Dionex VWD rear panel (see Figure 2-5). After
Figure 2-3. Dionex VWD Interior View (Front Cover Removed)
2
3
4
5
6
1Tubing Slots
Tubing Chase
2
Leak Sensor
4
5
6
3
Leak Drain
Flow Cell
Lamp Housing Cover
1
1
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fixing the leak and drying the sensor, clear the ALARM LED (see
Section 4.2).
2.2.3 Flow Cells
A flow cell is not included with the Dionex VWD and must be
specifically ordered. Dionex offers two PEEK cells for use with the
Dionex VWD:
•The standard (analytical) flow cell (P/N 066346), with a volume of
11 L, is designed for standard bore applications with 3- to 4-mm ID
separator columns and flow rates of 0.5 to 5.0 mL/min.
•The semi-micro flow cell (P/N 6074.0300), with a volume of 2.5 L,
is designed for microbore applications with 2-mm ID separator
columns and flow rates up to 1.0 mL/min.
The flow cells are optimized for fast separations with no loss in
chromatographic resolution. An identification chip is installed in each cell
at the factory. The chip stores unique information about the cell, including
the cell type and the serial number. When the cell is installed, a contact on
the flow cell's rear panel connects the chip to the detector electronics. The
detector downloads the information to Chromeleon, where it is used for
System Wellness and Predictive Performance functions (see
Section 2.6.2).
The flow cells are equipped with a built-in heat exchanger. The heat
exchanger helps adapt the temperature of the solvent to the flow cell
temperature before the solvent enters the flow cell. The total heat
exchanger volume is 8.8 L for the standard cell and 5 L for the semi-
micro cell.
The detector is shipped with a dummy cell. Before initial operation of the
detector, replace the dummy cell with the flow cell. See Section B.4 for
flow cell installation instructions.
Do not operate either the standard or semi-micro flow cell without
flow for more than 5 minutes while a lamp is on. The heat from the
lamp may damage the PEEK cell.
Do not use the standard or semi-micro flow cell with normal phase or
chlorinated solvents; these solvents will damage the PEEK cell.