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  • Dionex ICS-5000+ Ion Chromatography System Operator's Manual

    Document No. 065446 Revision 02

    December 2014

  • © 2014 Thermo Fisher Scientific Inc. All rights reserved.

    AES, AMMS, Atlas, CES, Chromeleon, ERS, IonPac, MicroMembrane, and OnGuard, are registered trademarks of Thermo Fisher Scientific Inc. in the United States. Acrobat, Adobe, and Adobe Reader are registered trademarks of Adobe Systems Incorporated in the United States and other countries. Microsoft and Windows are registered trademarks of Microsoft Corporation in the United States and other countries.

    The following are registered trademarks in the United States and possibly other countries: Kel-F is a registered trademark of 3M Corporation. KIMWIPES is a registered trademark of Kimberly-Clark Corporation. PharMed and Tygon are registered trademarks of Saint-Gobain Performance Plastics. Ultem is a registered trademark of General Electric Company. Ultrajet is a registered trademark of ITW Chemtronics.

    PEEK is a trademark of Victrex PLC. TitanHP is a trademark of Rheodyne LLC.

    All other trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries.

    Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the product operation. This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.

    The contents of this document are subject to change without notice. All technical information in this document 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, omissions, damage, or loss that might result from any use of this document, even if the information in the document is followed properly.

    Revision history: Revision 01 released November 2012; initial release of instrument Revision 02 released December 2014; support for low-temperature Dionex ICS- 5000+ Detector/Chromatography Module (DC)

    Software version: Chromeleon 7.1 SR2 (or later) or Chromeleon 6.8 SR12 (or later) for a system including a standard DC; Chromeleon 7.2 SR2 (or later) for a system including a low-temperature DC

    For Research Use Only. Not for use in diagnostic procedures.

  • Doc. 065446-02 12/14 i

    1 • Introduction

    1.1 Dionex ICS-5000+ System Overview . . . . . . . . . . . . . . . . . . . . . . . . . 1

    1.1.1 Dionex ICS-5000+ System Components . . . . . . . . . . . . . . . . 3

    1.1.2 Dionex ICS-5000+ System Control . . . . . . . . . . . . . . . . . . . 11

    1.2 Dionex ICS-5000+ System Documentation . . . . . . . . . . . . . . . . . . . . 14

    1.3 Dionex ICS-5000+ System Operator’s Manual . . . . . . . . . . . . . . . . . 15

    1.4 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . 16

    1.4.1 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . 17

    1.4.2 Safety Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

    1.4.3 Regulatory Compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

    1.5 Deionized Water Requirements for IC . . . . . . . . . . . . . . . . . . . . . . . . 20

    2 • Description

    DP/SP Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 2.1 DP/SP Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

    2.2 DP/SP Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

    2.2.1 Pump Heads . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

    2.2.2 Pressure Transducer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

    2.2.3 Proportioning Valves (Gradient pump only) . . . . . . . . . . . . 25

    2.2.4 Vacuum Degassing Module . . . . . . . . . . . . . . . . . . . . . . . . . 25

    2.2.5 Piston Seal Wash System . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

    Contents

  • Dionex ICS-5000+ Operator’s Manual

    ii Doc. 065446-02 12/14

    2.2.6 Static Mixer (Analytical IC only) . . . . . . . . . . . . . . . . . . . . . 27

    2.2.7 High-Pressure Trap Column (Analytical IC only) . . . . . . . . 28

    2.2.8 Pulse Damper (Capillary IC only) . . . . . . . . . . . . . . . . . . . . 28

    2.3 DP/SP Flow Schematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

    2.3.1 Isocratic Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . 29

    2.3.2 Gradient Pump Flow Schematic . . . . . . . . . . . . . . . . . . . . . . 30

    2.4 DP/SP Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

    2.5 Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

    2.5.1 EO (Optional) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35

    2.5.2 Pressurizing Eluent Reservoirs . . . . . . . . . . . . . . . . . . . . . . . 35

    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

  • Contents

    Doc. 065446-02 12/14 iii

    2.13 High-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68

    2.13.1 4-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

    2.13.2 6-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

    2.13.3 10-Port Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

    2.14 CD Conductivity Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

    2.14.1 Heated Conductivity Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

    2.14.2 Suppressor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74

    2.14.3 System Flow Schematics for Conductivity Detection . . . . . 75

    2.15 ED Electrochemical Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78

    2.15.1 Electrochemical Detector Cell . . . . . . . . . . . . . . . . . . . . . . . 78

    2.15.2 Combination pH-Ag/AgCl Reference Electrode . . . . . . . . . 80

    2.15.3 Palladium Hydrogen (PdH) Reference Electrode . . . . . . . . . 82

    2.16 DC Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83

    2.17 I/O Option . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

    2.17.1 I/O Option Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88

    2.17.2 Analog Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89

    2.17.3 Power, Relays, and TTL Outputs . . . . . . . . . . . . . . . . . . . . . 91

    2.17.4 TTL Inputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

    2.18 Automation Manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98

    2.18.1 AM High-Pressure Switching Valves . . . . . . . . . . . . . . . . . 100

    2.18.2 AM Low-Pressure Valves . . . . . . . . . . . . . . . . . . . . . . . . . . 101

    2.18.3 AM High- and Low-Pressure Valve Control . . . . . . . . . . . 102

    2.18.4 RCH-1 Reaction Coil Heater . . . . . . . . . . . . . . . . . . . . . . . 105

    2.19 Electrochemical Detection Modes . . . . . . . . . . . . . . . . . . . . . . . . . . 106

    2.19.1 DC Amperometric Detection . . . . . . . . . . . . . . . . . . . . . . . 107

  • Dionex ICS-5000+ Operator’s Manual

    iv Doc. 065446-02 12/14

    2.19.2 Integrated and Pulsed Amperometric Detection . . . . . . . . 107

    2.19.3 Cyclic Voltammetry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110

    2.19.4 Waveforms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 110

    2.19.5 Storing and Reprocessing Amperometry Data . . . . . . . . . . 114

    TC Description . . . . . . . . . .

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