Thermo Scientific Dionex ICS Series Manuel utilisateur

Dionex ICS Series Photodiode Array

Detector Operator’s Manual

Document No. 065378

Revision 01

January 2012

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reproduction of the whole or any part of this document is strictly prohibited, except with

the written authorization of Thermo Fisher Scientific Inc.

The contents of this document are subject to change without notice. All technical

information in this document is for reference purposes only. System configurations and

specifications in this document supersede all previous information received by the

purchaser.

Thermo Fisher Scientific Inc. makes no representations that this document is complete,

accurate, or error-free and assumes no responsibility and will not be liable for any errors,

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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.

Doc. 065378-01 1/12 i

1 • Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.1 Detector Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

1.2 Theory of Photodiode Array Detection . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.2.1 Advantages of Photodiode Array Detection . . . . . . . . . . . . . . . . 3

1.3 Operator’s Manual Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

1.4.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

1.4.2 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

1.4.3 Declaration of Conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

2•Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.1 Front Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.2 Inside Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

2.3 Optical System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.3.1 Flow Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

2.4 Electronics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

2.5 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

2.6 Operating Guidelines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

2.6.1 Mobile Phases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

2.6.2 Solvent Delivery System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

Contents

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ii Doc. 065378-01 1/12

2.7 Chromatography Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27

2.7.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .27

2.7.2 3D Data Acquisition License . . . . . . . . . . . . . . . . . . . . . . . . . . .30

2.7.3 System Wellness and Predictive Performance . . . . . . . . . . . . .30

3 • Operation and Maintenance . . . . . . . . . . . . . . . . . . . . . . . .33

3.1 Getting Started . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33

3.1.1 Initial Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33

3.1.2 Connect to the Chromeleon 7 Client . . . . . . . . . . . . . . . . . . . . .34

3.1.3 Connect to the Chromeleon 6.8 Client . . . . . . . . . . . . . . . . . . .35

3.1.4 Turn On the Lamps . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.2 System Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.3 Routine Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38

3.3.1 Direct Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .38

3.3.2 Automated Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41

3.3.3 Stand-Alone Analog Operation . . . . . . . . . . . . . . . . . . . . . . . . .41

3.4 Optimizing Detector Performance . . . . . . . . . . . . . . . . . . . . . . . . . . . . .43

3.5 Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55

3.6 Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .55

4 • Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .59

4.1 Alarms and Error Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .59

4.2 ALARM LED Is Lighted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .73

4.3 Lamp Does Not Light/Lamp LED Is Flashing Rapidly . . . . . . . . . . . . .73

Contents

Doc. 065378-01 1/12 iii

4.4 No Detector Response . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

4.5 Noisy Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

4.6 Drifting Baseline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78

4.7 Deuterium Lamp Intensity Reading Too Low . . . . . . . . . . . . . . . . . . . . 79

4.8 Wavelength Calibration Fails . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

4.9 Wavelength Verification Fails . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

4.10 No Spectra Collected . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

4.11 Low Spectral Resolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

4.12 Peaks Too Large or Small . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

4.13 Poor Peak Shape . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84

4.14 Faulty USB Communication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86

4.14.1 Moduleware Run-Time Diagnostics . . . . . . . . . . . . . . . . . . . . 87

4.14.2 Software Diagnostics and Calibration . . . . . . . . . . . . . . . . . . . 87

5•Service. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

5.1 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

5.2 Cleaning the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

5.3 Removing Trapped Air from the Flow Cell . . . . . . . . . . . . . . . . . . . . . 93

5.4 Removing the Flow Cell from the Optical Bench . . . . . . . . . . . . . . . . . 94

5.5 Replacing the Flow Cell Windows . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95

5.6 Replacing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

5.7 Replacing the Deuterium Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

5.8 Replacing the Tungsten Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

5.9 Replacing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103

Dionex PDA Operator’s Manual

iv Doc. 065378-01 1/12

A • Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105

A.2 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105

A.3 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .105

A.4 Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .106

A.5 Flow Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .107

A.5.1 Standard Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .107

A.5.2 Semi-Micro Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .107

A.5.3 Semi-Preparative Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . .108

A.6 Heat Exchangers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .108

B • Installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .111

B.1 Facilities Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .111

B.2 Unpacking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .112

B.3 Installing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .113

B.4 Connecting the Waste Line . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .116

B.5 Connecting the Analog Outputs (Optional) . . . . . . . . . . . . . . . . . . . . .116

B.6 Connecting the Relays/TTLs (Optional) . . . . . . . . . . . . . . . . . . . . . . .117

B.7 Connecting to the Chromeleon PC . . . . . . . . . . . . . . . . . . . . . . . . . . . .118

B.7.1 Before You Begin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .118

B.7.2 Chromeleon 7: Starting the Instrument Controller Service . . .119

B.7.3 Chromeleon 6.8: Starting the Server . . . . . . . . . . . . . . . . . . . .119

B.7.4 Connecting the USB Cable . . . . . . . . . . . . . . . . . . . . . . . . . . .120

B.8 Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123

Contents

Doc. 065378-01 1/12 v

B.9 Installing the USB Device Drivers . . . . . . . . . . . . . . . . . . . . . . . . . . . 124

B.10 Configuring the Dionex PDA in Chromeleon . . . . . . . . . . . . . . . . . . . 125

B.10.1 Using the USB Auto Configuration Wizard . . . . . . . . . . . . . . 125

B.10.2 Selecting Configuration Properties . . . . . . . . . . . . . . . . . . . . 127

B.11 Starting the Chromeleon Client . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

C • Reordering Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

Dionex PDA Operator’s Manual

vi Doc. 065378-01 1/12

Doc. 065378-01 1/12 1

1 • Introduction

1.1 Detector Overview

The Thermo Scientific Dionex™ICS Series Photodiode Array Detector (Dionex

PDA) (P/N 074114) is an optical chromatography detector capable of measuring

absorbance signals and absorbance spectra from 190 to 800 nm. The Dionex PDA

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 PDA can be used in numerous laboratory

environments for routine analysis, as well as for sophisticated research tasks.

A deuterium lamp optimizes the UV range (190 to 380 nm) and a tungsten lamp

optimizes the visible range (380 to 800 nm). When using the Dionex PDA, up to

five single wavelengths (2D chromatograms) can be collected without the

necessity for collecting 3D data. Collecting individual wavelengths instead of the

spectra offers two advantages: it eliminates the need to perform signal extractions

for analyses that do not require spectral data and it conserves disk space.

Figure 1-1. Thermo Scientific Dionex ICS Series Photodiode Array Detector

Dionex PDA Operator’s Manual

2Doc. 065378-01 1/12

Key features of the Dionex PDA include:

•The deuterium and tungsten lamps ensure low baseline noise, high signal

intensity, and applications flexibility in the wavelength range from 190 to

800 nm.

•The 1024-element photodiode array optimizes spectral resolution.

•The built-in holmium oxide filter verifies wavelength calibration accuracy.

•Five flow cells are available for standard, semi-micro, and semi-preparative

applications.

•LEDs on the front cover provide detector status at a glance.

•Four analog outputs support data collection on alternate data collection

systems.

•The detector is controlled with a PC (personal computer) running Microsoft®

Windows Vista® or Windows®XP and either the Chromeleon®7

Chromatography Data System or the 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.

1.2 Theory of Photodiode Array Detection

Monochromatic variable wavelength detectors monitor eluting components of the

sample at a single wavelength (ideally, the wavelength of maximum absorbance).

Photodiode array detectors scan a range of wavelengths every few milliseconds

and continually generate spectral information. Wavelength, time, and absorbance

can all be plotted.

Photodiode array detectors provide three-dimensional information that allows an

accurate assessment of peak identity, purity, and quantitation in a single analysis.

Software support for photodiode array detectors includes peak purity and spectral

library search functions to help determine peak homogeneity and identity.

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