Dionex ASE 150 Operator's Manual

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ASE® 150

Accelerated Solvent Extractor

Operator's Manual

Document No. 065207

Revision 02

September 2008

This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transmitted, transcribed, stored in a retrieval system, or transmitted into any human or computer language, in any form or by any means, electronic, mechanical, magnetic, manual, or otherwise, or disclosed to third parties without the express written permission of Dionex Corporation, 1228 Titan Way, Sunnyvale, California 94088-3603 U.S.A.

DISCLAIMER OF WARRANTY AND LIMITED WARRANTY

THIS PUBLICATION IS PROVIDED “AS IS” WITHOUT WARRANTY OF ANY KIND. DIONEX CORPORATION DOES NOT WARRANT, GUARANTEE, OR MAKE ANY EXPRESS OR IMPLIED REPRESENTATIONS REGARDING THE USE, OR THE RESULTS OF THE USE, OF THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY, RELIABILITY, CURRENTNESS, OR OTHERWISE. FURTHER, DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR CHANGES.

TRADEMARKS

AutoSeal is a trademark of Dionex Corporation. ASE 150 is a registered trademark of Dionex Corporation. Acrobat, Adobe, and Adobe Reader are registered trademarks of Adobe Systems, Incorporated. C-2000 and Hastelloy are registered trademarks of Haynes International, Inc. PEEK is a trademark of Victrex PLC. Perlast is a registered trademark of Precision Polymer Engineering, Ltd. Teflo n and Viton

are registered trademarks of E. I. duPont de Nemours & Company.

PRINTING HISTORY

Revision 01, April 2008 Revision 02, September 2008

1 • Introduction

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

1.2 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.2.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.2.2 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

1.3 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

1.4 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

2•Description

2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2.1.1 Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

2.1.2 Sample Cells and Rinse Cells . . . . . . . . . . . . . . . . . . . . . . . . . . 11

2.1.3 Collection Vessels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

2.1.4 Solvent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.1.5 Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

2.2 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

2.3 ASE 150 Extraction Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

2.4 Method Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

2.5 Preprogrammed Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

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3 • Operation and Maintenance

3.1 Preparing to Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25

3.1.1 Selecting and Preparing Solvent . . . . . . . . . . . . . . . . . . . . . . . .25

3.1.2 Filling the Solvent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . .29

3.1.3 Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31

3.1.4 Installing the Cell Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34

3.1.5 Filling the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37

3.1.6 Installing the Collection Vessel . . . . . . . . . . . . . . . . . . . . . . . . .39

3.1.7 Installing the Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . .41

3.2 Running . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42

3.2.1 Selecting the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42

3.2.2 Selecting the Cell Size . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42

3.2.3 Verifying the Cell Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .43

3.2.4 Starting the Run and Checking the Oven Status . . . . . . . . . . . .43

3.2.5 Installing the Sample Cell in the Cell Holder . . . . . . . . . . . . . .44

3.2.6 Completing the Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .45

3.3 Performing Post-Run Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46

3.3.1 Cleaning the Sample Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46

3.3.2 Processing Extracts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46

3.4 Stopping a Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47

3.5 Rinsing/Priming the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .48

3.6 Editing a Custom Method (Methods 1 through 24) . . . . . . . . . . . . . . . .49

3.7 Developing a New Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .52

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3.8 Performing Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

3.8.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

3.8.2 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

3.8.3 Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

3.9 Shutting Down . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

4 • Troubleshooting

4.1 Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

4.2 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65

4.3 Gas Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

4.4 Stopped System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67

Contents

5•Service

5.1 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

5.2 Replacing the Cell End Cap Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69

5.3 Replacing the Cell End Cap O-Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . 72

5.4 Removing the Right-Side Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

5.5 Replacing Pump Check Valve Cartridges . . . . . . . . . . . . . . . . . . . . . . . 75

5.5.1 Before Beginning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

5.5.2 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

5.5.3 Removing the Check Valves and Cartridges . . . . . . . . . . . . . . 76

5.5.4 Installing New Check Valve Cartridges . . . . . . . . . . . . . . . . . . 77

5.5.5 Reinstalling the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . 77

5.5.6 Cleaning the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . 77

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5.5.7 Reinstalling the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78

5.5.8 Completing the Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78

5.6 Replacing Pump Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79

5.6.1 Before Beginning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79

5.6.2 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79

5.6.3 Replacing the Piston High-Pressure Seal . . . . . . . . . . . . . . . . .79

5.6.4 Replacing the Piston Air Seal . . . . . . . . . . . . . . . . . . . . . . . . . .81

5.6.5 Reinstalling the Pump and Completing the Procedure . . . . . . .83

5.7 Replacing the Pressure Relief Valve . . . . . . . . . . . . . . . . . . . . . . . . . . .84

5.8 Rebuilding the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .86

5.8.1 Removing the Static Valve from the System . . . . . . . . . . . . . .88

5.8.2 Disassembling the Static Valve Body . . . . . . . . . . . . . . . . . . . .90

5.8.3 Installing the New Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .92

5.8.4 Reassembling the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . .93

5.8.5 Reinstalling the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . . . .97

5.9 Replacing the Source Needle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99

5.10 Replacing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102

A • Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103

A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103

A.2 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103

A.3 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104

A.4 Pneumatic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104

A.5 Front Panel Display and Keypad . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104

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Contents

A.6 Sample Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104

A.7 Collection Vessels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104

A.8 Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105

B • Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

B.1 Facility Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107

B.2 Installation Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108

B.2.1 Connecting the Nitrogen Gas Source . . . . . . . . . . . . . . . . . . . 108

B.2.2 Connecting the Drain Hose . . . . . . . . . . . . . . . . . . . . . . . . . . . 110

B.2.3 Checking the Oven Voltage Switches. . . . . . . . . . . . . . . . . . . 110

B.2.4 Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . 111

B.2.5 Checking Pressure Readings. . . . . . . . . . . . . . . . . . . . . . . . . . 112

B.2.6 Connecting the Solvent Reservoir. . . . . . . . . . . . . . . . . . . . . . 113

B.2.7 Installing the Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

B.2.8 Adjusting the Cell Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116

B.2.9 Selecting Setup Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118

B.2.10 Rinsing the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120

C • User Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125

C.1 Operational Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126

C.1.1 Menu Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126

C.1.2 Status Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127

C.1.3 Setup Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

C.1.4 Method Editor Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129

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ASE 150 Operator’s Manual

C.2 Diagnostic Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131

C.2.1 Diagnostics Menu. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131

C.2.2 Sensors Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .132

C.2.3 Regulators Screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .133

C.2.4 Hydrocarbon Sensor Screen. . . . . . . . . . . . . . . . . . . . . . . . . . .134

C.2.5 Extraction Counters Screen . . . . . . . . . . . . . . . . . . . . . . . . . . .135

C.2.6 Moduleware Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .136

D • Reordering Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . .137

E • Theory of ASE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .141

E.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .141

E.2 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .143

E.3 Method Optimization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .145

E.3.1 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .145

E.3.2 Extraction Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .148

E.4 Method Development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .151

E.5 Selectivity in ASE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .152

E.6 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157

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1.1 Overview

1 • Introduction

The ASE

150 Accelerated Solvent Extractor is a system for extracting either

organic or inorganic compounds from a variety of solid or semisolid samples at a variety of pH values. The ASE 150 can be used with organic solvent, aqueous buffer, water, and small amounts of mineral acids. The ASE 150 accelerates the traditional extraction process by using solvent at elevated temperatures and pressures. Pressure is maintained in the sample cell to maintain the heated solvent in a liquid state during the extraction. After heating, the extract is rinsed from the sample cell into a collection vessel and is ready for analysis.

Solvent Reservoir

Sample Cell

and Oven

Location

Waste

Figure 1-1. ASE 150 Accelerated Solvent Extractor

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Collection Vessel

ASE 150 Operator’s Manual

The ASE 150 is designed to minimize the amount of solvent used without sacrificing the speed of extraction or ease of operation. Samples are extracted one at a time, and the extraction process is typically completed in 15 to 25 minutes. All functions are controlled from the ASE 150 front panel.

Built-in safety diagnostics monitor the system during operation. If a problem occurs, the front panel displays an error message that identifies the problem. In addition, the method currently running is aborted and basic system functions are shut down until the situation is corrected.

1.2 About This Manual

1.2.1 Overview

The electronic version (i.e., PDF file) of the ASE 150 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 Adob

Chapter 1 Introduction

Chapter 2 Description

Chapter 3 Operation and Maintenance

Chapter 4 Troubleshooting

Chapter 5 Service

Appendix A Specifications

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e® Acrobat® or Adobe Reader® for assistance.

Introduces the ASE 150; explains the conventions used in this manual, including safety-related information.

Describes ASE 150 operating features and the extraction process.

Provides operating instructions and routine preventive maintenance procedures.

Lists error messages and how to troubleshoot them; lists operating problems and how to resolve them.

Provides step-by-step instructions for routine service and parts replacement procedures that the user can perform.

Provides specifications and installation site requirements.

1 • Introduction

Appendix B Installation

Appendix C User Interface

Appendix D Reordering Information

Appendix E Theory of ASE

Describes how to install the ASE 150.

Illustrates and describes the display screens on the ASE 150 front panel.

Lists spare parts for the ASE 150.

Describes the theory behind performing extractions with ASE.

1.2.2 Safety Messages and Notes

This manual contains warnings and precautionary statements that can prevent personal injury and/or damage to the ASE 150 when 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, may 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.

Messages d’avertissement en français

Signale une situation de danger immédiat qui, si elle n'est pas évitée, entraînera des blessures graves à mortelles.

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ASE 150 Operator’s Manual

Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures graves à mortelles.

Signale une situation de danger potentiel qui, si elle n'est pas évitée, pourrait entraîner des blessures mineures à modérées. Également utilisé pour signaler une situation ou une pratique qui pourrait gravement endommager l'instrument mais qui n'entraînera pas de blessures.

Warnhinweise in Deutsch

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.

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

the user to an unexpected result of an action, suggest how to optimize instrument performance, etc.

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1.3 Safety and Regulatory Information

The ASE 150 was manufactured by Dionex Corporation at the following location: 527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The ASE 150 is designed for solvent extraction applications and should not be used for any other purpose. Operation of an ASE 150 in a manner not specified by Dionex may result in personal injury.

If you have a question regarding appropriate usage, contact Dionex before proceeding. In the U.S., call 1-800-346-6390 and select the Technical Support option. Outside the U.S., call the nearest Dionex office.

1.4 Safety Labels

The cTUVus Mark safety label and the CE Mark label on the ASE 150 indicate that the ASE 150 is in compliance with the following standards.

EMC Susceptibility and Emissions

• EN 61326-1:2006

1 • Introduction

Safety

• CAN/CSA-C22.2 No. 61010-1:2004

• EN 61010-1:2001

• UL 3101-1/10.93

• UL 61010-1:2004

The symbols below appear on the ASE 150 or on ASE 150 labels.

Alternating current

Primary protective conductor terminal

Secondary protective conductor terminal

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ASE 150 Operator’s Manual

Power supply is on

Power supply is off

Hot surface

Indicates a potential hazard. Refer to the operator’s manual for an explanation of the hazard and how to proceed.

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2.1 Operating Features

Figure 2-1 illustrates the main operating features of the ASE 150 Accelerated

Solvent Extractor.

2 • Description

Figure 2-1. ASE 150 Operating Features

Solvent Reservoir

Sample Cell

Oven

Control Panel

Door OPEN Lever

Waste Bottle

Needle UP/DOWN Switch

Collection Vessel

(250-mL bottle shown)

Drip Tray

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ASE 150 Operator’s Manual

Solvent Reservoir

A 2-liter solvent reservoir is installed in a recess on top of the ASE 150. The recess contains a plastic liner that collects any solvent leaks or spills that may occur and directs them through a drain tube to the rear panel. A drain hose connects to the drain tube and is routed to a waste container.

Sample Cell

Before a sample is run or a rinse cycle is performed, a sample cell or rinse cell must be installed in the cell holder on the inside of the cell door. To access the cell holder, push down on the

Oven

The oven is located behind the cell door. This area also houses the AutoSeal™ tips, which seal the cell during a run.

Control Panel

The ASE 150 control panel includes a display screen and a membrane keypad, which are used to control ASE 150 operation.

OPEN lever and then pull open the door.

Waste Bottle

The waste bottle is a 250-mL collection bottle that is sealed with a special built-in cap assembly.

Needle Up/Down Switch

The UP/DOWN toggle switch controls the position of the source and vent needles. When the needles are in the “down” position, they pierce the collection vessel septum. The source needle allows the extract to flow from the sample cell into the collection vessel. The vent needles allow displaced gases to escape to the waste bottle and the system vent.

Drip Tray

A pull-out drip tray is installed below the oven to collect any liquid leaks that may occur during a run or rinse cycle.

Collection Vessel

After each extraction, the collection vessel (either a 250-mL collection bottle or a 60-mL collection vial) contains solvent and the analytes extracted from the sample.

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2 • Description

Safety Shields

The doors on the waste and collection vessel compartments are safety shields that protect operators in the rare case of a bottle or vial breakage. The doors must be closed for safe operation.

2.1.1 Control Panel

Use the control panel screen and buttons to control ASE 150 operation. The screen displays status and operating information. You can edit any

field on the screen that contains a blinking cursor. A field without a blinking cursor is for display only.

STATUS SETUP

METHOD EDITOR DIAGNOSTICS

START

RINSE

STOP

Figure 2-2. ASE 150 Control Panel

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ASE 150 Operator’s Manual

Button Function

START

RINSE

STOP

Starts the currently selected method. The LED starts flashing when the oven is within 1 °C of the set point, indicating it is okay to load the sample cell into the oven. During the method run, the LED is lighted, but does not flash. When the method finishes running (or is aborted), three beeps are emitted and the LED turns off. See Section 2.4

for details about methods.

Starts a rinse cycle in which about 5 mL of solvent is pumped through the system. During the rinse cycle, the LED is lighted. When the rinse cycle is complete (or is aborted), three beeps are emitted and the LED turns off.

Note: Always install a rinse cell and a collection vessel before starting a rinse cycle. See Section 3.5

for instructions.

Interrupts the currently running method or rinse cycle and displays the

ABORT screen. Pressing the button lights the

LED. The LED turns off when you select an option on the

ABORT screen. See Section 3.4 for details.

Exits the screen currently displayed and returns to the screen one level up in the hierarchy. For example, if the

EDITOR

the

screen is displayed, pressing MENU returns you to

MENU screen. See Figure C-1 for an overview of the

METHOD

screens. When the cursor is in an editable field, pressing

discards any change and reverts to the previously selected parameter.

Selects the field the cursor is currently pointing to. On the

MENU or DIAGNOSTICS screen, this selects and displays a

different screen. On other screens, pressing

ENTER moves

the cursor from the left margin to the first field in that line that can be edited; it also changes the normal cursor into the blinking editing cursor.

When the cursor is in an editable field, pressing

ENTER saves

the parameter currently displayed in the field.

Table 2-1. ASE 150 Control Panel Button Functions

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Button Function

Moves the cursor, in the direction of the arrow, to the next selectable line on the display (if any).

When the cursor is in an editable field, pressing an arrow button displays the next or previous parameter or numeric value allowed for the field.

Note: Pressing and holding down an arrow button moves the cursor continuously through the allowed settings.

Table 2-1. ASE 150 Control Panel Button Functions (Continued)

2.1.2 Sample Cells and Rinse Cells

NOTE Appendix D contains part numbers for cells, bottles,

vials, and other accessories.

Sample Cells

Cell Material Sizes Available (mL) Used For

Stainless steel 1, 5, 10, 22, 34, 66, and

100

Zirconium 66 and 100 Extraction of basic or acidic

2 • Description

Extractions with solvents

matrices, and extractions with solvents

Sample cells consist of a cell body and two interchangeable caps, which are screwed onto each end of the cell body. The cell body and end caps are made of the same material. Inside each end cap is a frit in the same material as the cell, as well as a PEEK™ seal. During a run, the cell end caps are compressed by the oven to form a tight seal between the caps and the cell body.

Always tighten the cell end caps by hand. Use of a wrench or other tool can damage the cell, as well as the seals inside the cell end caps.

Each cell end cap contains an external O-ring. Teflon® O-rings (P/N 049457, pkg. of 50) are standard. Use Viton® O-rings (P/N 056325, pkg. of 50) for dioxins and other high temperature applications.

If Viton external O-rings are installed on the cell end caps, do not use acetone or other ketones.

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ASE 150 Operator’s Manual

Rinse Cells

Rinse cells are similar in appearance to sample cells, but are blue in color. During a rinse cycle, solvent passes directly through the rinse cell and into the collection vessel. For more information about rinse cycles, see

Section 3.5

The rinse cell size must be matched to the size of the sample cell, as indicated in the table below.

Use this rinse cell: With this sample cell:

Short (P/N 060174) 1 mL, 5 mL, 10 mL, 22 mL, 34 mL Medium (P/N 060175) 66 mL Long (P/N 060176) 100 mL

Ordering Sample Cells in Other Sizes

To perform a run with a cell in a different size than the size originally ordered, order the cells from Dionex. You will also need to order the Startup Kit appropriate for the new cell size. For cell and Startup Kit part numbers, see Appendix D

Note that installation of a different sample cell size will require a few additional changes:

• Reposition the cell holder to accommodate the new sample cell size,

if required. For instructions, refer to Section B.2.8

• Before beginning a run, specify the new cell size on the SETUP screen

(see Section C.1.3

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2.1.3 Collection Vessels

The following collection vessels are available:

Collection Vessel Part Number Quantity

60-mL clear vials 048784 Pkg. of 72 60-mL amber vials 048781 Pkg. of 72 60-mL clear graduated vial, Class A 068226 1 60-mL clear graduated vial, Class B 068248 1 250-mL clear bottles 056284 Pkg. of 12 250-mL clear graduated bottle, Class A 068225 1 250-mL clear graduated bottle, Class B 068249 1

Before each run, carefully inspect all collection vessels for chips, scratches, or cracks. If a collection vessel shows any sign of damage, do not use it.

Use each nongraduated collection vessel once only. Graduated collection vessels may be used multiple times, provided they are undamaged.

La présence de fêlure ou d’égratignures sur les flacons de collecte doit être vérifiée avant chaque extraction. N’utilisez jamais un flacon endommagé.

Les flacons non gradués sont à usage unique. Les flacons gradués peuvent être réutilisés tant qu’ils sont intacts.

Untersuchen Sie vor jedem Lauf alle Sammelgefäße auf Abplatzungen, Kratzer oder Risse. Wenn ein Sammelgefäß eine Beschädigung aufweist, sollten Sie es nicht mehr verwenden.

Graduierte Sammelgefäße können mehrfach verwendet werden, vorausgesetzt sie weisen keine Beschädigung auf.

2 • Description

Use each collection vessel cap and septum once only. This prevents solvent leaks caused by piercing the septum in the cap multiple times.

An adapter (P/N 066392) is required to install a 60

-mL vial in the

collection vessel area. The adapter is included in the Startup Kits for 1

-mL, 5-mL, 10-mL, 22-mL, and 34-mL sample cells.

The collection vessel caps (used with all bottles and vials) contain a solvent-resistant septum. During a run, the needle mechanism is lowered so that the needles pierce the septum, creating a liquid flow path from the

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ASE 150 Operator’s Manual

sample cell to the collection vessel. After a run, the collection vessel contains solvent and the analytes extracted from the sample.

2.1.4 Solvent Reservoir

The ASE 150 Ship Kit (P/N 066399) includes a 2-liter glass bottle with shatterproof plastic coating (P/N 045901) and a bottle cap assembly (P/N 068077) with tubing and fittings for the inlet and outlet connections. For instructions on how to install the solvent reservoir, see Section 3.1.2

Use only Dionex solvent reservoirs. These are glass bottles with a shatterproof plastic coating. To prevent operator injury, make sure the pressure applied to the bottles does not exceed 0.07 MPa (10 psi).

Utilisez uniquement des réservoirs à solvant Dionex. Ce sont des réservoirs en verre à revêtement incassable en plastique. Veillez à ce que la pression exercée sur ces réservoirs ne dépasse pas 0,07 MPa.

Verwenden Sie ausschließlich die Lösemittelbehälter von Dionex. Dabei handelt es sich um Glasbehälter mit einer splittersicheren Plastikbeschichtung. Vergewissern Sie sich, daß der Druck, der auf die Behälter ausgeübt wird, 0,07 MPa nicht übersteigt.

Never fill the solvent reservoir or disconnect the tubing connections to the solvent and gas connectors during a run or rinse cycle. At these times, the solvent reservoir is pressurized. If you remove the bottle cap, the ASE 150 may not operate to specification.

2.1.5 Waste Bottle

A 250-mL collection bottle (without the cap) is used to collect system waste. Three vent lines, one from the pressure relief valve and two from the needle mechanism, are connected to the built-in waste bottle cap. The waste bottle collects the small amounts of condensed solvent vented through these lines.

A vent outlet line is also connected to the waste bottle cap; gas is vented out this line to the rear panel. The ASE 150 Ship Kit (P/N 066399) provides vent tubing (P/N 053514) that you can connect to the vent outlet on the rear panel (see Figure 2-3

NOTE Check the waste bottle daily and empty whenever

necessary.

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) and then route to a vent hood.

2.2 Rear Panel

Figure 2-3 illustrates the rear panel of the ASE 150.

2 • Description

Power

Oven Voltage

Switches

Model Data

Label

Nitrogen Gas

Inlet

Vent Outl et

Drain

Figure 2-3. ASE 150 Rear Panel

• The POWER switch provides on/off control of the main power for the system.

The power receptacle also includes the fuse holder. For instructions on how to replace the fuses, see Section 5.10

• The oven voltage switches must be set to match the voltage from the power

source at the ASE 150 installation site. For instructions on how to set the switches, see Section B.2.3

• The model data label lists fuse and power information, as well as the ASE 150

serial number. You will be asked to provide the serial number when ordering replacement parts for the system.

• The NITROGEN connector is connected to a nitrogen supply regulated to

between 0.97 and 1.38 MPa (140 and 200 psi); 1.03 MPa (150 psi) is recommended. For installation instructions, see Section B.2.1

• The VENT connector provides a connection for the vent outlet line. For

installation instructions, see Section B.2.1

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ASE 150 Operator’s Manual

• The drain directs solvent spills from the bottle area on top of the ASE 150 to

the rear panel. A drain hose connects to the fitting. For installation instructions, see Section B.2.2

2.3 ASE 150 Extraction Process

Preparing to Run an Extraction

The following steps are required before the ASE 150 can perform an extraction. Refer to Chapter 3

• Fill the solvent reservoir.

• Prepare the sample and load it into the sample cell.

• Install the waste bottle and collection vessel.

• Select or create a method.

• Press the START button.

• Verify that the STATUS on the STATUS screen is OVEN READY (see Figure 2-5)

and the LED on the

for detailed instructions for each step.

START button is flashing.

• Install the sample cell in the cell holder and close the cell door.

• Press the START button.

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2 • Description

Performing the Extraction

After you complete the preparation steps described on page 16 and press START the second time, the ASE 150 performs the extraction. The extraction process consists of six main steps.

1. Fill the cell with solvent—the pump is turned on and the static valve is closed (see

Figure 2-4

). Solvent is pumped into the sample cell until the cell pressure reaches

10.35 MPa (1500 psi). Thereafter, the static valve

opens occasionally to maintain the pressure at 10.35 MPa (1500 psi).

2. Heat the cell (equilibration)— the temperature in the cell is heated to the set point specified in the method.

Solvent

Bottle

Oven

Pump

Pressure

Relief Valve

Purge Valve

Sample Cell

Static Valve

3. Static extraction—the cell remains filled with the solvent at the temperature set point.

Waste Bottle

Figure 2-4. Extraction Process Schematic

Collection Vessel

Nitrogen

4. Rinse with fresh solvent—the static valve opens and the extract flows into the collection vessel. Fresh solvent is pumped through the cell.

5. Purge solvent from the system—the purge valve opens and gas purges the remaining solvent from the cell into the collection vessel.

6. Relieve pressure—the pressure relief valve opens and residual pressure is released from the cell.

NOTE Static extraction and rinsing can be repeated multiple

times.

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ASE 150 Operator’s Manual

Monitoring the Progress of a Run

To monitor the progress of a run, press MENU, move the cursor to STATUS (if necessary), and press

ENTER. The STATUS screen appears (see Figure 2-5).

STATUS STATIC METHOD PCB PRESSURE TEMP 100C

Figure 2-5. Status Screen Example

The

STATUS screen operating parameters are updated in real time.

• STATUS—the current system status. During a run, the status field displays the

following status states (in the order given): Oven Wait, Oven Ready, Load, Preheat (optional), Fill, Heat, Static, Rinse, Purge, Relief, Unload, and Idle.

• METHOD—the name or number of the current method.

• VOL—the approximate volume of solvent (in mL) delivered by the pump

since the method started running.

VOL 1565PSI TIME

75mL

2:25

• PRESSURE—the current sample cell pressure reading.

• TEMP—the temperature specified in the method.

• TIME—the elapsed time since the method started running.

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2.4 Method Control

A method determines how the ASE 150 performs the sample extraction. Methods are defined on the

METHOD EDITOR screen (see Figure 2-6).

2 • Description

METHOD TEMPERATURE STATIC TIME RINSE VOLUME

Figure 2-6. Method Editor Screen (Initial View)

The following method parameters define the method. See Section C.1.4 detailed descriptions of the method parameters.

100C

5MIN

60%

for

• TEMPERATURE—the temperature at which to heat the cell.

• STATIC TIME—the number of minutes to maintain the cell contents (sample

and solvent) at the temperature set point.

• RINSE VOLUME—the amount of solvent to rinse through the sample cell after

the static extraction.

• PURGE TIME—the amount of time the cell is purged with nitrogen.

• STATIC CYCLE—the number of times the static extraction and rinse cycles are

performed.

• CELL TYPE—the type of cell to use (stainless steel or zirconium).

Two types of methods are available:

• Preprogrammed methods are application-specific methods created by Dionex.

These methods cannot be changed or deleted by the user. For a list of the parameters for each preprogrammed method, see Section 2.5

• Custom methods are user-programmable methods. All custom methods

initially contain the default method parameters. You can modify these methods as required. For instructions on how to edit a custom method, see

Section 3.6

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ASE 150 Operator’s Manual

2.5 Preprogrammed Methods

To help you quickly produce results with the ASE 150, Dionex provides nine preprogrammed methods. These methods are designated by three-letter abbreviations (see the table below).

Preprogrammed Method Method Name

Semivolatiles BNA Total Fat (crude) FAT Chlorinated Herbicides HRB Organochlorine Pesticides OCP Organophosphorous Pesticides OPP Polychlorinated Biphenyls PCB Dioxins and Furans PDF Polymer Additives PPE Total Petroleum Hydrocarbons TPH

The remainder of this section lists the recommended solvent and the operating conditions for each preprogrammed method. You cannot edit or delete a preprogrammed method.

BNA (Semivolatiles) Method Parameters

Solvent MeCl2/Acetone (1:1, v/v) Temperature 100 °C

Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

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2 • Description

FAT (Total Fat) Method Parameters

Solvent Hexane/Acetone (4:1) Temperature 125 °C Static Time 5 min Rinse Volume 100% Purge Time 60 sec Static Cycle 3 Cell Type Stainless steel

HRB (Chlorinated Herbicides) Method Parameters

Solvent MeCl2/Acetone (1:1) with 1%

3PO4

Temperature 100 °C Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

OCP (Organochlorine Pesticides) Method Parameters

Solvent Hexane/Acetone (1:1, v/v) Temperature 100 °C Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

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ASE 150 Operator’s Manual

OPP (Organophosphorous Pesticides) Method Parameters

Solvent MeCl2/Acetone (1:1, v/v) Temperature 100 °C

Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

PCB (Polychlorinated Biphenyls) Method Parameters

Solvent Hexane Temperature 100 °C Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

PDF (Dioxins and Furans) Method Parameters

Solvent Toluene Temperature 200 °C Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

22 Doc. 065207-02 9/08

2 • Description

PPE (Polymer Additives) Method Parameters

Solvent 2.5% Cyclohexane in Isopropyl

Alcohol

Temperature 140 °C Static Time 3 min Rinse Volume 100% Purge Time 60 sec Static Cycle 3 Cell Type Stainless steel

TPH (Total Petroleum Hydrocarbons) Method Parameters

Solvent MeCl2/Acetone (1:1, v/v) Temperature 175 °C

Static Time 5 min Rinse Volume 60% Purge Time 100 sec Static Cycle 1 Cell Type Stainless steel

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3 • Operation and Maintenance

3.1 Preparing to Run

3.1.1 Selecting and Preparing Solvent

Precautions

Do not use solvents with an autoignition point below 200 °C. The table below lists some solvents that should not be used with the ASE 150. If you have a question about solvent suitability, contact Dionex.

Do Not Use These Solvents Autoignition Point

Carbon disulfide: CS Diethylether: (C 1,4-dioxane: C

N'utilisez pas de solvants ayant un point éclair inférieur à 200 °C. Le tableau ci-dessous liste quelques solvants qui ne doivent pas être utilisés avec l'ASE 150. Contactez Dionex si vous avez un doute concernant l’usage d’un solvant absent de la liste.

O 180 °C

2H5)2

4H8O2

100 °C

180 °C

Solvants à ne pas utiliser Point d'auto-inflammation

Disulfure de carbone: CS Éther diéthylique: (C 1,4-dioxane: C

Verwenden Sie keine Lösungsmittel, deren Selbstentzündungstemperatur unter 200°C liegt. Die untenstehende Tabelle zeigt einige Lösungsmittel, die Sie nicht mit dem ASE 150 verwenden sollten. Bei Fragen zur Eignung von Lösungsmitteln wenden Sie sich bitte an Dionex.

Nicht zu verwendende Lösungsmittel

4H8O2

Kohlendisulfid: CS Diethyläther: (C 1,4-dioxan: C

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2H5)2

4H8O2

2H5)2

O180 °C

100 °C

O 180 °C

180 °C

Selbstentzündungstemperatur

100 °C

180 °C

ASE 150 Operator’s Manual

Guidelines for Selecting and Preparing Solvents

• When developing a new method, select a solvent or solvent mixture

that has a high solubility for the analytes of interest, but not for the sample matrix. If you have been using another method (Soxhlet, for example), use the same solvent with the ASE 150 that you used with the other method.

• Before running a preprogrammed method, refer to Section 2.5 for the

recommended solvent.

• Use HPLC-grade or pesticide-grade solvents.

• Use organic or aqueous solvents.

• Use single-component or multiple-component solvents.

• Solvents do not generally need to be degassed. Degas solvents only if

the analyte of interest oxidizes easily.

• If Viton external O-rings are installed on the cell end caps, do not use

acetone and other ketones.

• Although the zirconium components in the ASE 150 flow path are

more resistant to acids and bases at elevated temperatures than other metallic materials, follow these guidelines to prevent degradation and ensure optimum performance:

a. As a general rule, strong mineral acids such as hydrochloric acid

should not be used (at any concentration) as extraction solvents. This is because there are components in the flow path of the system (for example, the pump head) that are constructed of stainless steel and will corrode when used with strong acids. Sulfuric acid or nitric acid can be pumped as a solvent at concentrations less than 0.1% by volume. For additional details about acids that can be pumped as solvents, see Table 3-1

Using corrosive acids or bases can damage stainless steel cells and will void the product warranty.

b. Weak bases such as ammonia can be used at small percentages

(<5% by volume). Strong bases such as sodium hydroxide or potassium hydroxide can be pumped as extraction solvents at concentrations less than 0.1% by volume. For additional details about bases that can be pumped as solvents, see Table 3- 1

26 Doc. 065207-02 9/08

3 • Operation and Maintenance

c. Weak acids such as phosphoric or acetic acid can be used as

extraction solvents in small percentages (<5% by volume). Weak bases such as ammonia can be used at small percentages (<5% by volume).

d. Noncorrosive additives such as buffers (acetate, phosphate, etc.)

can be used as extraction solvents at moderate percentages.

e. In some cases, nitric or hydrochloric acid can be added directly to

the sample before it is placed into a zirconium cell (not a stainless steel cell). For example, 1 to 2 mL of 5% to 10% HCl can be added directly to a soil sample before it is loaded into a zirconium cell for extraction.

f. Table 3- 1

lists the allowable concentrations for several acids and bases. If a sample needs to be treated with acids stronger than the concentrations here, pretreat the sample with the concentrated acid before loading it into a zirconium cell (not a stainless steel cell). For more details about sample preparation, see

Section 3.1.3

Acid or Base Concentration

HCl 8 M No No Yes

HCl 10% No Yes Yes

HCl 0.1 M No Yes Yes

NaOH 8 M No No N/A

NaOH 10% No Yes N/A

NaOH 0.1 M Yes Yes N/A

8 M No No Yes

2SO4

Okay to pump from solvent reservoir? (Okay to use SST or Zr cells)

Add to sample and transfer to Zr cell? (Do not use SST cells)

Add to sample matrix with ASE Prep CR and transfer to Zr cell? (Do not use SST cells)

10% No Yes Yes

2SO4

5% solution Yes Yes Yes

2SO4

Table 3-1. Guidelines for Use of Acids and Bases with the ASE 150

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ASE 150 Operator’s Manual

Acid or Base Concentration

Okay to pump from solvent reservoir? (Okay to use SST or Zr cells)

Add to sample and transfer to Zr cell? (Do not use SST cells)

Add to sample matrix with ASE Prep CR and transfer to Zr cell? (Do not use SST cells)

H2SO4 0.1 M Yes Yes Yes

KOH 8 M No No N/A

KOH 10% No Yes N/A

KOH 0.1 M Yes Yes N/A

HNO

8 M No No Yes

10% Yes Yes Yes

HNO

0.1 M Yes Yes Yes

HNO

OH 8 M No No N/A

OH < 5% Yes Yes N/A

OH 0.1 M Yes Yes N/A

Trifluoroacetic acid

Ye s Ye s Ye s

< 5%

Acetic acid < 5% Yes Yes Yes

Phosphoric acid

Ye s Ye s Ye s

<5%

Table 3-1. Guidelines for Use of Acids and Bases with the ASE 150 (Continued)

If acids, bases, salts, or buffers are used as extraction solvents, rinse the system with 100% polar organic solvent (for example, acetone or methanol) or distilled water before turning off the power.

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3 • Operation and Maintenance

3.1.2 Filling the Solvent Reservoir

Use only Dionex solvent reservoirs. These are glass bottles with a plastic, shatterproof coating. Make sure the pressure applied to the bottles does not exceed 0.07 MPa (10 psi).

Never fill the solvent reservoir or disconnect the tubing connections to the solvent and gas connectors (see Figure 3-1 rinse cycle. At these times, the solvent reservoir is pressurized. If you remove the bottle cap when the solvent reservoir is pressurized, the ASE 150 may not operate to specification.

1. If you plan to run a preprogrammed method, refer to Section 2.5 for the recommended solvent. If you plan to run a custom method, review the solvent selection guidelines in Section 3.1.1

) during a run or

2. Fill the solvent reservoir with prepared solvent to the level indicated in Figure 3-1

NOTE The solvent level in the reservoir must remain

below the gas line. This prevents solvent from coming into contact with the pneumatic valves.

3. Place the bottle in the recess on top of the system.

4. Insert the solvent and gas lines extending from the underside of the bottle cap assembly into the bottle (see Figure 3-1

). Make sure the

end-line filter on the solvent line rests on the bottom of the bottle.

5. Hand-tighten the lock ring cap securely over the stopper.

6. If they are not already connected, screw the solvent line fitting into the solvent connector on the ASE 150 and then push the gas line fitting into the gas connector.

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ASE 150 Operator’s Manual

NOTE Always connect the solvent line to the solvent

connector first, and then the gas line to the gas connector. If you need to disconnect the lines, reverse the order. It is not necessary to disconnect the solvent and gas lines before refilling the bottle.

End-Line Filter

Figure 3-1. Solvent Reservoir Connections

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3.1.3 Preparing the Sample

If you have successfully followed a particular sample pretreatment procedure for another extraction method, continue using this procedure with the ASE 150. If you have never run an extraction—or if you are preparing a new sample—follow the guidelines here. This section discusses two sample pretreatment procedures:

• Samples that are dry, wet, or liquid should be mixed with a drying or

dispersing agent before being loaded into the cells.

• Samples with large particle sizes should be ground before being

loaded into the cells.

NOTE: Most problems with the ASE (accelerated solvent extraction) process are caused by errors made during sample preparation. To obtain high quality analytical results, pay careful attention to the sample preparation phase of the method. For more details, see Appendix E

Guidelines for Selecting a Drying or Dispersing Agent

• Although sodium sulfate is readily available, it should not be used in

ASE 150 cells. The use of sodium sulfate with very wet samples (30% moisture) will result in clogging of system components (such as the solvent line or needles) with recrystallized sodium sulfate. This occurs particularly if a mixed solvent with a polar component such as methanol or acetone is used. In these cases, use pelletized diatomaceous earth (DE) (P/N 062819) as a drying agent and mix it with the sample before loading into the sample cell (see the sample preparation guidelines on page 32 a drying agent in the cell in place of sodium sulfate for all levels of moisture.)

3 • Operation and Maintenance

). (Alternatively, DE can be used as

• For very wet samples, regardless of which drying agent is used, you

may add sodium sulfate to the collection vessels after collection and then pass the extracts through either a drying column or drying cartridge to dry the extract completely. At the temperatures used during ASE 150 extractions, more water is co-extracted than with other extraction procedures. To ensure good analyte recovery, thoroughly rinse the sodium sulfate out of the collection vessel and the cleanup column.

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ASE 150 Operator’s Manual

• If a sample needs to be treated with acids stronger than the

concentrations listed in Table 3- 1 concentrated acid before loading it into the cell. After the pretreatment, mix the sample with ASE Prep CR Resin (P/N 080024) to partially neutralize the acid to approximately 0.1 M. The sample may need to be mixed with pelletized diatomaceous earth (DE) (P/N 062819) to absorb water, depending on how much acid was used to pretreat the sample.

For example, if a food sample is treated with 10 mL of 8 M HCl, mix the liquid hydrolysate with 30 to 40 g of ASE Prep CR and 15 g of DE. When the sample is thoroughly mixed, add it to the zirconium cell. (Do not use a stainless steel cell.) Use this ratio of acid to ASE Prep CR whenever using strong acids for pretreatment of samples.

If you have any questions about compatibility of an acid or base, please contact Dionex.

Guidelines for Sample Preparation with a Drying or Dispersing Agent

, pretreat the sample with the

The following mixtures are recommendations only; adjust the proportions as required.

• If the sample appears dry, use this mixture:

4 grams sample to 1 gram DE Mix the sample and the DE thoroughly in a small bottle, beaker, or

mortar.

• If the sample appears wet, use this mixture:

4 grams sample to 2 grams DE Mix the sample and the DE thoroughly in a small bottle, beaker, or

mortar.

• If the sample is pure liquid, use 5 grams sample to 3 grams DE.

Fill the cell with DE and then add the sample.

NOTE Certain pure liquid samples may be mixed with

drying or dispersing agents other than DE. For a current list of approved materials, contact Dionex.

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3 • Operation and Maintenance

Guidelines for Grinding

• For an efficient extraction to occur, the solvent must make contact

with the target analytes. The more surface area that can be exposed in a sample, the faster extraction will occur. Therefore, samples with large particle sizes should be ground prior to extraction. Often a large, representative sample can be ground, and then weighed portions of the ground sample can be used for extraction.

• Soil and sediment samples usually do not need to be ground, but it

may be necessary to remove stones or sticks from the samples prior to extraction.

• Polymer samples must be in a ground state for an efficient extraction

of additive compounds. Materials such as polymers and rubbers are best ground at reduced temperatures; for example, liquid nitrogen.

• Animal or plant tissue samples can be homogenized using any

procedure such as a blender or tissue homogenizer.

Sample Preparation by Grinding

Grind the sample with any of the following tools: a conventional mortar and pestle, an electric grinder, or an electric mill. For the most efficient extraction, grind until particles are smaller than 1 mm.

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3.1.4 Installing the Cell Filter

A disposable filter must be installed in the bottom end cap of the sample cell before sample is loaded. The filter prevents blockage of the frit in the bottom cap. For installation instructions, see page 34 to the information here to determine the appropriate filter material and size.

Cell filters are available in two materials:

• Use cellulose filters for most extraction methods that use organic

solvents.

• Use glass-fiber filters for aqueous extractions, where cellulose may

provide inadequate filtration or may interfere with the analytical technique.

Cell filters are available in two sizes:

• Use 27-mm filters for 1-mL, 5-mL, 10-mL, or 22-mL cells.

• Use 30-mm filters for 34-mL, 66-mL, or 100-mL cells.

Each ASE 150 Startup Kit includes a package of 100 cellulose filters, in the size appropriate for the sample cell size to be used. For information about reordering filters or ordering filters in a different material or size, refer to Appendix D

and page 35. Refer

To install a 27-mm filter in a 1-, 5-, 10-, or 22-mL cell:

1. Unscrew the bottom cap from the cell body.

Groove

To identify the cell top and bottom, designate the end of the cell with the groove around the body and the Dionex logo, serial

Logo, Serial

Number, and Size

number, and cell size as the cell top (see Figure 3-2

34 Doc. 065207-02 9/08

Figure 3-2. Sample Cell Top (Smaller Cells)

3 • Operation and Maintenance

2. Place a 27-mm filter in the center of the cell bottom cap (see Figure 3-3

PEEK

Bottom Cap of a

1-, 5-, 10-, or 22-mL Cell

Seal

3. To prevent leaks, check that no part of the filter overlaps onto the PEEK seal.

Figure 3-3. Installing a 27-mm Cell Filter

27-mm Filter

4. Carefully place the cell body over the bottom cap, screw the body onto the cap, and hand-tighten.

Always tighten the cell end caps by hand. Use of a wrench or other tool can damage the cell, as well as the seals inside the cell end caps.

To install a 30-mm filter in a 34-, 66-, or 100-mL cell:

1. Unscrew the top cap from the cell body and verify that a cap is installed on the bottom of the cell.

Groove

To identify the cell top and bottom, designate the end of the cell with the groove around the body and the

Logo and

Serial

Number

Dionex logo and serial number as the cell top (see Figure 3-4

Always tighten the cell end caps by hand. Use of a wrench or other tool can damage the cell, as well as the seals inside the cell end caps.

Do not place the 30-mm filter in the bottom cap before installing the cap; this creates an improper seal and allows leaks.

Figure 3-4. Sample Cell Top (Larger Cells)

2. Follow the steps in Figure 3-5 to install the 30-mm filter.

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ASE 150 Operator’s Manual

Insert a 30-mm filter into the cell at a slight angle.

Position the filter insertion tool (P/N 056929) over the filter.

Slowly push the insertion tool straight into the cell.

Push down until the filter is in full contact with the end cap.

Figure 3-5. Installing a 30-mm Cell Filter in a 34-, 66-, or 100-mL Cell

NOTE The procedure for installing 30-mm filters in

stainless steel and zirconium cells is the same. The photos in Figure 3-5

show a zirconium cell.

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3.1.5 Filling the Cell

Precautions:

• When filling the cell with sample, keep the threads on the cell body

and end cap as clean as possible to prevent thread fouling and extend the life of the cell.

• Also make sure that the ends of the cell body and the seals in the end

caps are clean; if debris remains here, it will damage the cell body and/or allow leaks during the run.

To fill a cell:

1. Use the funnel provided in the ASE 150 Startup Kit to carefully load the sample into the top of the sample cell. To accommodate different sample cell sizes, three funnels (with different inner diameters) are available (see Figure 3-6

3 • Operation and Maintenance

Funnel for 1-mL cells (P/N 068076

)

Funnel for 5-, 10-, and 22-mL cells (P/N 068075

Figure 3-6. Sample Funnels

)

Funnel for 34-, 66-, and 100-mL cells (P/N 056699

)

2. (Optional) To reduce the amount of solvent used during the run, fill any void volume in the cell with an inert material such as Ottawa sand (Fisher S23-2).

3. Using a soft brush or cloth, wipe all debris off the threads of the top cell end cap.

4. Screw the top cap onto the cell body. Hand-tighten the cap.

Always tighten the cell end caps by hand. Use of a wrench or other tool can damage the cell, as well as the seals inside the cell end caps.

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ASE 150 Operator’s Manual

5. Check the ends of each cell end cap to verify that the O-rings are in place and are in good condition (see Figure 3-7

• If an O-ring is dislodged, press

it into place, using the O-ring insertion tool (P/N 049660), provided in the ASE 150 Ship Kit (P/N 066399).

• If an O-ring is missing, place a

new O-ring over the opening in the end of the cell end cap. Press the O-ring into place, using the O-ring insertion tool (see Figure 3-8 information about ordering Orings, refer to Appendix D

). For

Verify that O-ring are installed and in good condition

Figure 3-7. Inspecting Cell O-Rings

O-Ring Insertion Tool (P/N 049660)

Place O-ring in opening and press into place

with insertion tool.

• If any O-ring has a hole size of

less than 0.5 mm, replace it. If a white Teflon O-ring is discolored, replace it (see the following instructions).

Figure 3-8. Installing a Cell End Cap O-Ring

To replace a cell end cap O-ring:

Be careful not to scratch the interior of the cell end cap when installing or removing the cell O-ring. Scratches on the sealing surface will prevent the O-ring from sealing properly and may result in leaks during operation.

1. Locate the small flathead screwdriver (P/N 046985) in the ASE 150 Ship Kit (P/N 066399).

2. Insert the tip of the screwdriver into the end cap and carefully pick out the O-ring. (This may be easier to do if you first remove the cap from the cell body and place it flat on the workbench.)

38 Doc. 065207-02 9/08

3 • Operation and Maintenance

3. Place a new O-ring over the opening in the end of the cell end cap. Press the O-ring into place using the O-ring insertion tool (see

Figure 3-8

3.1.6 Installing the Collection Vessel

During the extraction process, sensors determine if a collection vessel is present and, if so, whether it is full. If you want to attach a label to a collection vessel, or write an identification name or number on it, be sure the location does not block the sensors. Figure 3-9 locations for this information.

shows the acceptable

5.25 cm (2.07 in)

Bottle Label

Okay

3.45 cm (1.36 in)

Vial Label Okay

Figure 3-9. Acceptable Locations for Collection Vessel Labels

Before each run, carefully inspect all collection vessels for chips, scratches, or cracks. If a collection vessel shows any sign of damage, do not use it.

Use each nongraduated collection vessel once only. Graduated collection vessels may be used multiple times, provided they are undamaged.

La présence de fêlure ou d’égratignures sur les flacons de collecte doit être vérifiée avant chaque extraction. N’utilisez jamais un flacon endommagé.

Les flacons non gradués sont à usage unique. Les flacons gradués peuvent être réutilisés tant qu’ils sont intacts.

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ASE 150 Operator’s Manual

Untersuchen Sie vor jedem Lauf alle Sammelgefäße auf Abplatzungen, Kratzer oder Risse. Wenn ein Sammelgefäß eine Beschädigung aufweist, sollten Sie es nicht mehr verwenden.

Graduierte Sammelgefäße können mehrfach verwendet werden, vorausgesetzt sie weisen keine Beschädigung auf.

Use each collection vessel cap and septum once only. This prevents solvent leaks caused by piercing the septum in the cap multiple times.

1. Open the collection vessel compartment door and toggle the needle switch to the

UP position (see Figure 3-10).

2. If you are using a 60 adapter (P/N 066392) and then place the adapter on the collection bottle holder (see Figure 3-10 bottle, place the bottle directly on the collection bottle holder.

3. Toggle the needle switch to the

Needle Switch

Collection Bottle Holder

60-mL

Collection

Vial

Figure 3-10. Installing the Collection Vessel

Adapter for Vial

-mL collection vial, place the vial into the

). If you are using a 250-mL collection

DOWN position and close the door.

250-mL

Collection

Bottle

40 Doc. 065207-02 9/08

3.1.7 Installing the Waste Bottle

Use a 250-mL collection bottle (without a cap) for the waste bottle.

1. Open the waste compartment door.

2. Tilt the waste bottle at a slight angle and position it below the built-in bottle cap.

3. While being careful not to bend the tubing that extends from the bottle cap, insert the bottle into the bottle cap.

4. Tilt the cap and bottle toward you and screw the bottle into the cap.

5. Hand-tighten the bottle onto the cap to ensure a good seal.

3 • Operation and Maintenance

6. Release the bottle, allowing it to swing gently into place.

7. Close the waste compartment door.

Figure 3-11. Installing the Waste Bottle

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ASE 150 Operator’s Manual

3.2 Running

3.2.1 Selecting the Method

1. Press MENU to display the MENU screen (see Figure 3-12).

STATUS SETUP METHOD EDITOR DIAGNOSTICS

Figure 3-12. Menu Screen

2. Move the cursor to

SETUP and press ENTER. The SETUP screen

appears (see Figure 3-13

METHOD CELL SIZE UNITS REDUCE RELIEF

Figure 3-13. Setup Screen

3. Press

ENTER to move the cursor to the method editing field.

4. Press an arrow button to step through the custom method numbers and the names of the preprogrammed methods. To edit a custom method, see Section 3.6 methods, refer to Section 2.5

5. When the method required for the run is displayed, press

3.2.2 Selecting the Cell Size

The ASE 150 determines various internal operating parameters (for example, the rinse volume) based on the cell size selected on the screen (see Figure 3-13 of the cell in use, select the correct size:

). If the selected cell size does not match the size

PCB 100ML PSI OFF

. For descriptions of the preprogrammed

ENTER.

SETUP

1. On the

SETUP screen, move the cursor to CELL SIZE and press ENTER.

2. Press an arrow button to step through the cell sizes.

3. When the correct cell size is displayed, press

42 Doc. 065207-02 9/08

ENTER.

4. Press MENU to return to the MENU screen.

3.2.3 Verifying the Cell Type

If you are going to run a custom method (method numbers 1 through 24), verify that the correct cell type is selected in the method.

3 • Operation and Maintenance

1. On the

ENTER. The METHOD EDITOR screen (see Figure 3-18) is displayed.

2. Press the down arrow until

3. If the selected cell type is incorrect, press arrow button to select the other type. Press

For details about editing custom methods, see Section 3.6

MENU screen, move the cursor to METHOD EDITOR and press

CELL TYPE is displayed.

ENTER and then press an

ENTER.

3.2.4 Starting the Run and Checking the Oven Status

1. On the MENU screen, move the cursor to STATUS and press ENTER.

STATUS screen (see Section C.1.2) appears.

The

2. Press

Do not install the cell while the status is OVEN WAIT. Installing the cell before the oven is ready will cause an error.

3. When the oven is within 1 °C of the set point, the

START, and then observe the STATUS field. If the STATUS is

OVEN WAIT, the oven temperature is not yet at the set point.

STATUS field

changes to

OVEN READY (see Figure 3-14) and the LED on the START

button begins flashing. You can now install the cell in the cell holder.

STATUS METHOD

PRESSURE

TEMP

Figure 3-14. Status Screen

Always install the cell in the cell holder. If you install the cell directly in the oven, the cell door will not close and the run will not start.

Doc. 065207-02 9/08 43

OVEN READY PCB

100C

VOL 0mL

0PSI

TIME

5:00

ASE 150 Operator’s Manual

3.2.5 Installing the Sample Cell in the Cell Holder

The installation procedure is the same for rinse and sample cells. A sample cell is shown in the photos.

1. Open the cell door.

2. While holding the cell at a slight angle, position the bottom end cap under the bottom latch of the cell holder.

3. Raise the cell so that the bottom end cap lifts the bottom latch.

Top L atch

Bottom

Latch

Bottom Cell End Cap

4. Straighten the cell until it is vertical, and then lower it until the top end cap rests on the top latch of the cell holder.

5. Close the cell door.

Figure 3-15. Installing a Sample Cell

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3.2.6 Completing the Run

1. Verify that a collection vessel and a waste bottle are installed (see

Section 3.1.6

cell, collection vessel, and waste bottle doors are closed.

and Section 3.1.7); the needle switch is down; and the

3 • Operation and Maintenance

2. Press

Do not attempt to open the cell door while a run is in progress.

N'ouvrez pas la porte pendant une extraction.

Halten Sie die Tür während der Extraktion geschlossen.

3. Monitor the run on the

4. When the run is complete, three beeps are emitted, the

5. Toggle the needle switch to the

START to begin the run. A typical run takes 15 to 25 minutes.

STATUS screen (see Figure 3-14).

turns off, and the

STATUS screen displays IDLE.

UP position and remove the collection

START LED

vessel containing the extract from the holder. Refer to Section 3.3 post-run procedures.

Cells are extremely hot after a run. Be especially cautious with cells that have been heated over 50 °C (122 °F).

Les cellules sont extrêmement chaudes après une extraction. Faites particulièrement attention aux cellules qui ont été chauffées à plus de 50 °C.

for

Die Zellen sind nach ihrer Entnahme sehr heiß. Seien Sie besonders vorsichtig, wenn Zellen über 50°C erhitzt wurden.

6. Put on the thermal gloves (P/N 060372) provided in the ASE 150 Ship Kit (P/N 066399).

7. Remove the cell from the cell holder and place it on the cell rack (P/N 059927) to cool.

8. Close the cell door until the next run, to save energy and prevent anyone from accidentally touching a hot surface.

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ASE 150 Operator’s Manual

3.3 Performing Post-Run Procedures

3.3.1 Cleaning the Sample Cells

Cells are extremely hot after an extraction. Allow cells to cool for at least 15 minutes before handling. Be especially cautious with cells that have been heated over 50 °C (122 °F).

Les cellules sont extrêmement chaudes après une extraction. Laissez-les refroidir pendant au moins 15 minutes avant de les manipuler. Faites particulièrement attention aux cellules qui ont été chauffées à plus de 50 °C.

Die Zellen sind nach ihrer Entnahme sehr heiß. Lassen Sie die Zellen mindestens 15 Minuten abkühlen. Seien Sie besonders vorsichtig, wenn Zellen über 50 °C erhitzt wurden.

After use, empty the cells and rinse the cell bodies and end caps with water or organic solvent.

• Both stainless steel and zirconium cell bodies (but not cell end caps)

can be cleaned in a dishwasher or high temperature cleaning unit. Do not exceed 200 °C (392 °F) when performing high temperature cleaning.

• For most applications, simply rinsing the end caps is sufficient. If

necessary, disassemble the end caps (see Section 5.2 soak in solvent to clean them.

• Do not use detergent to clean the end cap frits.

3.3.2 Processing Extracts

The composition of the extracts generated by the ASE 150 is very close to that generated by Soxhlet and other standard solid-liquid extraction techniques when using the same solvent. Use the same analytical method for ASE 150 extracts that you employed for extracts obtained from other techniques.

) and sonicate or

46 Doc. 065207-02 9/08

3.4 Stopping a Run

To stop a run before the end of the method, press STOP. This stops the run and displays the

ABORT screen (see Figure 3-16).

ABORT METHOD CONTINUE METHOD

3 • Operation and Maintenance

ABORT

Figure 3-16. Abort Screen

Move the cursor to the preferred option and press

ENTER.

• ABORT METHOD—cancels the method. If necessary, a purge is done to remove

solvent from the sample. Then, residual pressure is relieved from the system.

• CONTINUE METHOD—resumes the run from the point at which the STOP

button was pressed.

Runs Stopped Automatically

The ASE 150 contains built-in diagnostics and sensors that continuously monitor the system. Under certain conditions (for example, if the collection vessel becomes too full or if the hydrocarbon vapor level exceeds the upper limit), the system will automatically stop a run. If this occurs, the ASE 150 screen will display an error message; the message will remain on-screen until you press a button to clear it or until it is replaced by another error message. For a list of error messages (and corrective action to take), see Section 4.1

NOTE After a run is stopped (whether manually or

automatically), rinse the system before resuming operation. For instructions on how to run a rinse cycle, see Section 3.5

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ASE 150 Operator’s Manual

3.5 Rinsing/Priming the System

During a rinse cycle, approximately 5 mL of solvent is pumped through the system. Run a rinse cycle at the following times:

• After initial setup

• After refilling the solvent reservoir

• After changing solvents (rinse twice to remove all of the previous solvent)

• When the solvent lines contain air

• When acids, bases, salts, or buffers are used as extraction solvents, rinse the

system with deionized water at the end of operation.

• After the ASE 150 has been shut down for more than one day (see

Section 3.9

To run a rinse cycle:

1. Rinse cells are similar to sample cells, but they are blue in color. Check that the rinse cell size is matched to the sample cell size.

)

Use this rinse cell: With this sample cell:

Short (P/N 060174) 1 mL, 5 mL, 10 mL, 22 mL, 34 mL Medium (P/N 060175) 66 mL Long (P/N 060176) 100 mL

2. Install the rinse cell in the cell holder. Rinse cells are installed in the same way as sample cells; for instructions, see Section 3.2.5

3. Close the cell door.

4. Open the collection vessel compartment door, toggle the needle switch (see

Figure 3-10 Section 3.1.6

5. Toggle the needle switch to the

) to the UP position, and install a new collection vessel (see

DOWN position.

6. Close the door.

7. Press

RINSE to begin the rinse cycle. The LED on the RINSE button turns on,

and will remain lighted while the rinse cycle is in progress.

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3 • Operation and Maintenance

When the rinse cycle is complete (after about 1 minute), three beeps are emitted and the

RINSE button LED turns off.

8. Remove the collection vessel used for the rinse cycle.

9. If the oven is hot and you want to start a run right away: a. Put on the thermal gloves (P/N 060372) provided in the ASE 150 Ship Kit

(P/N 066399).

b. Remove the rinse cell from the cell holder and place it on the cell rack

(P/N 059927) to cool.

c. Close the cell door until the next run, to save energy and prevent anyone

from accidentally touching a hot surface.

3.6 Editing a Custom Method (Methods 1 through 24)

If none of the ASE 150 preprogrammed methods described in Section 2.5 is suitable for a particular extraction, edit one of the custom methods provided with the ASE 150.

Before beginning, review the method development guidelines in Section 3.7 the range of values allowed for each method parameter in Table 3- 1

. All

parameters in the custom methods are initially set to their default values.

Parameter Function Value Range TEMPERATURE

STATIC TIME

RINSE VOLUME

Temperature at which to heat the cell. Off, 40 to

200 °C (default = 100)

The number of minutes to maintain the cell contents (sample and solvent) at the temperature set point.

Amount of solvent to rinse through the sample cell after the static heating step, expressed as a percentage of the cell volume. For example, if the

RINSE VOLUME is set to 50%, 5 mL is

rinsed through a 10-mL cell, 17 mL is rinsed through a 34-mL cell, and so on.

Table 3-1. Method Parameters

0 to 99 min (default = 5)

0 to 150% volume in 5% increments (default = 60)

and

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ASE 150 Operator’s Manual

Parameter Function Value Range PURGE TIME

Amount of time the cell is purged with nitrogen. Dionex recommends the following settings:

• 40 to 80 seconds for a 1-mL, 5-mL,

10-mL, or 22-mL cell

• 70 to 110 seconds for a 34-mL cell

• 160 to 200 seconds for a 66-mL cell

• 250 to 290 seconds for a 100-mL cell

STATIC CYCLE

CELL TYPE

Number of times the static heating and rinsing steps are performed. When more than one cycle is specified, the rinse volume is divided among the cycles.

Specifies the type of cell used. SST (stainless

Table 3-1. Method Parameters (Continued)

20 to 900 sec (default = 100)

1 to 5 (default = 1)

steel) (default)

Zr (zirconium)

To edit a custom method (for example, method 1):

1. Press MENU to display the MENU screen.

STATUS SETUP METHOD EDITOR DIAGNOSTICS

Figure 3-17. Menu Screen

50 Doc. 065207-02 9/08

3 • Operation and Maintenance

2. Move the cursor to METHOD EDITOR and press ENTER. The METHOD EDITOR screen appears (see Figure 3-18 view additional parameters, press the down arrow button.

). All parameters do not fit on one screen. To

METHOD TEMPERATURE STATIC TIME RINSE VOLUME

PURGE TIME STATIC CYCLE CELL TYPE

SAVE

Figure 3-18. Method Editor Screen (All Parameters Shown)

The

METHOD EDITOR screen displays the parameters for the method last

selected on the

SETUP screen (see Section C.1.3).

100C

5MIN

60%

100SEC

SST

Press the down arrow button to scroll through the list of parameters.

3. To select a different method to edit: a. Press

ENTER to move the cursor to the method editing field.

b. Press an arrow button to step through the method numbers (1 through 24). c. When the desired method number is displayed, press

ENTER.

4. To edit the method: a. Press an arrow button to move the cursor to the first parameter that you

want to change (for example,

TEMPERATURE).

b. Press

ENTER. The cursor moves to the editing field.

NOTE If you decide not to edit this field, press MENU to

return the cursor to the left margin of the screen.

c. Press an arrow button to step through the values allowed for the

highlighted value. (Pressing and holding the arrow button steps through the values more rapidly.) When the required value is displayed, press

ENTER.

d. If other changes are required, repeat Step a

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through Step c.

ASE 150 Operator’s Manual

5. To save the method: a. Press an arrow button to move the cursor to b. To save the modified version of the method to the current method number,

ENTER.

press

NOTE Saving to the current method number will

permanently overwrite the previous version of the method.

c. To save to a different method number, press an arrow button to select the

desired number and press

d. Press

MENU to exit the METHOD EDITOR screen and return to the MENU

ENTER.

screen.

3.7 Developing a New Method

Follow the procedure below to develop a method for a new sample type.

1. Select a solvent (see Section 3.1.1

2. Prepare the sample (see Section 3.1.3

3. Edit a custom method (see Section 3.6

4. Run the new method three times (with the same cell and sample, into three separate collection vessels) and analyze the extracts.

SAVE and press ENTER.

5. If target analytes are present in extract 2 or 3, make the adjustments listed below (one at a time) to the method. After each adjustment, repeat the method and analyze the extract.

a. Raise the temperature. In general, raising the temperature increases the

efficiency of the extraction process. However, because compounds can degrade at high temperatures, it is advisable to raise the temperature in small increments (10 to 20 °C). The maximum allowable temperature of the ASE 150 is 200 °C. If oxidation is a concern, degas the solvent before use.

b. Run two static/rinse cycles. Extending the static time enhances diffusion

of the analytes into the extraction fluid. Separating the static time into two cycles, instead of using one longer cycle, allows the introduction of fresh

52 Doc. 065207-02 9/08

3 • Operation and Maintenance

solvent midway through. This helps maintain a favorable solvent/sample equilibrium for samples that are heavily loaded or otherwise difficult to extract.

c. Increase the rinse volume to allow more solvent to pass through the

sample.

NOTE When using 100-mL cells, it may be necessary to

balance the number of static cycles and the rinse volume to prevent the collection bottle from being overfilled.

6. If analytes still appear in the extract from the second extract, make the adjustments listed below.

a. Run three static/rinse cycles. b. Raise the temperature again. c. Increase static time. d. Select a different solvent or consider additional pretreatment of the

sample, such as grinding or hydrolysis.

When target analytes no longer appear in the extract from the second extract, the method is complete for this sample type.

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ASE 150 Operator’s Manual

3.8 Performing Routine Maintenance

This section describes routine maintenance procedures that the user can perform. All other ASE 150 maintenance procedures must be performed by qualified Dionex personnel.

3.8.1 Daily Maintenance

• Check the gas supply to the instrument.

• Fill the solvent reservoir, if needed.

• Perform a rinse cycle. After filling the solvent reservoir, always run

two rinse cycles (see Section 3.5

• Empty the waste bottle, if needed.

• Check for leaks.

• Pull out the drip tray holder below the waste collection vessel

compartments (see Figure 2-1 remove it from the holder, dispose of the liquid, and reinstall the tray.

) to clear the solvent lines of air.

). If the drip tray contains liquid,

3.8.2 Periodic Maintenance

NOTE The EXTRACTION COUNTERS screen indicates the

number of extractions the ASE 150 has performed (see Section C.2.5

• Replace the PEEK seals (P/N 061687, pkg. of 50) inside the cell end

caps after approximately 50 extractions (see Section 5.2

• Replace the external O-rings (P/N 049457, pkg. of 50 Teflon O-rings;

P/N 056325, pkg. of 50 Viton O-rings) in the cell end caps and rinse cells after approximately 50 to 75 extractions (see Section 5.3 (Viton O-rings are for use in high temperature applications, such as dioxin extraction.)

• Verify that the tips of the three needles that extend from the bottom of

the needle mechanism are straight and not damaged or worn. To view the needles, open the collection vessel compartment door and toggle the needle switch to the

54 Doc. 065207-02 9/08

UP position (see Figure 3-10).

To replace the source needle, see Section 5.9. To replace the vent needles, contact Dionex.

• Approximately every 6 months, open the cell door and inspect the

upper and lower AutoSeal tips. If a tip is damaged or worn, it should be replaced. Contact Dionex for assistance.

• Replace the O-ring, filter, and seals in the static valve every 6 to

12 months (see Section 5.8

• Clean the exterior of the system with water and a mild detergent.

3.8.3 Annual Maintenance

• Dionex recommends performing preventive maintenance annually.

An ASE 150/ASE 350 Preventive Maintenance Kit (P/N 068954) is available.

• If you frequently extract an acidic or basic sample, consider having

the solvent lines replaced when the annual maintenance is performed. The solvent lines must be replaced by a qualified Dionex representative.

3 • Operation and Maintenance

3.9 Shutting Down

Overnight or Longer Shutdowns

• If acids, bases, salts, or buffers are used as extraction solvents, rinse the

system with 100% polar organic solvent (for example, acetone or methanol) or distilled water (see Section 3.5

• After extracting with a 100% organic solvent, you may turn off the power

immediately. If the shutdown is for more than one night, also turn off the gas supply.

Before Shipping the ASE 150

1. After extracting with a solvent that contains acids, bases, or other strong additive, rinse the system with either 100% organic solvent or distilled water (see Section 3.5

2. Empty the solvent reservoir, reconnect the reservoir to the system, and run one or more rinse cycles to remove solvent from the lines.

3. Turn off the gas supply, disconnect the gas source at the ASE 150 rear panel, and remove the solvent reservoir.

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) before turning off the power.

ASE 150 Operator’s Manual

56 Doc. 065207-02 9/08

This chapter is a guide to troubleshooting minor problems that may occur while operating the ASE 150 Accelerated Solvent Extractor.

• Section 4.1 describes error messages and how to troubleshoot them.

• The remaining sections in this chapter describe operating problems and how

to resolve them.

If you are unable to resolve a problem by following the instructions here, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office. Please have this chapter at hand when talking with Technical Support personnel.

4.1 Error Messages

The ASE 150 can identify several potential operating problems. If one of these problems occurs, an error message is displayed on the screen. The message remains until you press any button to clear it or until another error message appears.

4 • Troubleshooting

Each error message is identified by a number. This section lists the error messages and explains how to respond if an error occurs. Most problems can be resolved by the user.

Error 001

Cause:

Action:

Doc. 065207-02 9/08 57

Oven compression low.

Insufficient nitrogen gas pressure applied to the oven compression system during a run.

Check the REGULATORS screen (see Section C.2.3). When the oven is compressed, the

0.03 MPa (130 ± 5 psi). If the the gas pressure supplied to the ASE 150. It should be between 0.97 and 1.38 MPa (140 and 200 psi); 1.03 MPa (150 psi) is recommended. If necessary, replace the gas cylinder.

If the error message reappears, contact Dionex for assistance.

COMPRESSION field should read 0.90 ±

COMPRESSION field is low, check

ASE 150 Operator’s Manual

Error 002

Cause:

Action:

Error 003

Cause:

Action:

Error 004

Cause:

System pressure low.

Insufficient nitrogen gas pressure applied to the system.

Check the REGULATORS screen (see Section C.2.3). The SYSTEM field should read 0.34 ± 0.02 MPa (50 ± 3 psi). If the

SYSTEM field

is low, check the gas pressure supplied to the ASE 150. It should be between 0.97 and 1.38 MPa (140 and 200 psi); 1.03 MPa (150 psi) is recommended. If necessary, replace the gas cylinder.

If the error message reappears, contact Dionex for assistance.

Oven temperature low.

The heater cable connection to the power supply is loose, or a heater component malfunctioned.

Contact Dionex for assistance.

Oven temperature high

The heater cable connection to the power supply is loose, or a heater component malfunctioned.

Action:

Error 005

Cause:

Action:

Contact Dionex for assistance.

Cell pressure threshold exceeded.

A blockage in the system.

Run a rinse cycle (see Section 3.5). If the rinse runs without error, the sample cell may be plugged. Replace the cell filter (see

Action:

Section 3.1.4

(see Section 5.2

If the rinse has the same error, there may be a blockage in the solvent

). If the error still appears, clean or replace the cell frit

lines. Contact Dionex for assistance.

58 Doc. 065207-02 9/08

Error 006 Collection bottle full.

4 • Troubleshooting

Cause:

Action:

The collection vessel (bottle or vial) is full.

Install a new collection vessel and continue the run. When the run is complete, combine the extracts from both vessels. Reduce the rinse volume in the method before running again.

Cause:

Water vapors are condensing on the upper walls of the collection vessel.

Action:

Cause:

Change the solvent from 100% water to 1% MeOH, if possible.

A label or written information is blocking the area read by the collection vessel sensor.

Action:

Cause

Action:

Make sure the label is positioned correctly (see Figure 3-9).

Solvent is leaking into the collection vessel.

If solvent leaks into the collection vessel during the static cycle, the static valve seals are worn. Rebuild the static valve (see Section 5.8

Action:

Error 007 Collection bottle not detected.

Cause:

If the error message reappears, contact Dionex for assistance.

The collection vessel (bottle or vial) is not installed.

Action:

Error 008 Cell not detected.

Cause:

Install the collection vessel (with the cap screwed on) and toggle the needle switch to the

DOWN position (see Figure 3-10).

If the error message reappears, contact Dionex for assistance.

No sample cell or rinse cell is installed, or the sensor failed to detect the cell.

Action:

Install the appropriate cell (see Section 3.2.5). The installation procedure for sample cells and rinse cells is identical.

Action:

Doc. 065207-02 9/08 59

If the error message reappears, contact Dionex for assistance.

ASE 150 Operator’s Manual

Error 009 Pump volume limit exceeded.

Cause:

Action:

An empty (or incorrectly installed) solvent reservoir.

Refill the solvent reservoir, if necessary. Check that the solvent reservoir is correctly installed (see Section B.2.6

Cause:

Action:

A leak somewhere in the system.

Remove the right-side panel of the ASE 150 (see Section 5.4). Inspect the following fittings for leaks (see Figure 4-1 fittings, pump check valves, pressure transducer fittings, pressure relief valve fittings, static valve fittings, and solvent line fittings. Use a 1/4-inch open-end wrench (P/N 049452) to tighten any leaking fittings. Do not overtighten!

If tightening does not stop a leak, the tubing and fitting assembly must be replaced. Contact Dionex for assistance.

Action:

Pull out the drip tray holder below the oven and check the drip tray. If the tray contains liquid, remove it from the holder, dispose of the liquid, and reinstall the tray. Then, remove the collection vessel and waste bottle from the system. Remove the lower trim panel and check for leaks near the oven and the AutoSeal mechanism.

Error 010 Analog-to-digital converter failed.

Cause:

Failure of the main PC board (printed circuit board). The board must be replaced.

): pump

Action:

Contact Dionex for assistance.

60 Doc. 065207-02 9/08

Error 011 Solvent vapor threshold exceeded.

4 • Troubleshooting

Cause:

Action:

Cause:

Action:

Cause:

Action:

A leaking cell.

Check for foreign material on the threads of the cap, the seal surface, and the cell body. If necessary, replace the O-rings and/or seals (see

Section 5.2

Tighten the cell end caps hand-tight. Do not use a wrench or other

tool.

Incomplete purging of solvent from the cell during the purge cycle.

The optimal purge time varies, depending on the sample cell size (see

Table 3-1 )

. If you are running a preprogrammed method, create a custom method with the appropriate purge time. If you are already running a custom method, edit the method to increase the purge time. For instructions on editing a custom method, see Section 3.6

A leak somewhere in the system.

Remove the right-side panel of the ASE 150 (see Section 5.4). Inspect the following fittings for leaks (see Figure 4-1

): pump fittings, pump check valves, pressure transducer fittings, pressure relief valve fittings, static valve fittings, and solvent line fittings. Use a 1/4-inch open-end wrench (P/N 049452) to tighten any leaking fittings. Do not overtighten!

If tightening does not stop a leak, the tubing and fitting assembly must be replaced. Contact Dionex for assistance.

Action:

Error 012 Clamp plate temperature low.

Cause:

The heater cable connection to the power supply is loose, or a heater component malfunctioned.

Action:

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Contact Dionex for assistance.

ASE 150 Operator’s Manual

Error 013 Clamp plate temperature high.

Cause:

The heater cable connection to the power supply is loose, or a heater component malfunctioned.

Action:

Error 014 Oven unable to reach temperature.

Cause:

Contact Dionex for assistance.

Incorrect settings of the oven voltage switches on the ASE 150 rear panel.

Action:

Set both oven voltage switches to match the voltage from the power source at the installation site: either

Cause:

and 120 Vac) or details, see Section B.2.3

The heater cable connection to the power supply is loose, or a heater

220 (for voltages between 220 and 240 Vac). For

component malfunctioned.

Action:

Error 015 Unable to rinse.

Cause:

Contact Dionex for assistance.

The pump could not deliver the specified rinse volume within the allotted time. The cell or lines may be plugged.

110 (for voltages between 100

Action:

Run a rinse cycle (see Section 3.5). If the rinse runs without error, the sample cell may be plugged. Replace the cell filter (see

Action:

Section 3.1.4

If the rinse has the same error, there may be a blockage in the solvent

) and the cell frit (see Section 5.2).

lines. Contact Dionex for assistance.

62 Doc. 065207-02 9/08

Error 016 Unable to fill cell.

4 • Troubleshooting

Cause:

Action:

Cause:

Action:

Cause:

Action:

Cause:

Action:

An empty (or incorrectly installed) solvent reservoir.

Refill the solvent reservoir, if necessary. Check that the solvent reservoir is correctly installed (see Section B.2.6

A leaking static valve seal.

Check the collection vessel for liquid. If liquid is present, replace the static valve seals (see Section 5.8

A leaking fitting somewhere in the system.

Remove the right-side panel of the ASE 150 (see Section 5.4). Inspect the following fittings for leaks (see Figure 4-1

If tightening does not stop a leak, the tubing and fitting assembly must be replaced. Contact Dionex for assistance.

A leaking check valve (internally).

Replace both check valve cartridges (see Section 5.5).

Error 017 Remove cell during oven wait period.

Cause:

A sample cell was installed in the cell holder before the temperature set point was reached.

Action:

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Remove the cell from the cell holder. Never install the cell until the

STATUS field (on the STATUS screen) indicates OVEN READY and

the LED on the front panel

Section 3.2.4

START button is flashing. For details, see

ASE 150 Operator’s Manual

Error 018 Oven heater AC line voltage too high.

Cause:

Incorrect settings of the oven voltage switches on the ASE 150 rear panel.

Action:

Set both oven voltage switches to match the voltage from the power source at the installation site: either

Action:

and 120 Vac) or details, see Section B.2.3

If selecting the correct switch settings does not correct the problem,

220 (for voltages between 220 and 240 Vac). For

contact Dionex for assistance.

Error 020 Oven heater malfunction.

Cause:

Incorrect settings of the oven voltage switches on the ASE 150 rear panel.

Action:

Set both oven voltage switches to match the voltage from the power source at the installation site: either

Action:

and 120 Vac) or details, see Section B.2.3

If selecting the correct switch settings does not correct the problem,

220 (for voltages between 220 and 240 Vac). For

contact Dionex for assistance.

110 (for voltages between 100

Error 021 Top plate heater AC line voltage too high.

Cause:

Incorrect settings of the oven voltage switches on the ASE 150 rear panel.

Action:

Set both oven voltage switches to match the voltage from the power source at the installation site: either and 120 Vac) or details, see Section B.2.3

220 (for voltages between 220 and 240 Vac). For

110 (for voltages between 100

If selecting the correct switch settings does not correct the problem, contact Dionex for assistance.

64 Doc. 065207-02 9/08

Error 023 Top plate heater malfunction.

4 • Troubleshooting

Cause:

Action:

Error 024 Cell size wrong.

Cause:

Action:

Incorrect settings of the oven voltage switches on the ASE 150 rear panel.

Set both oven voltage switches to match the voltage from the power source at the installation site: either and 120 Vac) or details, see Section B.2.3

If selecting the correct switch settings does not correct the problem, contact Dionex for assistance.

The cell type specified in the method is zirconium, but the cell size specified on the are available only in 66 mL or 100 mL sizes.)

Select the correct cell size on the SETUP screen (see Section C.1.3) or, if you are using a stainless steel cell and the cell size is correct, change the cell type on the

4.2 Liquid Leaks

110 (for voltages between 100

220 (for voltages between 220 and 240 Vac). For

SETUP screen is less than 66 mL. (Zirconium cells

METHOD screen (see Section C.1.4).

• Worn-out seal in sample cell end cap

Replace the seal (see Section 5.2

• Missing or worn-out cell O-rings

Check the ends of the cell to verify that the O-rings are in place and in good condition. If any O-ring has a hole size of less than 0.5 mm, replace it. If a white Teflon O-ring is discolored, replace it (see Section 5.3

O-rings should last for approximately 50 extractions. To view the number of extractions the ASE 150 has performed, go to the screen (see Section C.2.5

EXTRACTION COUNTERS

• Leak in solvent flow path

Remove the right-side panel of the ASE 150 (see Section 5.4 following fittings for leaks (see Figure 4-1

Doc. 065207-02 9/08 65

): pump check valves, pressure

). Inspect the

ASE 150 Operator’s Manual

transducer fittings, pressure relief valve fittings, static valve fittings, and solvent line fittings. Use a 1/4-inch open-end wrench (P/N 049452) to tighten any leaking fittings. Do not overtighten!

If tightening does not stop a leak, the tubing and fitting assembly must be replaced. Contact Dionex for assistance.

If the pump head is leaking, replace the pump seals (see Section 5.6

Rear Panel

Solvent

Bottle

Oven

Sample Cell

Purge

Valve

Pressure

Relief

Valve

Static Valve

Prime Valve

Pump Outlet

Nitrogen In

Vent

Pump

Pressure

Waste Bottle

Front Components Right-Side Components

Collection

Vessel

Transducer

Check

Valve

Pump Inlet

= Gas Lines = Solvent Line

Figure 4-1. ASE 150 Plumbing Diagram

66 Doc. 065207-02 9/08

• Leaking into waste bottle during static cycle

If liquid drips into the waste bottle when the cell is under pressure and the static valve is closed, the pressure relief valve is worn and must be replaced (see Section 5.7

• Leaking into collection vessel during static cycle

If solvent leaks into the collection vessel during the static cycle, the static valve seals are worn and the valve must be rebuilt (see Section 5.8

4.3 Gas Leaks

Gas leaks are usually audible. In addition, excessive gas consumption often indicates a gas leak.

If you suspect a leak, check the following locations: gas supply, rear panel, solvent reservoir, and interior connections. Listen for leaks and run your hand over the area to feel for escaping gas.

If you find a loose connection, push the tubing firmly onto its fitting. If the fitting or tubing continues to leak, replace it.

4 • Troubleshooting

4.4 Stopped System

• Electrical cables improperly installed

Remove the right-side panel of the ASE 150 (see Section 5.4 electrical cables are seated properly in their connectors on the main PC board (printed circuit board).

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). Check that all

ASE 150 Operator’s Manual

68 Doc. 065207-02 9/08

5•Service

This chapter describes ASE 150 Accelerated Solvent Extractor service and repair procedures that users may perform. All procedures not included here, including electronics-related repair procedures, must be performed by Dionex personnel. For assistance, contact Dionex Technical Support. In the U.S., call 1-800-346-

6390. Outside the U.S., call the nearest Dionex office. Before replacing any part, refer to the troubleshooting information in Chapter 4

correctly identify the cause of the problem.

Substituting non-Dionex parts (extraction cells, extraction cell components, valves, etc.) may impair the performance of the ASE 150, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information.

5.1 Replacing Tubing and Fittings

Use a 1/4-inch open-end wrench (P/N 049452) to tighten any leaking fittings. Do not overtighten!

If tightening a fitting does not stop a leak, the tubing and fitting assembly must be replaced. Contact Dionex for assistance.

5.2 Replacing the Cell End Cap Seal

A worn PEEK seal is deeply grooved and will fail to form a tight seal between the cell cap and body during a run, causing leaks.

1. Unscrew the cell end cap from the cell body (see Figure 5-1

Wear safety glasses when removing the old snap ring from the cell end cap or installing a new snap ring.

Le port de lunettes de sécurité est requis lors du changement de l’anneau de serrage sur le bouchon des cellules d’extraction.

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ASE 150 Operator’s Manual

Tragen Sie eine Schutzbrille, wenn Sie den alten Sicherungsring von der Verschlusskappe der Zelle entfernen oder wenn Sie einen neuen Sicherungsring installieren.

Do not disassemble the cell end cap after each use. This can cause the seal to fail prematurely.

2. Remove the snap ring from the end cap, using the snap ring tool (P/N 056684) provided in the ASE 150 Ship Kit (P/N 066399).

a. Insert the pointed ends of the tool into the

two holes in the snap ring (see Figure 5-1

b. Squeeze the handles of the tool together to

reduce the diameter of the ring. At the same time, carefully pull the ring out of the cap.

c. Carefully release the handles of the tool

and remove the ring from the tool.

NOTE The procedure for stainless steel

and zirconium caps is identical. The photos show a stainless steel cap.

3. Remove the cap insert (see Figure 5-2

). Remove the PEEK seal from the groove in the bottom of the cap insert.

4. Remove the frit from the bottom of the end cap.

5. Clean the frit by sonicating it in solvent (or replace it).

Snap Ring

Too l

Cell End Cap

Figure 5-1. Removing the Snap Ring

Snap Ring

Cap Insert

Seal

Frit

Cell End Cap

Figure 5-2. Cell End Cap Disassembled

70 Doc. 065207-02 9/08

5•Service

6. Refer to Figure 5-3 and the following steps to reassemble the sample cell. a. Place the new or cleaned frit into the bottom of the end cap. b. Press a new PEEK seal (P/N 061687, pkg. 50) into the bottom of the cap

insert.

c. Align the pins in the cap insert with the grooves in the end cap and then

place the insert, with the seal facing down, into the end cap.

7. With the cap assembly upright on the workbench, install the snap ring: a. Insert the snap ring tool into the holes on the ring. b. Squeeze the tool handles to bring the ends of the ring together. c. Insert the ring into the cap. Using your fingers, push the ring under the lip

of the end cap. After verifying that the entire ring is under the lip, release the tension on the tool and remove the tool from the ring.

d. Screw the cap back onto the cell body and hand-tighten.

Cell Body

Snap Ring

Cap Insert

Cell End Cap Assembly

Figure 5-3. Sample Cell Assembly

Doc. 065207-02 9/08 71

Seal

Frit

End Cap

O-Ring

ASE 150 Operator’s Manual

5.3 Replacing the Cell End Cap O-Ring

1. Locate the small flathead screwdriver (P/N 046985) and the O-ring insertion tool (P/N/ 049660) in the ASE 150 Ship Kit (P/N 066399).

2. Insert the tip of the screwdriver into the end cap and carefully pick out the Oring. (This may be easier to do if you first remove the cap from the cell body and place it flat on the workbench.)

3. Place a new O-ring (Teflon, P/N 049457, pkg. of 50; Viton, P/N 056325, pkg. of 50) over the opening in the end of the cell end cap. Press the O-ring into place, using the O-ring insertion tool (see Figure 5-4

O-Ring Insertion Tool (P/N 049660)

Place O-ring in opening and press into place with insertion tool.

Figure 5-4. Installing the Cell O-Ring

72 Doc. 065207-02 9/08

5.4 Removing the Right-Side Panel

Several parts that the user can service are located behind the panel on the right side of the ASE 150.

Removing the Right-Side Panel

1. Make sure the ASE 150 power is turned on and the gas supply is on. (This ensures that the AutoSeal mechanism is lowered.)

5•Service

2. Toggle the needle switch to the

UP position. If a collection vessel is installed,

remove the vessel from the holder and set it aside.

3. Turn off the gas supply. Disconnect the gas source at the ASE 150 rear panel and let the system vent.

4. Turn off the ASE 150 main power switch.

5. Unscrew the waste bottle and remove the bottle from the compartment.

6. Close the waste bottle and collection vessel compartment doors.

7. Remove the lower front trim panel of the ASE 150: a. Slide the drip tray out about halfway. b. Place your fingers in the indentations on both sides of the lower front trim

panel and pull the panel toward you to remove it (see Figure 5-5

Figure 5-5. Removing the Lower Front Trim Panel

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ASE 150 Operator’s Manual

8. Using a #2 Phillips screwdriver, remove the two screws on the right side of the inner front panel. One screw is at the top right corner; the other is at the bottom right corner (see Figure 5-6

Figure 5-6. Inner Front Panel

Remove this screw

Opening for screwdriver

Remove this screw

9. Insert a screwdriver into the opening located beneath the top screw hole (see

Figure 5-6

). Push the screwdriver in until the right-side panel slides back

about 1/2 inch. To prevent scratches or other damage to the panel, do not

let the panel fall onto the workbench.

10. Remove the right-side panel from the system and set it aside.

Reinstalling the Right-Side Panel

1. Hold the panel against the right side of the system. Engage the small tabs on the top and bottom of the panel with the slots in the chassis. Pull the panel forward until it locks into place.

2. Replace the two Phillips screws on the inner front panel.

3. Slide the drip tray out about halfway.

4. Carefully align the lower trim panel with the edges of the instrument, and then gently push the panel into place.

5. Reinstall the waste bottle and collection vessel.

6. Reconnect the gas source and turn on the gas supply.

7. Turn on the ASE 150 main power switch.

74 Doc. 065207-02 9/08

5.5 Replacing Pump Check Valve Cartridges

5.5.1 Before Beginning

Disconnect the solvent reservoir and remove it from the top of the ASE

150. Run a rinse cycle (see Section 3.5 solvent when the inlet tubing is disconnected.

5.5.2 Removing the Pump

1. Follow the instructions in Section 5.4 to disconnect the gas source and remove the right-side panel. The ASE 150 pump is behind the right-side panel in the lower right corner (see Figure 5-7

). This prevents siphoning of

5•Service

Press Fittings

Outlet Check

Valve Inlet Check

Valve Pump PC

Board Cable

Mounting Screws

Figure 5-7. ASE 150 Pump (Behind Right-Side Panel)

2. Disconnect the red tubing and the transparent blue tubing from the two black elbow press fittings ( ) on top of the pump.

To disconnect a press fitting, use your fingers (or a small open-end wrench) to press the ring on the fitting in, while at the same time pulling the tubing out.

3. Use a 1/4-inch open-end wrench to disconnect the stainless steel fitting from the outlet check valve ( ).

4. By hand, disconnect the PEEK fitting from the inlet check valve ( ).

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ASE 150 Operator’s Manual

5. Disconnect the gray cable from the pump PC board ( ).

6. Use a 3-mm hex screwdriver (P/N 060154) to remove the screws in the left and right end plates ( ) on the pump. These screws secure

the pump to the component panel.

5.5.3 Removing the Check Valves and Cartridges

1. Use a 1/2-inch open-end wrench to loosen the inlet check valve housing. Remove the housing and then remove the check valve cartridge from the housing (see Figure 5-8

Inlet Check

Valve Cartridge

Inlet Check

Valve Housing

Figure 5-8. Disassembled ASE 150 Pump Inlet Check Valve

2. Turn the pump over, so that the outlet check valve is facing down.

3. Use a 1/2-inch open-end wrench to loosen the outlet check valve housing. Remove the housing and then remove the check valve cartridge from the housing.

NOTE The housing for the inlet check

valve assembly has a 1/4-28 port. The housing for the outlet check valve assembly has a 1032 port (see Figure 5-9

76 Doc. 065207-02 9/08

Inlet Check Valve:

1/4-28 Port

Outlet Check Valve

10-32 Port

Figure 5-9. Check Valve Housings

5.5.4 Installing New Check Valve Cartridges

1. Install the new inlet cartridge (P/N 047755) in the inlet

Double-hole

check valve housing so that the double-hole end of the cartridge is visible (see

Figure 5-10

2. Install the new outlet cartridge (P/N 057346) in the outlet check valve housing so that

Inlet

Check

Valve

Flow

the arrow on the cartridge points down.

Figure 5-10. Check Valve Assemblies

5.5.5 Reinstalling the Check Valves

1. Install the inlet check valve assembly on the bottom of the pump head.

5•Service

Flow

Outlet Check

Valve

2. Install the outlet check valve assembly on the top of the pump head.

3. Tighten the check valves fingertight, and then use a wrench to tighten an additional one-quarter to one-third turn.

Overtightening may damage the pump head and check valve housing and crush the check valve seats.

5.5.6 Cleaning the Check Valves

Clean the check valves if new check valves are unavailable.

1. Place the check valve housings and cartridges in a beaker with methanol. Sonicate or agitate for several minutes.

2. Rinse each check valve housing and cartridge thoroughly with filtered, deionized water.

3. Reinstall the check valves on the pump.

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ASE 150 Operator’s Manual

5.5.7 Reinstalling the Pump

1. Reinstall the pump on the component panel.

2. Reconnect the red gas line to the left press fitting on top of the pump. Reconnect the transparent blue gas line to the right press fitting.

3. Reconnect the solvent lines to the inlet and outlet check valve housings.

4. Reconnect the cable to the pump PC board.

5.5.8 Completing the Procedure

1. Follow the instructions on page 74 to reinstall the right-side panel.

2. Reconnect the gas source at the ASE 150 rear panel and turn on the gas supply.

3. Turn on the ASE 150 main power switch.

4. Rinse the system (see Section 3.5 normal.

) and check that the pump flow is

78 Doc. 065207-02 9/08

5.6 Replacing Pump Seals

5.6.1 Before Beginning

Disconnect the solvent reservoir and remove it from the top of the ASE

150. Run a rinse cycle (see Section 3.5 solvent when the inlet tubing is disconnected.

5.6.2 Removing the Pump

Follow the instructions in “Removing the Pump” on page 75.

5.6.3 Replacing the Piston High-Pressure Seal

1. Use a 3-mm hex driver (P/N 060154) or wrench to loosen and remove the two screws securing the pump head to the body.

5•Service

). This prevents siphoning of

2. Slide the pump head straight off the pump (see Figure 5-11

Lateral motion while disengaging the pump head from the pump may break the piston.

Figure 5-11. Removing the Pump Head

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ASE 150 Operator’s Manual

3. Turn the pump head over so that the open end is down. The tan piston guide (see Figure 5-12 gently tap the head on the workbench to dislodge the guide. Save the piston guide (it will be reinstalled in Step 7

High-Pressure

Figure 5-12. Replacing the ASE 150 Piston High-Pressure Seal

4. If tapping the head on the bench does not remove the piston guide, use the wooden end of a cotton-tipped swab to pry the guide out of the pump head. Discard the used piston guide.

) should drop out of the head; if it does not,

Piston Guide

Seal

5. To remove the orange high-pressure seal from the pump head, insert the wooden end of a cotton-tipped swab and pry out the seal. Discard the seal.

Do not use a sharp tool (such as tweezers) to remove or install the high-pressure piston seal. This will scratch the seal and the inside of the pump housing; these scratches will prevent a proper seal and allow leakage.

6. Hold the new high-pressure seal (P/N 066162), with the smaller diameter (ringed) side of the seal facing down, and drop it into the pump head cavity.

7. If the piston guide was easily removed from the pump head (Step 3

), place the original piston guide on top of the highpressure seal and firmly press it into place. This also seats the highpressure seal in the pump head.

80 Doc. 065207-02 9/08

If you had to pry the piston guide out of the pump head (Step 4), install a new piston guide (P/N 066109) as described above. The original piston guide may have been scratched during removal, so do not use it again. A scratched guide will not seal properly.

8. Reinstall the pump head onto the pump

5.6.4 Replacing the Piston Air Seal

1. Remove the PC board from the side of the pump (see Figure 5-13, view A).

2. Loosen the two bolts that hold the two end plates together (see

Figure 5-13

, view B).

5•Service

Figure 5-13. Removing the Pump PC Board and End Plate Bolts

Pump End Plate

3. Remove the right end plate from the pump cylinder (see Figure 5-14

Right End Plate

Pump Cylinder

Figure 5-14. Removing the Pump Right End Plate

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ASE 150 Operator’s Manual

4. Remove the left end plate from the cylinder, exposing the piston (see

Figure 5-15

Figure 5-15. Removing the Pump Left End Plate

Piston

Left End Plate

5. To remove the piston air seal from the left end plate (see Figure 5-16 insert the wooden end of a cotton-tipped swab and pry out the seal. Discard the seal.

Do not use a sharp tool (such as tweezers) to remove or install the piston air seal. This will scratch the seal and the inside of the pump housing; these scratches will prevent a proper seal and allow leakage.

Left End Plate

Piston Air Seal

Piston

Figure 5-16. Removing the Piston Air Seal

6. Insert the new piston air seal (P/N 066163), with the closed end facing down, into the end plate. Gently press the seal into place with a cotton-tipped swab (or other tool with a soft tip).

82 Doc. 065207-02 9/08

5•Service

7. Gently insert the piston into the new seal in the left end plate. Push the pump cylinder over the O-ring on the left end plate. Push the pump cylinder over the O-ring on the right end plate.

8. Loosely secure the end plates together with the two bolts removed previously.

9. Place the assembled pump on a flat surface. Make sure all four alignment marks on the pump cylinder and end plates are aligned (see

Figure 5-17

other. The pump should sit evenly on the flat surface without rocking.

). Press down on the end plates to square them with each

Figure 5-17. Alignment Marks on Pump Cylinder and End Plates

10. Tighten the two bolts evenly.

11. Reattach the PC board to the side of the pump.

5.6.5 Reinstalling the Pump and Completing the Procedure

1. Reinstall the pump on the component panel.

2. Reconnect the red gas line to the left press fitting on top of the pump. Reconnect the transparent blue gas line to the right press fitting.

3. Connect the solvent lines to the inlet and outlet check valve housings.

4. Reconnect the cable to the PC board.

5. Follow the instructions on page 74

6. Reconnect the gas source at the ASE 150 rear panel and turn on the gas supply.

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to reinstall the right-side panel.

ASE 150 Operator’s Manual

7. Turn on the ASE 150 main power switch.

8. Reset the screen (see Section C.2.5

PUMP STROKE counter on the EXTRACTION COUNTERS

5.7 Replacing the Pressure Relief Valve

1. Follow the instructions in Section 5.4 to disconnect the gas source and remove the right-side panel.

2. The pressure relief valve is installed in the upper left corner of the component panel (see Figure 5-18 elbow press fitting on the valve.

To disconnect a press fitting, use your fingers (or a small open-end wrench) to press the ring on the fitting in, while at the same time pulling the tubing out.

3. Use a 1/4-inch open-end wrench to disconnect the stainless steel line ( ) from the right side of the valve. (This tubing connects to the pump transducer.)

4. Use the wrench to disconnect the Hastelloy® line ( ) from the left side of the valve. (This tubing connects to the upper AutoSeal tip.)

11 22

, ). Disconnect the yellow gas tubing ( ) from the

Pressure Relief Valve

Yellow Gas Tubing

Stainless Steel Line

Hastelloy Line

Green PEEK Waste Line

Allen Hex Screw

Splash Guard

Figure 5-18. Connections to the Pressure Relief Valve

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5•Service

5. Use the wrench to disconnect the green PEEK waste line ( ) from the top of the valve.

6. Use a 9/64-inch Allen wrench to loosen the hex screw on the clamp ring

below the valve base ( ).

7. Lift the old valve off the valve base.

8. Remove the splash guard ( ) on the old valve by removing the two Phillips

screws on the valve.

9. Attach the splash guard to the new pressure relief valve (P/N 048889).

10. Lower the new pressure relief valve onto the valve base. Tighten the Allen hex screw on the clamp ring.

11. Reconnect all of the lines.

12. Follow the instructions on page 74

to reinstall the right-side panel.

13. Turn on the ASE 150 main power switch.

14. Reconnect the gas source at the ASE 150 rear panel and turn on the gas supply.

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ASE 150 Operator’s Manual

5.8 Rebuilding the Static Valve

Leaking from the source needle into the collection vessel during the static cycle indicates that the static valve is worn and must be rebuilt. The rebuild procedure consists of replacing a few parts (an O-ring, a filter, and two seals) and then cleaning the inside of the valve body.

Before proceeding, check that the following kits are on hand. The kits contain the replacement parts and special tools required to rebuild the valve.

• Order a Static Valve Repair Kit (P/N 068115) each time the valve requires

rebuilding.

Part Number Item Quantity

065254 ASE 150/ASE 350 Static Valve Repair

Kit Instructions

066165 High-pressure flangeless seal 2 067326 Perlast® O-ring 1 067327 Zirconium filter 1

Table 5-1. Static Valve Repair Kit Contents

• Order a Static Valve Tool Kit (P/N 068116) only the first time the valve

requires rebuilding. Figure 5-19

Part Number Static Valve Tool Quantity

049293 Tubing, orange (extension tubing) 60.96 cm (24 in) 057395 Union (for extension tubing) 1 067394 Piston-side seal insertion tool 1 067395 Inlet-side seal insertion tool 1 068117 Alignment tool 1 068118 Spacer tool 1 068119 Push screw tool 1 068245 Seal removal tool 1

Table 5-2. Static Valve Tool Kit Contents

illustrates each tool.

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Piston-Side Seal

Insertion Tool

(P/N 067394)

Spacer Tool

(P/N 068118)

Inlet-Side Seal

Insertion Tool

(P/N 067395)

Seal Removal Tool

(P/N 068245)

Alignment Tool (P/N 068117) and

Push Screw Tool (P/N 068119)

Figure 5-19. Static Valve Tools

Additional Required Items

• #2 Phillips screwdriver

• 1/4-inch open-end wrench (P/N 049452); provided in the ASE 150 Ship Kit

(P/N 066399)

• 2.5-mm hex wrench

• 5/8-in open-end wrench or socket

• Large flathead screwdriver

• Cotton-tipped swabs (or other tool with a soft tip)

• Isopropyl alcohol (IPA) or acetone

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ASE 150 Operator’s Manual

5.8.1 Removing the Static Valve from the System

1. Turn off the ASE 150 main power switch.

2. Follow the instructions in Section 5.4

to disconnect the gas source

and remove the right-side panel. The static valve is installed on the lower left side of the component

panel, below the pressure relief valve (see Figure 5-20

1 4

Lines (2)

Dark Yellow

Orange Tubing

Figure 5-20. Removing the Static Valve

Mounting Screws (4)Hastelloy

3. Using a 1/4-inch open-end wrench, disconnect the two Hastelloy fluid

lines from the valve .

4. Disconnect the dark yellow and orange tubing from the press

fittings on the valve. To disconnect a press fitting, use your fingers (or a small open-end

wrench) to press the ring on the fitting in, while at the same time pulling the tubing out.

5. Using a 2.5-mm hex wrench, remove the four screws that secure

the static valve to the ASE 150.

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5•Service

6. Remove the static valve assembly from the system and place it on the workbench (see Figure 5-21

Figure 5-21. Static Valve

7. Using a 2.5-mm hex wrench, remove the two mounting screws that secure

Mounting Screws

the valve body to the base plate of the valve assembly.

Valve Body

8. Follow these steps to remove the piston from the static valve: a. Locate the slot in the piston

holder. If necessary, rotate the piston holder so that the opening

Piston

Holder

Piston

in the slot faces up.

b. Guide the piston out of the

piston holder by lifting the valve body straight up. This removes both the piston and the valve body. Do not drop the piston.

Dropping the piston may cause scratches or breakage. If the piston is damaged, it cannot be used again and must be replaced.

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ASE 150 Operator’s Manual

c. Pull the piston out of the valve body and place it in a secure

location.

5.8.2 Disassembling the Static Valve Body

1. Remove the nut installed in each side of the valve body: a. Using a 5/8-in open-end wrench

or socket, remove the nut on the inlet side of the valve body.

b. Remove the seal backup ring

and the filter from the inlet side (they may fall out on their own). Save the seal backup ring. You can discard the filter.

c. Using a large flathead

screwdriver, remove the nut on the piston side of the valve body.

Inlet-Side

Nut

Seal

Backup

Ring

Filter

Piston-

Side Nut

Do not use a sharp object inside the valve body. Any scratches on the valve body will prevent a proper seal and allow leakage.

90 Doc. 065207-02 9/08

2. Insert the flat end of the seal removal tool (P/N 068245) into the piston side of the valve body and push the inlet-side seal out of the valve body.

3. Pull the seal removal tool out of the valve body.

4. Insert the flat end of the seal removal tool into the inlet side of the valve body and push the seal out of the piston side of the valve body.

5•Service

Flat End of Seal Removal Too l

Inlet-Side Seal

Piston-Side Seal

5. Insert the pointed end of the seal removal tool into the valve body. Slide the tool between the valve body and O-ring and pull the O-ring out of the valve body.

6. Using a cotton-tipped swab (or other tool with a soft tip), thoroughly clean the inside of the valve body. If necessary, moisten the area with IPA (isopropyl alcohol) or acetone to remove all debris, sediment, and precipitates.

Do not use a sharp object to clean the inside of the valve body. Any scratches on the valve body will prevent a proper seal and cause leakage.

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ASE 150 Operator’s Manual

5.8.3 Installing the New Seals

1. Push the piston through the pistonside seal insertion tool (P/N 067394).

2. Wet a new seal (P/N 066165) with IPA (isopropyl alcohol) for lubrication.

3. Note that one side of the seal is flat, while the other side contains an Oring. Orient the O-ring side of the seal so that it faces away from the tool, and then slide the seal onto the piston.

4. Place the valve body, with the piston side (small opening) facing up, on the workbench.

5. Rest your thumbs on the back of the tool and press down firmly (with equal pressure) on the left and right sides of the tool. You should hear a snap as the new seal is seated in the valve body. Remove the piston and the tool from the valve body.

Piston-Side Seal

Insertion Tool

Piston-Side Seal

Insertion Tool

Seal

Piston

Seal O-Ring

Piston

NOTE: If there is no audible snap, check the seal for damage. An undamaged seal will lie completely flat in the valve body, with no visible edges. If the seal is damaged, remove it from the valve body. Contact Dionex to order a replacement seal.

Do not use a sharp object inside the valve body. Any scratches on the valve body will prevent a proper seal and allow leakage.

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Dionex ASE 150 Operator's Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1.1 Overview

1.2 About This Manual

1.2.1 Overview

1.2.2 Safety Messages and Notes

1.3 Safety and Regulatory Information

1.4 Safety Labels

2.1 Operating Features

2.1.1 Control Panel

2.1.2 Sample Cells and Rinse Cells

2.1.3 Collection Vessels

2.1.4 Solvent Reservoir

2.1.5 Waste Bottle

2.2 Rear Panel

2.3 ASE 150 Extraction Process

2.4 Method Control

2.5 Preprogrammed Methods

3.1 Preparing to Run

3.1.1 Selecting and Preparing Solvent

3.1.2 Filling the Solvent Reservoir

3.1.3 Preparing the Sample

3.1.4 Installing the Cell Filter

3.1.5 Filling the Cell

3.1.6 Installing the Collection Vessel

3.1.7 Installing the Waste Bottle

3.2 Running

3.2.1 Selecting the Method

3.2.2 Selecting the Cell Size

3.2.3 Verifying the Cell Type

3.2.4 Starting the Run and Checking the Oven Status

3.2.5 Installing the Sample Cell in the Cell Holder

3.2.6 Completing the Run

3.3 Performing Post-Run Procedures

3.3.1 Cleaning the Sample Cells

3.3.2 Processing Extracts

3.4 Stopping a Run

3.5 Rinsing/Priming the System

3.6 Editing a Custom Method (Methods 1 through 24)

3.7 Developing a New Method

3.8 Performing Routine Maintenance

3.8.1 Daily Maintenance

3.8.2 Periodic Maintenance

3.8.3 Annual Maintenance

3.9 Shutting Down

4.1 Error Messages

4.2 Liquid Leaks

4.3 Gas Leaks

4.4 Stopped System

5.1 Replacing Tubing and Fittings

5.2 Replacing the Cell End Cap Seal

5.3 Replacing the Cell End Cap O-Ring

5.4 Removing the Right-Side Panel

5.5 Replacing Pump Check Valve Cartridges

5.5.1 Before Beginning

5.5.2 Removing the Pump

5.5.3 Removing the Check Valves and Cartridges

5.5.4 Installing New Check Valve Cartridges

5.5.5 Reinstalling the Check Valves

5.5.6 Cleaning the Check Valves

5.5.7 Reinstalling the Pump

5.5.8 Completing the Procedure

5.6 Replacing Pump Seals

5.6.1 Before Beginning

5.6.2 Removing the Pump

5.6.3 Replacing the Piston High-Pressure Seal

5.6.4 Replacing the Piston Air Seal

5.6.5 Reinstalling the Pump and Completing the Procedure

5.7 Replacing the Pressure Relief Valve

5.8 Rebuilding the Static Valve

5.8.1 Removing the Static Valve from the System

5.8.2 Disassembling the Static Valve Body

5.8.3 Installing the New Seals