Dionex ASE 100 Operator's Manual

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ASE 100

ACCELERATED SOLVENT EXTRACTOR

OPERATOR'S MANUAL

Document No. 031842

Revision 01

May 2002

Page 2

This publication is protected by federal copyright law. No part of this publication may be copied or distributed, transm itted, tr anscri bed , 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 REGA RDIN G TH E USE, OR T HE R ESULTS OF THE USE, OF THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY, RELIABILITY, CURRENTNES S, 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 and ASE® 100 is a registered trademark of Dionex Corporati on.

Teflon Company.

and Viton® are registered trademarks of E. I. duPont de Nemours &

PRINTING HISTORY

Revision 01, May 2002

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1 • Introduction

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

1.2 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-3

1.2.1 Typefaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4

1.2.2 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . .1-4

1.3 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .1-6

2 • Description

2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-1

2.1.1 Control Panel Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-3

2.1.2 Control Panel Keypad . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-4

2.2 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-9

2.3 Extraction Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-11

2.4 Method Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-13

2.5 Preprogrammed Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-14

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2.1.3 Extraction Cells and Rinse Cells . . . . . . . . . . . . . . . . . . . . . . .2-6

2.1.4 Collection Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-7

2.1.5 Solvent Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-8

2.1.6 Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2-9

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ASE 100 Accelerated Solvent Extractor

3 • Operation and Maintenance

3.1 Preparing to Run an Extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.1 Selecting and Preparing Solvent . . . . . . . . . . . . . . . . . . . . . . . 3-1

3.1.2 Filling the Solvent Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-3

3.1.3 Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5

3.1.4 Installing the Cell Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-7

3.1.5 Filling the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9

3.1.6 Installing the Collection Bottle . . . . . . . . . . . . . . . . . . . . . . . 3-11

3.1.7 Rinsing/Priming the System . . . . . . . . . . . . . . . . . . . . . . . . . 3-12

3.2 Editing a Custom Method (1–24) . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13

3.3 Guidelines for Method Development . . . . . . . . . . . . . . . . . . . . . . . . . 3-17

3.4 Running an Extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-20

3.5 Post-Extraction Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .3-24

3.5.1 Cleaning the Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24

3.5.2 Processing Extracts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24

3.6 Aborting a Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25

3.7 Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-26

3.7.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-26

3.7.2 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-26

3.8 Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27

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4 • Troubleshooting

4.1 Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-1

4.2 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-8

4.3 Gas Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-10

4.4 System Stops . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4-10

5•Service

5.1 Replacing the Seal in the Cell End Cap . . . . . . . . . . . . . . . . . . . . . . . . .5-2

5.2 Replacing the Cell O-Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-4

5.3 Removing the Right Side Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-5

5.4 Cleaning and/or Replacing Pump Check Valves . . . . . . . . . . . . . . . . . .5-8

Contents

5.4.1 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-8

5.4.2 Removing the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . .5-10

5.4.3 Cleaning the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . .5-10

5.4.4 Reinstalling the Inlet Check Valve . . . . . . . . . . . . . . . . . . . . .5-10

5.4.5 Reinstalling the Outlet Check Valve . . . . . . . . . . . . . . . . . . .5-11

5.4.6 Reinstalling the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-11

5.4.7 Completing the Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . .5-11

5.5 Replacing the Piston Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-12

5.5.1 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-12

5.5.2 Replacing the Piston Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-13

5.5.3 Reinstalling the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-14

5.5.4 Completing the Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . .5-14

5.6 Replacing the Relief Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5-15

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ASE 100 Accelerated Solvent Extractor

5.7 Replacing the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18

5.8 Replacing the Source Needle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20

5.9 Replacing the Solvent Outlet Line . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23

5.10 Replacing the Lower AutoSeal Tip . . . . . . . . . . . . . . . . . . . . . . . . . . 5-29

5.11 Replacing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34

A • Specifications

A.1 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1

A.2 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1

A.3 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-1

A.4 Pneumatic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2

A.5 Front Panel Display and Keypad . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2

A.6 Extraction Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2

A.7 Collection Bottles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2

A.8 Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .A-2

B • Installation

B.1 Facility Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-1

B.2 Installation Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-2

B.2.1 Nitrogen Connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-2

B.2.2 Electrical Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-4

B.2.3 Checking Pressure Readings . . . . . . . . . . . . . . . . . . . . . . . . . .B-6

B.2.4 Solvent Bottle Connections . . . . . . . . . . . . . . . . . . . . . . . . . . .B-8

B.2.5 Waste Bottle Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . .B-10

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B.2.6 Rinsing the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-11

B.2.7 Adjusting the Cell Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . B-13

B.2.8 Inspecting the Cell. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-15

B.2.9 Completing the Installation. . . . . . . . . . . . . . . . . . . . . . . . . . B-16

C • User Interface

C.1 Operational Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2

C.1.1 Main Screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2

C.1.2 Status Screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3

C.1.3 Setup Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-4

C.1.4 Method Editor Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-7

C.2 Diagnostic Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-9

Contents

C.2.1 Diagnostics Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-9

C.2.2 Sensors Screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-10

C.2.3 Regulators Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-11

C.2.4 Hydrocarbon Sensor Screen . . . . . . . . . . . . . . . . . . . . . . . . . C-12

C.2.5 Extraction Counters Screen . . . . . . . . . . . . . . . . . . . . . . . . . . C-13

C.2.6 Moduleware Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-14

D • Reordering Information

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ASE 100 Accelerated Solvent Extractor

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1.1 Overview

The ASE organic o r ino rganic compounds from a varie ty of solid and/or semiso li d sampl es . The ASE 100 accelerates the traditional extraction process by using solvent at elevated temperatures and pressures. Pressure is applied to the sample extraction cell to maintain the heated solvent in a liquid state during the extraction. After heating, the extract is flushed from the sample cell into a collection bottle and is ready for analysis.

100 Accelerated Solvent Extractor is a system for extracting either

1 • Introduction

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Figure 1-1. ASE 100 Accele rated Solvent Extractor

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ASE 100 Operator’s Manual

The ASE 100 is designed to minimize the amount of solvent used without sacrific in g the speed of extracti on or eas e of oper ation. Samples are ex tr act ed on e at a time, and the extraction process is typically completed in 15 to 25 minutes. All functions are controlled from the ASE 100 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.

The ASE 100 is available in four product versions:

Product Description Part Number

ASE 100 with 10 mL extraction cells 059700 ASE 100 with 34 mL extraction cells 059701 ASE 100 with 66 mL extraction cells 059702 ASE 100 with 100 mL extraction cells 059703

Each ASE 100 is shipped from Dionex with two extraction cells in the sizes indicated above, one rinse cell in the required size, and 12 collection bottles.

1-2

Ordering Extraction Cells in Other Sizes

The ASE 100 accommodates four extraction cell sizes (10 mL, 34 mL, 66 mL, or 100 mL). To perform an extraction with a cell in any size other than the size included with your system, order the appropriate cells from Dionex. Cells are available individually and in packages of six. For cell descriptions and part numbers, see Appendix D of this manual.

Note that installation of a different extraction cell will require a few additiona l changes:

Reposition the cell holder to accommodate the new extraction cell size, if

required. For instructions, refer to Section B.2.7. Order a new rinse cell, if required. The rinse cell size must be matched to the

extraction ce ll size. For deta ils, see Section 2.1.3. Before beginning a n e xtr acti on, speci fy the ne w cel l size on the

SETUP

screen

(see Section C.1.3).

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1.2 About This Manual

1 • Introduction

Chapter 1

Introduction

Chapter 2

Description

Chapter 3

Operation and

Maintenance

Chapter 4

Troubleshooting

Chapter 5

Service

Appendix A

Specifications

Appendix B

Installation

Presents a brief overview of the ASE 100 Accelerated Solvent Extractor. Explain s the meaning of safety messages and icons in the manual and safety labels on the instrument.

Describes the physical aspects of the ASE 100: the front panel controls, rear panel connections, electronics, and mechanical components. Briefly describes the extraction process.

Describes key operating features and how to create, edit, and run methods. Lists routine preventive maintenance requirements.

Lists possible causes of minor problems, as well as stepby-step procedures to resolve them.

Contains step-by-step instructions for routine service and parts replacement procedures.

Lists the ASE 100 specifications and installation site requirements.

Describes how to install the ASE 100.

Appendix C

User Inte rface

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Appendix D

Reordering

Information

Illustrates and describes all of the display screens selected from the ASE 100 front panel.

Lists names and part numbers for spare parts for the ASE

100.

1-3

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ASE 100 Operator’s Manual

1.2.1 Typefaces

Uppercase bold t ype indic ates an ASE 100 fr ont panel b utton, the name of a screen, or an on-screen entry. For example:

Press

RINSE

The

MAIN

Move the cursor to the

to start the rinse cycle.

screen has four options.

field .

SA VE

1.2.2 Saf et y Me ss ages and Notes

This manual contains warnings and precautionary statements that can prevent personal injury and/or damage to the ASE 100 when properly followed. Safety messages appear in bold type and are accompanied by icons, as shown here.

Indicates an imminentl y hazardous situation whic h, i f 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.

Indicates that the function or process of the instrument may be impaired. Operation does not constitute a hazard.

1-4

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1 • Introduction

Messages d’avertissement en français

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

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

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

Warnhinweise in Deutsch

Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder schwerwiegenden Verletzungen führen.

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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 verwen det, wenn eine Situation zu schweren Schäden am Gerät führen kann, jedoch keine Verletzungsgefahr besteht.

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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ASE 100 Operator’s Manual

1.3 Safety Labels

The TUV GS, C, US Mark safety label and the CE Mark label on the ASE 100 indicate that the ASE 100 is in compliance with the following standards: EN 61010-1:1993 (safety), CAN/CSA-C22.2 No. 1010.1-92 (safety), UL 31011/10.93 (safety), EN 50082-1:1992 (susceptibility), and EN 55011:1991 (emissions).

The symbols below appear on the ASE 100 or on ASE 100 labels.

Alternating current

Protective conductor terminal

Power supply is on

1-6

Power supply is off

Hot surface

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Section 2.1 and Section 2.2 describe key operating features and components

of the ASE 100. Section 2.3 describes the extraction process of the ASE 100.

Section 2.4 describes method control of the ASE 100.

Section 2.5 lists the operating parameters for preprogrammed methods.

2.1 Operating Features

Figure 2-1 illustrates the main operating features of the ASE 100.

2 • Description

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Figure 2-1. ASE 100 Key Operating Features

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ASE 100 Operator’s Manual

Control Panel

The ASE 100 control panel includes a display screen and a membrane keypad with seven buttons. For more information about the display screen, refer to Section 2.1.1. For a description of the keypad buttons, refer to Section 2.1.2.

Cell Holder

Before a sample e xtrac tion or a rinse c ycl e is per formed, an e xtr action ce ll or ri nse cell, respectively , must be installed in the cell holder on the inside of the cell door. To access the cell holder , pus h do wn on th e and pull open the door.

Oven

The oven is located behind the cell door. This area also houses the AutoSeal™ tips, which seal the cell during an extraction. A pull-out drip tray is installed below the o v e n to coll ect an y l iquid l eak s that may occur dur ing an e xt ract ion or a rinse cycle.

Needle Mechanism

The needle mechanism includes a source needle and two vent needles. The

UP/DOWN

are in the “down” position, they pierce the collection bottle septum, allowing the extract to f low from the extraction cell into the collection bot t le. The vent needle s are connected to the w aste bot tle ca p and the sys tem v ent to allow displaced gases to escape.

toggle switch controls the position of the needles. When the needles

lever (to release the door latch)

OPEN

2-2

Solvent Bottle

A 1-liter or 2-lit er solv ent bottle is in stal led in a re cess on top of the AS E 100. The recess contains a plastic liner to contain any solvent leaks or spills that may occur.

Waste Bottle

The waste bottle is a 250 mL collection bottle that is sealed with a special cap assembly. The waste bottle cap is connected to the vent needles. This allows excess solvent vapors to condense and be collected in the waste bottle before being vented out the ASE 100 rear panel.

Collection Bottle

After each extraction, the 250 mL collection bottle contains solvent and the analytes extracted from the sample.

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2.1.1 Control Panel Screen

The control panel scree n disp lays s tatus an d opera ting i nforma tion f or th e ASE 100. Use the screen, in conjunction with the control panel keypad (see Section 2.1.2), to control ASE 100 operation.

You can edit any f ield on the screen that contains a blinking curso r . A f ield without a blinking cursor is for display only.

2•Description

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Figure 2-2. ASE 100 Control Panel

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ASE 100 Operator’s Manual

2.1.2 Contro l Panel Keypad

Use the control panel k e ypad, in c onjuncti on with t he contr ol panel screen (see Section 2.1.1), to control ASE 100 operation.

Three of the control panel buttons (

START, RINSE

, and

STOP

) let you

directly control the most frequently used functions.

Button Function

Starts the currently selected method. The LED starts flashing when the oven is within 5 °C of the set point. 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.

Starts a rinse cycle in which about 5 mL of solv ent is p umped 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.

Always install a rinse cell and a rinse bottle before

Note:

starting a rinse cycle; see Section B.2.6 for instructions. Interrupts the currently running method or rinse cycle and

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

ABORT

screen; see Section 3.6 for details.

The four screen na viga tion b utt ons (

screen. Pressing the button lights the

MENU, ENTER

, the up arrow, and the down arrow) are used in conjunction with the ASE 100 display to access less frequently used functions. The action of the navigation keys depends on whether the cursor is in

normal

mode or

editing

mode:

2-4

normal

mode, the cursor does no t blink and looks like

this. In

editing

mode, the cursor blinks and looks like this.

You can edit any field that contains a blinking cursor.

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2•Description

Button Function

Normal mode:

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

METHOD EDITOR

returns you to the

screen is displayed,

screen. See

MAIN

Figure C-1 for an overview of the screens.

Editing mode:

Rejects your editing change in a field and

reverts to the previously selected parameter.

Normal mode:

pointing to. On the

Selects the field the cursor is currently

MAIN

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.

Editing mode:

Saves the parameter currently displayed in a

field.

Normal mode:

Moves the cursor, in the direction of the arrow,

to the next selectable line on the display (if any).

Editing mode:

Pressing and releasing an arrow button displays the next or previous parameter or numeric value allowed for the field. Pressing and holding down an arrow button moves the cursor continuously through the allowed settings.

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ASE 100 Operator’s Manual

2.1.3 Extrac tion Cells and Rinse Cells

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

Extraction Cells

ASE 100 extraction cells are available in four sizes: 10 mL, 34 mL, 66 mL, and 100 mL. Interchangeable end caps scre w ont o each e nd of t he cell body. Each cell end cap contains a stainless steel frit and a seal. During a run, the cell caps are compressed to form a tight seal between the caps and the cell body.

An O-ring is installed on the outside of each cell cap. Teflon

(P/N 049457, pkg. of 50) are standard. Viton

O-rings (P/N 056325, pkg.

O-rings

of 50) are available for high temperature extractions, such as dioxins.

If a Viton (black) O-ring is installed on the outside of the cell cap, do not use acetone as the solvent for an extraction.

Note that only cell end caps with two knurled bands can be used with the ASE 100 (see Figure 2-3).

Cell end caps with two knurled bands can be installed in either the ASE 100 or ASE 300 Accelerated Solvent Extractor. However, end caps with one knurled band can only be used with the ASE 300.

2-6

Figure 2-3. Knurling on Cell End Caps

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Rinse Cells

During a rinse cycle, solvent passes directly through the blue rinse cell and into the collection bottle. For more information about rinse cycles, see Section 3.1.7 and Section B.2.6.

The rinse cell size ( short, medi um, or long) mus t be matche d to the si ze of the extraction cell, as indicated in the table below.

Use this rinse cell: With this extraction cell:

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

2.1.4 Collection Bottle

The 250 mL collection bottle (P/N 056284, pkg. of 12) is made of clear glass. The collection bottle cap contains a solvent-resistant septum. During an extraction, the needle mechanism is lowered so that the needles pierce the septum. This creates a liquid flow path from the extraction cell to the collection bottle.

2•Description

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After an extraction, the bottle contains solvent and the analytes extracted from the sample. Refer to S ection 3.5 for post-extraction procedures.

s with any glass object, the collection bottle may become

damaged after repeat ed use. Before each extraction, carefully inspect the collection b ottle for chips, scratches, or cracks. If you notice any signs of damage, dispose of the bottle and install a new one.

Replace the septum (P/N 04 9464, pkg. of 72) in the bottle cap after each extraction. Using the septum more than once may cause loss of sample and damage to the instrument.

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ASE 100 Operator’s Manual

2.1.5 Solvent Bottle

The ASE 100 Ship Kit (P/N 059397) includes a 2-liter glass bottle with shatterproof plastic coating (P/N 045901) and a bottle cap assembly (P/N 051977) with tubing and fitt ings f or the inl et and outle t conne ction s. For instructions on how to install the solvent bottle, see Section B.2.4.

Use only Dionex solvent bottles (1-liter, P/N 045900; 2-liter, P/N 045901). 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 (1 litre, N/P 045900; 2 litres, N/P 045901). Ce sont des réservoirs en verre à revêtement incassable en plast ique. Veillez à ce que la pression exercée sur ces réservoirs ne dépasse pas 0,07 MPa.

Verwenden Sie ausschließlich die Lösemittelbehälter von Dionex (1-Liter, Bestell-Nr. 045900 ; 2-Liter, Bes tell-Nr. 04 5901). 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.

2-8

NOTE Never fi ll the solvent bottle or disconnect the tubing

connections to the (see Figure 3-1) when the system is performing an extraction or a rinse cycle. During these times, the solvent bottle is pressurized. If you remove the bottle cap when the solvent bottle is pressurized, the ASE 100 may not operate to specification.

SOLVENT

and

GAS

connectors

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2.1.6 Waste Bottle

A 250 mL collection bottle (P/N 056284, pkg. of 12) serves as the waste bottle (see Figure 2-1) for the system.

Three vent lines, one from the pressure relief valve and two from the needle mechanism, are connec ted to the w aste bottle cap. The waste bottl e collects the small amounts of condensed solvent vented through these lines.

A vent outlet line is connected to the wast e bot tl e cap, also. Gas is vented out this line to the rear pan el of the ASE 100. F or instal lation ins tructi ons, see Section B.2.1.

NOTE Check the waste bottle regularly and empty

2.2 Rear Panel

Figure 2-4 illustrates th e rear panel of the ASE 100.

2•Description

whenever necessary.

The

POWER

The power re cepta cle al so inc ludes the fuse h older. For instructi ons on how to replace the fuses, see Section 5.11.

The oven voltage switches must be set to match the voltage from the power source at the ASE 100 installation site. For instructions on how to set the switches, see Section B.2.2.

The

NITROGEN

between 1.03 and 1.38 MPa (150 to 200 psi). For installat io n i nst ruc ti ons , see Section B.2.1.

The

VENT

installation instructions, see Section B.2.1. The model data label list s fuse and po wer informati on, as well as the ASE 100

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

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

connector is connected to a nitrogen supply regulated to

connector provides a connection for the vent outlet line. For

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ASE 100 Operator’s Manual

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Figure 2-4. ASE 100 Rear Panel

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2.3 Extraction Process

Before starting an extraction, perform the following steps. Re fer to Chapter 3 for detailed instructions for each step.

Prepare sample and load it into the extraction cell.

Set up a method.

2•Description

Press the

Verify that the system

on the Place the collection bottle, with the bottle cap screwed on, in the holder.

Lower the needle mechanism. Place the extraction cell in the cell holder and close t he cell door.

Press

From this point, the ASE 100 automatically performs the extraction process. An extraction consists of six main steps:

Filling the cell with solvent

Heating the cell (equilibration)

Static extraction

Flushing with fresh solvent

Purging solvent from the system

End relief

START

button.

STATUS

button is flashing.

to begin the run.

OVEN READY

(see Figure 2-5) and the LED

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ASE 100 Operator’s Manual

You can monitor the progress of an extraction on the

STATUS

screen (a

MAIN

screen option). Operating parameters are updated in real time. Figure 2-5 illustrates a typical

Parameter Description STATUS

METHOD VOL

PRESSURE

TEMP TIME

STATUS

Table 2-1. Status Screen Parameters

screen. Table 2-1 describes the screen parameters.

Figure 2-5. Status Screen

The method step in progress, if any, or the current system status. If the latter is indicated, the

STATUS

will display one of the following descriptions: Initialize, Idle, Load, Fill, Preheat, Heat, Oven Wait, Ov en Ready, Static, Flush, Purge, Relief, Unload, Rinse, or Abort. If the status is Static or Flush, the cycle number is indicated.

The name or number of the current method. The approximate volume of solvent (in mL) delivered

by the pump since the method started running. The current pressure reading. Select the unit of measure

on the

SETUP

screen (see Section C.1.3). The temperature specified in the method. Elapsed time (in minutes and seconds) since the method

started running.

field

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2.4 Method Control

2•Description

method

defines all of th e timed ev ents that occur during a sample ext raction (see

Table 2-2). There are two types of methods:

Preprogrammed

methods are application-speci fic meth ods 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 customer-pr ogrammabl e methods. A ll custom m ethods initially contain the default method parameters. These methods can easily be modified ( i.e ., c ust om iz ed) by the user as required. For instruction s o n how to edit a custom method, see Section 3.2.

Parameter Function Value Range TEMPERATURE

STATIC TIME

FLUSH VOLUME

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

200°C (default=100)

Static solvent extraction time. 0 to 99 min

(default=5)

Amount of solvent to flush through the extraction cell after the static heating step. The

FLUSH VOLUME

of the cell volume; for example, if the

VOLUME

a 10 mL cell, 17 m L i s flus hed t hr oug h a 34 mL cell, and so on.

is set to 50%, 5 mL is flushed through

is expressed as a percentage

FLUSH

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

PURGE TIME

STATIC CYCLE

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Amount of time the cell is purge d with nitro gen . 20 to 900 sec

(default=100)

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

Table 2-2. Method Parameters

1 to 5 (default=1)

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ASE 100 Operator’s Manual

2.5 Preprogrammed Methods

To enable you to quickly produce res ul ts wit h t he ASE 100, Dionex pro v ide s nine preprogrammed methods. These methods are designated by three-letter abbrevia ti ons (se e 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

2-14

Total Petroleum Hydrocarbons TPH

The remainder of this section lists the operating conditions and recommended solvent 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 Flush Volume 60% Purge Time 100 sec Static Cycle 1

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2•Description

FAT (Total Fat) Method Parameters

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

HRB (Chlorinated Herbicides) Method Parameters

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

3PO4

Temperature 100 °C

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Static Time 5 min Flush Volume 60% Purge Time 100 sec Static Cycle 1

OCP (Organochlorine Pesticides) Method Parameters

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

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ASE 100 Operator’s Manual

OPP (Organophosphorous Pesticides) Method Parameters

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

Static Time 5 min Flush Volume 60% Purge Time 100 sec Static Cycle 1

PCB (Polychlorinated Biphenyls) Method Parameters

Solvent Hexane Temperature 100 °C Static Time 5 min Flush Volume 60% Purge Time 100 sec Static Cycle 1

PDF (Dioxins and Furans) Method Parameters

Solvent Toluene Temperature 200 °C Static Time 5 min Flush Volume 60% Purge Ti me 100 sec Static Cycle 1

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PPE (Polymer Additives) Method Parameters

Solvent 2.5% Cyclohexane in

Isopropyl Alcohol Temperature 140 °C Static Time 3 min Flush Volume 100% Purge Time 60 sec Static Cycle 3

TPH (Total Petroleum Hydrocarbons) Method Parameters

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

2•Description

Static Time 5 min Flush Volume 60% Purge Time 100 sec Static Cycle 1

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ASE 100 Operator’s Manual

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3 • Operation and Maintenance

3.1 Preparing to Run an Extraction

3.1.1 Selecting and Preparing Solvent

Do not use solvents with an autoignition point of 40 to 200 °C (104 to 392 °F). The table below is a partial list of solvents that should not be used with the ASE 100. If you have a question about solvent suitability, contact Dionex.

Solvents Not to Use Autoignition Point

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

O180

2H5)2

4H8O2

N'utilisez pas de solvants ayant un point d'auto-inflammation entre 40 et 200 °C. Le tableau ci-dessous donne la liste de quelques solvants qui ne devraient pas être utilisés avec l'ASE

100. Contactez Dionex si vous avez des questions sur le caractère approprié d'un solvant.

100 °C (212 °F)

180 °C (356 °F)

C (356 °F)

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Solvants à ne pas utiliser Point d'auto-infl amm atio n

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

2H5)2

4H8O2

100 °C

O180 °C

180 °C

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ASE 100 Operator’s Manual

Verwenden Sie keine Lösungsmittel, deren Selbstentzündungstemperatur bei 40° bis 200°C liegt. Die untenstehende Tabelle zeigt einige Lösungsmittel, die Sie nicht mit dem ASE 100 verwenden sollten. Bei Fragen zur Eignung von Lösungsmitteln wenden Sie sich bitte a n Dionex.

Nicht zu verwendende Lösungsmittel

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

When devel oping a ne w ex traction metho d, select a sol vent or solvent

2H5)2

4H8O2

O 180 °C

Selbstentzündungstemperatur

100 °C

180 °C

mixture that has a high solubility for the analytes of interest, but not for the sample matrix. If you have been using another extraction method (Soxhlet, for example), use the same solvent with the ASE 100 that you used with the other method.

Before running a prepr ogr ammed me tho d, r efe r to Section 2.5 for the

recommended solvent. Use HPLC- or pesticide-grade solvents.

Use organic or aqueous solvents.

Use single- or multiple-component solvents.

Weak acids and bases (pH >2 or pH <11) or other noncorrosive

additives can be used, but add them in small percentages (<5% by volume) to the solvent system. Do not use nitric, hydrochloric, or sulfuric acid with the ASE 100.

3-2

After extracting with acidic solvents or basic solvents, rinse the system with eit her 100% organic solvent (e. g., acetone or methanol) or distilled water before overnight shutdown.

Solvents do no t g enerally need to be degassed. Deg as solvents only if

the analyte of interest oxidizes easily.

Do not use acetone if the O-ring on the outside of the extraction cell cap is Viton (black).

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3.1.2 Filling the Solvent Bottle

Use only Dionex solvent bottles (1-liter, P/N 045900; 2-liter, P/N 045901). 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).

Utilisez uniquement des réservoirs à solvant Dionex (1 litre, N/P 045900; 2 litres, N/P 045901). Ce sont des réservoirs en verre à revêtement incassable en plas tique. Veillez à ce que la pression exercée sur ces réservoirs ne dépasse pas 0,07 MPa.

NOTE Never fi ll the solvent bottle or disconnect the tubing

3 • Operation and Maintenance

SOLVENT

and

GAS

connectors

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1. Fill the sol vent bottle with prepared solvent to the level indicated in Figure 3-1.

If you plan to run a preprogrammed method, refer to Section 2.5 for the recommended solv ent. I f you pla n to run a custom method , re vie w the solvent se lection guidelines in Section 3.1.1.

NOTE The solvent level in the bottle must remain below the

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

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

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ASE 100 Operator’s Manual

3. Insert the solvent outlet line extending from the underside of the bottle cap assembly into the bottle (see Figure 3-1). Make sure the inline filter rests on the bottom of the bottle. (This prevents air from being drawn through the line.)

4. Hand-tighten the re d lock ring cap securely over the stopper.

NOTE Always connect the outlet line to the

connector first, and then the inlet line to the connector. Reverse this order when disconnecting the lines. It is not necessary to disconnect the solvent and gas lines before refilling the solvent bottle.

SOLVENT

GAS

3-4

Figure 3-1. Solvent Bottle Connections (Top view)

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3.1.3 Preparing the Sample

Some samples must be mixed with a drying or dispersing agent before being loaded into the cell. If you have successfully followed a particular sample pretreatment procedure for another extraction method (Soxhlet, for example), us e the same procedu re with the ASE 100. If you hav e ne ver run an extraction before or if you are preparing a new sample, follow the guidelines here.

Drying or Dispersing Agent Selection Guidelines

The sample preparation guidelines in the next section mention two

drying and dispers ing ag ents: sodi um sulf at e (Na diatomaceous earth (DE). DE is easier to work with than sodium sulfate; it dries samples more quickly, provides a cleaner transfer of the mixtures to the cell, and extracts well. Sodium sulfate is more readily available, but it tends to clump the samples and this makes transfer more difficult.

The use of sodium sulfat e wit h very wet samples (30% moistu re) can

clog the frits in the cell with recrystallized sodium sulfate. This is most likely to occur when using a mixed solvent with acetone or methanol. To prevent clogging, substitute DE as a drying agent and mix it with the sample before loading into the extraction cell. Or, use DE as a drying agent in the cell for all levels of moisture.

3 • Operation and Maintenance

) and pelletized

2SO4

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To ensure that very wet samples are completely dried (regardless of

which drying agent is used), add sodium sulfate to the bottles after collection and then pass the extracts through either a drying column or a drying cartridge. At the temperatures used during ASE 100 extractions, m ore water is co- extracted than with other extraction procedures. To ensure good analyte recovery, thoroughly rinse the sodium sulfate from the bottle and the cleanup column.

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ASE 100 Operator’s Manual

Sample Preparation Guidelines

The mixtures here are recommendations; adjust the proportions as required for your extraction.

If the sample appears dry, use one of these mixtures:

4 grams sample to 1 gram DE 4 grams sample to 4 grams Na

2SO4

Mix the sample and the DE or Na2SO4 thoroughly in a small bottle, beaker, or mortar .

If the sample appears wet, use one of these mixtures:

4 grams sample to 2 grams DE 4 grams sample to 8 grams Na

2SO4

Mix the sample and the DE or Na2SO4 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.

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3.1.4 Installing the Cell Filter

A disposable filter must be installed in the bottom end of the extraction cell before sample is loaded. The filter prevents blockage of the stainless steel frit in the bottom cap.

There are two types of cell filters:

3 • Operation and Maintenance

Cellulose

filters (P/N 056780, pkg. 100) are appropriate for most extraction m ethods that use organic solvents. The ASE 100 Ship Kit (P/N 059397) includes a package of cellulose filters.

Glass-fiber

filters (P/N 056781, pkg. 100) are recommended for aqueous extractions, where cellulose may provide inadequate filtration or may interfere with the analytical technique.

1. Screw a cell cap onto the bottom of the cell body. (There is a groove around the top of the cell body, but no groove around the bottom.) Hand-tighten the cap.

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

Always tighten the bottom cell cap onto the cell before installing the cell filter. If you install the filter first, the cap will not seal properly and will allow leaks.

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ASE 100 Operator’s Manual

2. Follow the steps below to install the cell filter.

Insert a cellulose or glass-fiber 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.

3-8

Push down on the filter until it is in full contact with the end cap frit. (End cap not shown in photo.)

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3.1.5 Filling the Cell

NOTE 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/o r allow l eaks during the extraction.

1. Carefully load the sample into the top of the extraction cell, using the funnel (P/N 056699 ) pro vided i n the ASE 10 0 Ship Kit (P/N 0593 97).

3 • Operation and Maintenance

2. (

Optional

) To reduce the amount of solvent used during the extraction, 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.

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

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

5. Check the ends of each end cap to verify that the O-rings are in place and are in good condition (see Figure 3-2). If an O-ring is discolored or has a hole size of less than 0.5 mm, replace it:

a. Use a small flathead screwdriver (P/N 046985) to remove the old

O-ring from the cell cap.

b. Place a new O-ring over the openi ng in the end of the cel l cap and

press it into place, using the O-ring insertion tool (P/N 049660).

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ASE 100 Operator’s Manual

Figure 3-2. Inspecting Cell O-Rings

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3 • Operation and Maintenance

3.1.6 Installing the Collection Bottle

1. Toggle t he nee dle s witch o n th e fr ont pa nel ( see Fi gure 3-3) to the UP position.

2. Place a 250 mL collection bottle (P/N 056284, pkg. of 12), with the bottle cap screwed on, in the collection bottle holder (see Figure 3-3).

3. Toggle the needle switch to the

NOTE Reverse the steps above to remove the collection

bottle from the system.

Figure 3-3. Installing the Collection Bottle

DOWN

position.

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NOTE Verify that the waste bottle is installed (see

Section B.2.5).

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ASE 100 Operator’s Manual

3.1.7 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 bottle

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

solvent) When the solvent lines contain bubbles

After a run is aborted

Before shutting down the system, if an extraction used acidic solvents

or basic solvents (see Section 3.8) After a shutdown of more than one day (see Section 3.8)

Before starting a rinse cycle:

Check that the rinse cell size is matched to the extraction cell size.

Adjust the cell holder to accommodate the rinse cell, if necessa ry.

Install the rinse cell in the cell holde r.

Close the cell door.

When you are ready, press the detailed instructions, refer to Section B.2.6.

RINSE

button to start the rinse cycle. For

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3 • Operation and Maintenance

3.2 Editing a Custom Method (1–24)

If the ASE 100 preprogrammed methods (see Section 2.5) are not suitable for a particular e xtracti on, edit one of the 24

custom

All parameters in these methods are initially set to their default values. You can create a new method by editing either a custom method that still contains the default parameters or a custom method that you previously edited. The edited method can be saved to a new method number, if desired.

Before beginnin g, re vi ew the method de v elopment gui delines in Secti on 3.3. For a list of the values allowed for metho d parameters, see Table 3-3.

Parameter Function Value Range

methods provided with the sys tem.

TEMPERATURE

STATIC TIME

FLUSH VOLUME

PURGE TIME

STATIC CYCLE

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

200°C (default = 100)

Static solvent extraction time. 0 to 99 min

(default = 5)

Amount of solvent to flush through the extraction cell after the static heating step, expressed as a percentage of the cell volume. For example, if the 50%, 5 mL is flushed through a 10 mL cell , 17 mL is flushed through a 34 mL cell, and so on.

Amount of time the cell is purged with nitrogen. We recommend 40 to 80 seconds fo r a 10 mL cell, 70 to 110 seconds for a 34 mL cell, 160 to 200 seconds for a 66 mL cell, and 250 to 290 seconds for a 100 mL cell.

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

Table 3-3. Method Parameters

FLUSH VOLUME

is set to

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

20 to 900 sec (default = 100)

1 to 5 (default = 1)

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ASE 100 Operator’s Manual

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

1. Press

to display the

Figure 3-4. Main Screen

MAIN

screen.

2. Move the cursor to the The

METHOD EDITOR

Figure 3-5. Method Editor Screen (Additional text shown)

NOTE For convenience, Figure 3-5 illustrates all of the

method parameters. In reality, the screen displays no more than four lines of text at once. To scroll the screen and view additional lines of text, press an arrow button.

option and press

METHOD EDITOR

screen is displayed (see Figure 3-5).

ENTER

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3 • Operation and Maintenance

3. The

METHOD EDI TOR

selected on the displayed, press

screen displays the parameters for the method last

screen (see Sectio n C.1.3). If method 1 is not currently

SETUP

ENTER

to move the cursor to the method editing field. Use an arrow button to step through the method numbers (1 through 24). When 1 is displayed, press

ENTER

4. All method 1 parameters are set to the default values (see Table 3-3). Follow the steps below to edit the me thod as required.

a. Using an arrow butt on, mo v e the cur so r to the first parameter that

you want to change (for example,

b. Press

ENTER

to move the cursor to the editing field for this

TEMPERATURE

parameter. (This also highlights the value currently selected here.)

NOTE If you decide not to edit this field, press

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

ENTER

to save it and to return the cursor to

the left margin o f the screen.

5. When you finish editing, use one of the following options to save the method.

To save to the current method number:

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d. If other changes are required, repeat Steps a-c.

NOTE Saving to the current method number will

permanently overwrite the previous version of the method. There is no way to undo this action.

a. U sing an arrow button, m ove the cursor to b. Press c. Press

ENTER ENTER

to move the cursor to the

SAVE

to save the modified version of the method to the

SAVE

editing field.

current method number. The screen displays a message confirming that the method was saved.

d. Press

MAIN

screen.

to exit the

METHOD EDITOR

screen and return to the

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ASE 100 Operator’s Manual

To save to a different method number:

a. U sing an arrow button, m ove the cursor to b. Press

ENTER

to move the cursor to the

SAVE

editing field.

c. Press an arrow button to step through the method numbers (1

through 24). When the desired number is displayed, press

ENTER

. The screen displays a message confirming that the

method was saved.

d. Press

MAIN

screen.

to exit the

METHOD EDITOR

screen and return to the

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3 • Operation and Maintenance

3.3 Guidelines for Method Development

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

1. Select a solvent(s) (see Section 3.1.1).

2. Prepare the sample (see Section 3.1.3).

3. Press the

button to display the

4. Move the cursor to This displays the

METHOD EDITOR

MAIN

Figure 3-6. Main Screen

METHOD EDITOR

and press

screen.

ENTER.

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Figure 3-7. Method Editor Screen (Additional text shown)

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ASE 100 Operator’s Manual

5. The

METHOD EDITOR

selected on the want to edit, press

screen displays the parameters for the method last

screen (see Sectio n C.1.3). If this is not the meth od you

SETUP

ENTER

to move the cursor to the method editing field. Press an arrow button to step through the method numbers (1 through 24). When the correct method number is displayed, press

ENTER

to display the

parameters for this method.

6. Begin editing the method as follows: a. Using an arrow butt on, mo v e the cu rso r to the first parameter that

you want to change (for example,

b. Press

ENTER

to move the cursor to the editing field for this

TEMPERATURE

parameter.

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

highlighted parameter. When the required value is displayed, press

ENTER

to save it and to return the cursor to the left margin of the screen. Figure 3-8 shows how the screen would look after changing the temperature from the previous setting (100

150

C) to

3-18

Figure 3-8. Method Editor Screen after Editing (Additional text shown)

7. Repeat Step 6 to change other parameters, if required.

8. When you finish editing, assign a number to the new method as follows: a. Move the cursor to b. Press

ENTER

to move the cursor to the editing field.

SAVE

c. Press an arrow but ton to step t hro ugh the me thod numbe rs. When

the desired number is displayed, press

ENTER

to save the new

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3 • Operation and Maintenance

method to this number and to return the cursor to the left margin of the screen.

9. Run the new method

three times

(with the same cell and sample) and analyze

the extracts.

10. If target analytes are present in extract 2 or 3, make the adjustments listed below

(one at a time)

to the method. After each adju stment, repe at 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 temperature, it is advisable to keep the temperature below the maximum allowed (200 °C). If oxidation is a concern, degas the solvent before use.

b. Run two static/flush 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 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 flush 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 flush volume to prevent the collection bottle from being overfilled.

11. If analytes stil l appear in the extract from the second extract, m ake the adjustments list ed bel o w. When target ana lyte s no long er appear in the e xtract from the second extract, the method is complete for this sample type.

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a. Run three static/flush cycles. b. Raise the temperature again. c. Increase static time. d. Select a differ ent solvent.

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3.4 Running an Extraction

1. Press

2. Select

SETUP

This displays the

to display the

Figure 3-9. Main Screen

and press

SETUP

ENTER

screen.

MAIN

screen.

3-20

Figure 3-10. Setup Screen (Initial view)

3. Check that the selected method is correct. If it is not, use an arrow to move the cursor to

METHOD

, and then press

ENTER

to move the cursor to the editing field. Press an arrow button to step through the method numbers and names. When the method required for the extraction is displayed, press

This displays the

METHOD EDITOR

screen. If this is a custom method, check

ENTER.

that the parameters are appropriate for the extraction. Edit the method, if necessary. (Remember to press

after making a change.)

Enter

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3 • Operation and Maintenance

4. Press

5. On the

MAIN

This displays the

6. Press

START,

STATUS

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

to return to the screen, select the

STATUS

Figure 3-11. Status Screen

and then check the

OVEN WAIT

screen.

MAIN

STATUS

option and press

ENTER.

screen.

STATUS

field (on the

STATUS

screen). If the

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

OVEN WAIT.

Installing

7. When the oven is within 5 °C of the set point, the

OVEN READY

pkg. of 12) and toggle the needle switch to the

8. Open the cell door and install the cell in the cell holder.

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STATUS

field changes to

. You can now install an empty collection bottle (P/N 056284,

DOWN

s with any glass object, the collection bottle may become

damaged after repeated use. Before installing a used collection bottle, carefully inspect it for chips, scratches, or cracks. If there are any signs of damage, dispose of the bottle and install a new one.

Replace the septum (P /N 049464, pkg. of 72) in the collection bottle cap after each extraction. Us ing the septum more than once may cause loss of sample and may damage the ASE 100.

position.

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ASE 100 Operator’s Manual

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.

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

Raise the cell so tha t the bottom end cap lifts the bottom latch.

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

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3 • Operation and Maintenance

9. Close the cell door and press

START

to begin the extraction. A typical

extraction takes 15 to 25 minutes.

Do not attempt to open the cell door while an extraction is in progress.

N'ouvrez pas la porte pendant une extraction.

Halten Sie die Tür während der Extraktion geschlossen.

10. When the extracti on is compl ete, thr ee beeps a re emitte d and the turns off.

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

START

LED

11. If you need to start the next extraction right away, put on the thermal gloves (P/N 060372) supplied in the ASE 100 Ship Kit (P/N 059397), remove the cell from the cell holder, and place it on the cell rack (P/N 059927) to cool.

If you are not starti ng anot her e xtr acti on right a w ay, open the cell door and le t the cell cool in the cell holder for at least 15 minutes. Afterward, put on the thermal gloves, remove the cell from the cell holder, and place it on the cell rack. Close the cell door until the next extraction, to save energy and prevent anybody from accidentally touching the inside of the door while it is hot.

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

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

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12. Toggle the needle switch to the UP position and remove the collection bottle containing the extract from the bottle holder. Refer to Section 3.5 for postextraction procedures.

3.5 Post-Extraction Procedures

3.5.1 Cleaning the Cells

Cells are extremely hot after an extraction. 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 an extra ct ion, empty the cells and r in se the cell bodies a nd e nd caps with water or organic solvent. For most applications, it is sufficient to simply rinse the en d caps; h o we ver, if necessary, disassemble the end caps and sonicate or soak in solvent to clean them. See Section 5.1 for instructions on how to disassemble the cell.

The cell bodies (but not the caps) can be cleaned in a dishwasher or hightemperature cleaning unit, provided that the temperature does not exceed 400 °C (752 °F).

3.5.2 Processing Extracts

The composition of the e xtrac ts generat ed by th e ASE 100 is v ery clos e to that generated by Soxhlet and other standard solid-liquid extraction techniques when using the same solvent. Use the same analytical method for ASE 100 extracts that you employed for extracts obtained from other techniques.

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3.6 Aborting a Run

3 • Operation and Maintenance

To abort a run manually, press the the

ABORT

The preferred option and press

Option What it means: ABORT

METHOD

screen (see Figure 3-12).

ABORT

screen pres ents two options (see below). Move the cursor to the

Cancels the method. If necessary, a purge is done to remove solvent from the sample. Then, residual pressure is relieved from the system.

Figure 3-12. Abort Screen

ENTER.

button. This stops the run and displays

STOP

CONTINUE METHOD

The ASE 100 contains built-in diagnostics and sensors that continuously monitor the system. Under certain conditions (for example, if the collection bottle becomes too full or if the hydrocarbon vapor level exceeds the upper limit), the system will automatically abort a run. If this occurs, the ASE 100 screen will display an error mess age; th e mess age will remain on -scre en until you pres s a ke y 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.

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Resumes the run from the point at which the button was pressed.

NOTE After a run is aborted (whether manually or

automatically), rinse the system before resuming operation. For instructions on how to run a rinse cycle, see Section B.2.6.

STOP

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3.7 Routine Maintenance

This section describes routine maintenance procedures that the user can perform. All other ASE 100 maintenance procedures must be performed by qualified Dionex personnel.

3.7.1 Daily Maintenance

Fill the sol vent bottle, if needed. After filling the solvent bottle,

always run two rinse cycles to clear the solvent lines of bubbles (see Section 3.1.7).

Empty the waste bottle, if needed.

Check the gases.

Check for leaks.

Pull out the drip tra y holder belo w th e o v en and ch eck the plas tic dr ip

tray. If the tray contains liquid, remove it from the holder, dispose of the liquid, and reinstall the tray.

3.7.2 Periodic Maintenance

NOTE The

Replace the PEEK seals (P/N 049455, pkg. of 10; P/N 049454, pkg.

of 50) inside the cell end caps after approximately 50 extractions, or when they become worn (see Section 5.1).

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

P/N 056325, pkg. of 50 Viton O-rings) on the outside of the cell end caps and rinse cells after approximately 50 extractions, or when they become worn (see Section 5.2).

Verify that the source needle is straight. If it is not, try bending the

needle back slightly. If this does not straighten the needle, it should be replaced (see Section 5.8).

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

lower AutoSeal tip. Make sure the tip is not flattened, and that it is not

EXTRACTION COUNTERS

Section C.2.5) indicates the number of extractions the ASE 100 has performed.

screen (see

3-26

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scratched, gouged, or corro ded. If the t ip is damaged or worn, rep lace it (see Section 5.10).

3.8 Shutdown

Overnight Shutdown

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

immediately. No other action is required. After extracting with an acidic solvents or a basic solvent, rinse the system

with either 100% organic solvent or distilled water (see Section 3.1 .7) before turning off the power.

Longer Shutdowns

Before shutting down for more than one night:

1. After extracti ng with acidic solvents or basic solvents, rinse the system with either 100% organic solvent or distilled water (see Section 3.1.7) before turning off the power.

3 • Operation and Maintenance

2. Turn off the gas supply.

Before shipping the ASE 100:

1. After extracti ng with acidic solvents or basic solvents, rinse the system with either 100% organic solvent (e.g., acetone or methanol) or distilled water (see Section 3.1.7).

2. Empty the solvent bottle, reconnect the bottle to the system, and run one or more rinse cycles to ensure that all solvent is removed from the lines.

3. Remove the solvent bottle.

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ASE 100 Operator’s Manual

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This chapter is a guide to troubleshooting minor problems that may occur during operation of the ASE 100 Accelerated Solvent Extractor. Turn to the section of this chapter that be st describes the operating pr oblem; there, the possible cause s of the problem are listed in order of probability, along with the recommended corrective action. If an error message appears on the ASE 100 screen, refer to Section 4.1 for details.

If you are unable to resolve a problem, contact Dionex Technical Support. In the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

4.1 Error Messages

The ASE 100 Moduleware 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 key to clear it or until another error message appears.

Each error message is identi fi ed by a number. This section lists the error messages and explains how to respond if an error occurs . Most p robl ems can be resolved by the user.

4 • Troubleshooting

Error 001 Cause:

Action:

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Oven compression pressure low.

Insufficient nitrogen gas pressure applied to the oven compression system during an extraction.

Check the nitrogen supply; if it is low, replace it. Regulate the supply to between 1.03 and 1.38 MPa (150 and 200 psi);

1.03 MPa (150 psi) is recommended. Check the

the oven is compressed, the

0.90 ± 0.03 MPa (130 ± 5 psi); if it does not, adjust the pressure regulator for the compression oven.

If the error message appears again, contact Dionex for assistance.

REGULATORS

screen (see Section C.2.3). When

COMPRESSION

field should read

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ASE 100 Operator’s Manual

Error 002 Cause: Action:

System pressure low.

Insufficient nitrogen gas pressure applied to the system. Check the nitrogen supply; if it is low, replace it. Regulate the

supply to between 1.03 and 1.38 MPa (150 and 200 psi);

1.03 MPa (150 psi) is recommended.

Action:

Check the

SYSTEM

REGULATORS

field should read 0.34 ± 0.02 MPa (50 ± 3 psi); if it

does not, adjust the pressure regulator for the system gas to

0.34 MPa (50 psi).

Action:

If the error message appears again, contact Dionex for assistance.

Error 003 Oven temperature low. Cause:

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

Action:

Error 004 Oven temperature high

Contact Dionex for assistance.

screen (see Section C.2.3). The

4-2

Cause:

Action:

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

Contact Dionex for assistance.

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4 • Troubleshooting

Error 005 Cause: Action:

Cell pressure threshold exceeded.

A blockage in the system. Run a rinse cycle (see Section 3.1.7). If the rinse runs

successfully, the extraction cell may be plugged. Replace the cell filter (see Section 3.1.4) and the stainless steel cell frit (see Section 5.1).

Action:

If the rinse is not successful, there may be a blockage in the solvent lines. Contact Dionex for assistance.

Error 006 Collection bottle full. Cause:

Action:

The collection bottle is full. Empty the collection bottle. If the error message reappears,

contact Dionex for assistance.

Error 007 Collection bottle not detected. Cause:

The collection bottle is not installed, or the sensor failed to detect the bottle.

Action:

Error 008 Cell not detected. Cause:

Action:

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

DOWN

position

(see Section 3.1.6). If the error message reappears, contact Dionex for assistance.

No cell is installed, or the sensor failed to detect the cell. Install the appropriate cell (see either Section 3.4, Step 8, or

Section B.2.6.) The installation procedure for extraction cells and rinse cells is identical. If the error message reappears, contact Dionex for assistance.

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ASE 100 Operator’s Manual

Error 009 Pump volume limit exceeded. Cause:

If the pump exceeds the volume limit (250 mL), there is probably a leak somewhere in the system.

Action:

Remove the right side panel of the ASE 100 (see Section 5.3). Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings. Tighten any leaking fittings.

Action:

Pull out the drip tray holder below the oven and check the plastic drip tray. If the tray contains liquid, remove it from the holder, dispose of the liquid, and reinstall the tray. Then, remove the collection bottle and waste bottle from the system. Remove the lo wer trim pan el and check f or leaks near the ov en and the AutoSeal mechanism.

Error 010 Analog-to-digital converter failed. Cause:

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

Action:

Contact Dionex for assistance.

4-4

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Error 011 Solvent vapor threshold exceed ed.

4 • Troubleshooting

Cause: Action:

Cause:

Action:

Cause: Action:

Action:

The cell is leaking. 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 5.1). Tighten the cell end caps hand-tight.

Do not use a wrench or

other tool.

Solvent was not completely removed from the cell during the purge cycle.

The optimal purge time v aries, depending on t he extraction cell size (see Table 3-3). If you are running a preprogrammed method, create a custom method with the appropriate purge time (see Section 3.2). If you are already running a custom method, edit the method to increase the purge time (see Section 3.2).

A leaking fitting(s) somewhere in the system. Remove the right side panel of the ASE 100 (see Section 5.3).

Inspect the following fittings for leaks (see Figure 4-1): pump fittings, pump check valves, pressure transducer fittings, relief valve fittings, static valve fittings, and solvent line fittings. Tighten or replace any leaking fittings.

Error 012 Clamp plate temperature low. Cause:

Action:

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

Contact Dionex for assistance.

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ASE 100 Operator’s Manual

Error 013 Clamp plate temperature high. Cause:

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

Action:

Error 014 Oven unable to reach temperature. Cause:

Contact Dionex for assistance.

The heater cable connection to the power supply is loose, or there is a problem with a heater component.

Action:

The defective component should be replaced. Contact Dionex for assistance.

Error 015 Unable to flush. Cause:

Action:

The solvent bottle is empty, or is not properly installed. Refill the solvent bottle, if necessary. Check that the solvent

bottle is installed as instructed in Section B.2.4.

Cause:

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

Action:

Run a rinse cycle (see Section 3.1.7). If the rinse runs successfully, the extraction cell may be plugged. Replace the cell filter (see Section 3.1.4) and the stainless steel cell frit (see Section 5.1).

4-6

Action:

If the rinse is not successful, there may be a blockage in the solvent lines. Contact Dionex for assistance.

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Error 016 Unable to fill cell.

4 • Troubleshooting

Cause:

Insufficient pressure was applied to the cell during an extraction.

Action:

Error 017 Remove cell during oven wait period Cause:

An extraction cell was installed in the cell holder before the temperature set point was reached.

Action:

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

STATUS

READY

field (on the

STATUS

screen) indicates

and the LED on the front panel

flashing. For more details, refer to Section 3.4.

Start

OVEN

button starts

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ASE 100 Operator’s Manual

4.2 Liquid Leaks

Worn-out seal in extraction cell end cap

Replace the seal (see Section 5.1).

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. Replace an y O-ri ng wit h a hole size of less than 0.5 mm or a white Teflon O-ring that is discolored (see Section 5.2).

O-rings should last for approximately 50 extractions. To learn how many extractions the ASE 100 has performed, go to the screen (see Section C.2.5).

Leak in solvent flow path

EXTRACTION COUNTERS

If the pump head is leaking, replace the piston seal (see Section 5.5).

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 close d, the relief valve is dirty or worn and must be replaced (see Section 5.6).

Leaking into collection bottle during static cycle

If solvent leaks into the collection bottle during the static cycle, the static valve is dirty or worn and must be replaced (see Section 5.7).

4-8

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4 • Troubleshooting

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Figure 4-1. ASE 100 Plumbing Diagram

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ASE 100 Operator’s Manual

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 th e follo wing locations : gas supply, rear panel, solvent bottle, 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.

4.4 System Stops

Electrical cables improperly installed

Remove the right side panel of the ASE 100 (see Section 5.3). Check that all electrical cables are seated properly in their connectors on the main PCB (printed circuit board).

4-10

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5•Service

This chapter describes routine rep air and repl acement proc edures that the user can perform. All procedures not included here should be performed by Dionex personnel.

NOTE The ASE 100 electronics components cannot be serviced

by the user. All repairs involving the electronics must be performed by Dionex personnel.

Before replacing an y pa rt in th e ASE 100, ref er to the trouble shooting i nformat ion in Chapter 4 of this manual to isolate the cause of the problem. When ordering replacement parts, please specify the ASE 100 serial number listed on the model data label on the rear panel. To contact Dionex in the U.S., call 1-800-346-6390. Outside the U.S., call the nearest Dionex office.

Substituting non-Dionex parts may impair the performance of the ASE 100, thereby voiding the product warranty. Refer to the warranty statement in the Dionex Terms and Conditions for more information.

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ASE 100 Operator’s Manual

5.1 Replacing the Seal in the Cell End Cap

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.

2. Remove the snap ring from the end ca p, using the snap ring tool (P/N 056684) provided in the ASE 100 Ship Kit (P/N 059397).

a. Insert the pointed ends of the tool into the two holes in the snap

ring.

b. Squeeze the handles of the tool together to release the tension on

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

c. Carefully release the handl es of the tool and remov e the ring from

the tool.

3. Remove the cap insert. Remove the s eal from the groove in the bottom of the cap insert.

5-2

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

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

6. Place the stainless steel frit (either cleaned or new) into the bottom of the end cap.

7. Press a new seal into the bottom of the cap insert.

8. Align the pins in the cap insert with the grooves in the end ca p and t hen place the insert, with the seal facing down, into t he end cap.

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5•Service

9. With the cap assembly upright on the workbench, install the snap ring:

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Figure 5-1. Extraction Cell Assembly

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.

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5.2 Replacing the Cell O-Ring

Be careful not to scratch the int erior 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. Use the small flathead screwdriver (P/N 046985) provided in the ASE 100 Ship Kit (P/N 059397) to remove worn O-rings. To do so, insert the tip of the screwdriver into the end cap and carefully pick out the O-ring.

2. Place a new O-ring (Teflon: P/N 049457, pkg. of 50; Viton: P/N 056325, pkg. of 50) ov er the opening in the end of the ce ll cap and press it into place, using the O-ring insertion tool (P/N/ 049660) (see Figure 5-2).

5-4

Figure 5-2. Installing the Cell O-Ring

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5.3 Removing the Right Side Panel

Many parts that the user can service (the pump check valves, etc.) are located behind the panel on the right side of the ASE 100.

To remove the right side panel:

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

5•Service

3. Toggle the needle switch to the

position. If a collection bottle is installed,

remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel.

5. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each h and under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e tri m panel pops off the ball stu ds that secure it to the system.

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Figure 5-3. Removing the Lower Trim Panel

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ASE 100 Operator’s Manual

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

5-6

Figure 5-4. Depressio n in Lower Trim Panel

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6. Remove the right side panel of the ASE 100: a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). Push the screwdriver in until the right side panel slides back about 1/2 inch.

damage to the panel, do not let the panel fall onto the workbench.

c. R emove the right side panel from the system and s et it aside.

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To prevent scratches or other

To reinstall 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. Carefully align the lower trim panel with the edges of the instrument, and then

gently push the panel into place.

4. Reinstall the waste bottle.

5. Turn on the ASE 100 main power switch.

6. Reconnect the gas source at the ASE 100 rear panel and turn on the gas

supply.

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Figure 5-5. Removing the Right Side Panel

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5.4 Cleaning and/or Replacing Pump Check Valves

5.4.1 Removing the Pump

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

3. Toggle the needle switch to the

position. If a collection bottle is

installed, remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100

rear panel.

5. Remove the lower trim panel of the ASE 100:

a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each hand under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e trim panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

5-8

6. Remove the right side panel of the ASE 100:

a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). 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.

c. R emove the right side panel from the system and s et it aside.

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7. Disconnect the red tubing and the transparent blue tubing from the

two black elbow press fittings on top of the pump (see Figure 5-6).

8. Using a 1/4-inch open-end wrench, disconnect the stainless steel

fitting from the outlet check valve (see Figure 5-6).

9. Disconnect the PEEK fitting from the inlet check valve, by hand (see

Figure 5-6).

10. Disconnect the gray cable from the pump PC board (see Figure 5-6).

11. Using a 3 mm hex-screw driver (P/N 060154), remove the screws in the left and right end plates (see Figure 5-6) that secure the pump to the component panel.

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Figure 5-6. ASE 100 Pump

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5.4.2 Rem oving the Check Valves

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

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 housing. Remove the housing, and then remove the check valve cartridge from the housing.

5.4.3 Cleaning the Check Valves

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

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

5.4.4 Reinstalling the Inlet Check Valve

1. The inlet check valve assembl y h ousing has a 1/4-2 8 port . (Thi s is the larger of the two ports.) Place the inlet check valve cartridge (P/N 047755) in the inlet check valve housing so that the double-hole end of the cartridge is visible.

check valve

inlet

check valve

outlet

5-10

NOTE When correctly installed, liquid enters the

check valve through the large single hole and exits through the small double holes.

2. Install the c heck valve assembly. Tighten the check valve assembly just enough to seat (25 in-lb torque); tighten a little more only if it leaks.

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

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5.4.5 Reinstalling the Outlet Check Valve

1. The outlet check valve a ssembly housing has a 10-32 port. (This is the smaller of the two ports.) Place the outlet check valve cartridge (P/N 057346) in the outlet check valve housing so that the arrow points inwa rd.

NOTE When correctly installed, the arrow on the

outlet check valve housing points away from the pump.

2. With the pump inverted, reinstall the check valve assembly. Tighten the check valve just enough to seat (25 in-lb torque); tighten a little more only if it leaks.

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

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5.4.6 Reinstalling the Pump

1. Reinstall the pump on the component panel.

2. Reconnect the red gas line to the left pre ss 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 electrical connector to the pump PC board.

5.4.7 Completing the Procedure

1. Reinstall the right side panel: a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he sl ots in the chassis. Pull the panel forward until it locks into place.

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

2. Carefully align the lower trim pan el with the edges of the inst rument, and then gently push the panel into place.

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3. Reinstall the waste bottle.

4. Turn on the ASE 100 main power switch.

5. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply.

6. Rinse the system (see Section 3.1.7) and check that the pump flow is normal.

If cleaning the check valves does not eliminate the problem, replace both check valve cartridges (inlet check valve cartridge, P/N 047755; outlet check valve cartridge, P/N 057346).

5.5 Replacing the Piston Seal

5.5.1 Removing the Pump

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

3. Toggle the needle switch to the

position. If a collection bottle is

installed, remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel.

5. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each hand under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e trim panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

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e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

6. Remove the right side panel of the ASE 100: a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located between the two screw

holes (see Figure 5-5). Push the screwd ri ver in until the right side panel slides back about 1/2 inch.

damage, do not let the panel fall onto the workbench.

c. R emove the right side panel from the system and s et it aside.

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

8. Using a 1/4-inch open-end wrench, disconnect the stainless steel fitting from the outlet check valve (see Figure 5-6).

9. Disconnect the PEEK fitting from the inlet check valve (by hand).

10. Disconnect the gray cable from the pump PC board.

To prevent scratches or other

11. Remove the two screws in the e nd plates (see Figure 5-6) t hat secure the pump to the component panel.

5.5.2 Replacing the Piston Seal

1. Using a 3-mm hex driver or wrench, loosen and remove the two screws securing the pump head to the body.

2. Slide the pump head straight off the pump.

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

3. Turn the pump head upside down. The tan piston guide should drop out of the head; if it does not, gently tap the head on the lab bench to dislodge the guide. Save the piston guide (it will be reinstalled in Step 7).

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4. If tapping the head on the bench does not remove the piston guide, use the wooden end of a cot ton-tipped s wab to pry th e guide out of the pump head. Discard the used piston guide.

5. To remove the orange piston seal from the pump head, insert the wooden end of a cotton-t ipp ed swab and pry out the seal. Discar d the seal.

6. Hold the new piston seal (P/N 047583) over the cavity in the pump head, center the seal, and drop it into place.

7. If the piston guide was easily removed from the pump head (Step 3), place the original piston guide on top of the piston seal and firmly press it into place. This also seats the piston seal in the pump head.

If you had to pry the piston guide out of the pump head (Step 4), install a new piston guide (P/N 049014) 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.

5.5.3 Reinstalling the Pump

1. Reinstall the pump on the component panel.

2. Reconnect the red gas line to the left pre ss 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. Connect the electrical connector to J8 on the main board.

5.5.4 Completing the Procedure

1. Reinstall the right side panel: a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he s lot s i n t h e chassis. Pull the panel forward until it locks into place.

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

2. Carefully align the lower trim pan el with the edges of the inst rument, and then gently push the panel into place.

3. Reinstall the waste bottle.

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4. Turn on the ASE 100 main power switch.

5. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply.

5.6 Replacing the Relief Valve

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

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3. Toggle the needle switch to the

position. If a collection bottle is installed,

remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel.

5. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each h and under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e tri m panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

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ASE 100 Operator’s Manual

6. Remove the right side panel of the ASE 100: a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). Push the screwdriver in until the right side panel slides back about 1/2 inch.

damage to the panel, do not let the panel fall onto the workbench.

c. R emove the right side panel from the system and s et it aside.

7. The relief valve is installed in the upper left corner of the component panel

(see Figure 5-7). Disconnect the green gas tubing from the elbow press fitting on the valve.

8. Disconnect the stainless steel line from t he right side of the v alve. (Thi s tubing

connects to the pump transducer.)

To prevent scratches or other

5-16

Figure 5-7. Connections to the Relief Valve

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9. Disconnect the stainless steel line from the left side of the valve. (This tubing connects to the upper AutoSeal tip.)

10. Disconnect the green PEEK waste line from the top of the valve.

11. Loosen the Allen hex screw (9/64-inch) on the clamp ring below the valve base.

12. Lif t the old valve off the valve base.

13. Lower the new relief valve (P/N 048889) onto the valve base. Tighten the Allen hex screw on the clamp ring.

14. Reconnect all of the lines.

15. Reinstall the right side panel:

a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he sl ots in the chassis. Pull the panel forward until it locks into place.

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

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

17. Reinstall the waste bottle.

18. Turn on the ASE 100 main power switch.

19. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply.

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ASE 100 Operator’s Manual

5.7 Replacing the Static Valve

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

3. Toggle the needle switch to the

position. If a collection bottle is installed,

remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel.

5. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each hand under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e trim panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

6. Remove the right side panel of the ASE 100:

5-18

a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). 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.

c. R emove the right side panel from the system and s et it aside.

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7. The static valve is installed in the lower left corner of the component panel (see Figure 5-8). Disconnect the ora nge t ubing from t he el bo w pr ess fitting on the valve.

8. Disconnect the stainless steel line from the right side of the valve. (This line connects to the source needle.)

9. Disconnect the stainless steel line (P/N 059821) from the top of the valve. (This line c onnects to the lower AutoSeal tip.)

10. Loosen the Allen hex screw (9/64-inch) on the clamp ring below the valve base.

11. Lif t the old valve off the valve base.

12. Lower the new static valve (P/N 048778) onto the valve base. Tighten the Allen hex screw on the clamp ring.

13. Reconnect all of the lines.

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Figure 5-8. Connections to the Static Valve

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ASE 100 Operator’s Manual

14. Reinstall the right side panel: a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he s lot s i n t h e chassis. Pull the panel forward until it locks into place.

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

15. Carefully align the lower trim panel with the edges of the instrument, and then

gently push the panel into place.

16. Reinstall the waste bottle.

17. Turn on the ASE 100 main power switch.

18. Reconnect the gas source at the ASE 100 rear panel and turn on the gas

supply.

5.8 Replacing the Source Needle

1. Turn off the ASE 100 main power switch.

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

5-20

3. Toggle the needle switch to the

position. If a collection bottle is installed,

remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel.

5. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each hand under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e trim panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

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e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

6. Remove the right side panel of the ASE 100: a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). Push the screwdriver in until the right side panel slides back about 1/2 inch.

damage to the panel, do not let the panel fall onto the workbench.

c. R emove the right side panel from the system and s et it aside.

7. Using a 1/4-inch open-end wrench, di sconne ct t he st ainle ss stee l f i tti ng on t he

right side of the static valve (see Figure 5-8).

8. The needle assembly is secured to the inner front panel. The source needle

assembly is on the right side of the needle block (see Figure 5-9). Disconnect the 1/4-inch stainless steel fitting (part of the source needle assembly) from the needle block.

To prevent scratches or other

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Figure 5-9. Vent and Source Needles

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ASE 100 Operator’s Manual

9. Pull up the source needle assembly to remove the needle.

10. Insert the new sourc e needle asse mbly (P/N 059923) into the top of the needle block. Verify that the eye of the needle is toward the front of the needle block.

Be careful when handling the source needle. The tip of the needle is sharp; in addition, it is fragile and can easily be bent.

11. Reconnect the 1/4-inch stainless steel fitting to the needle block.

12. Reconnect the stainless steel tubing to the right side of the static valve.

13. Reinstall the right side panel:

a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he s lot s i n t h e chassis. Pull the panel forward until it locks into place.

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

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

15. Reinstall the waste bottle.

5-22

16. Turn on the ASE 100 main power switch.

17. Reconnect the gas source at the ASE 100 rear panel and turn on the gas supply.

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5.9 Replacing the Solvent Outlet Line

1. Make sure the ASE 100 power is turned on. (This ensures that the AutoSeal mechanism is lowered.)

2. Unscrew the waste bottle from the bottle cap and set the bottle aside.

5•Service

3. Toggle the needle switch to the

position. If a collection bottle is installed,

remove the bottle from the bottle holder and set it aside.

4. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel and let the s ystem vent.

5. Turn off the ASE 100 main power switch.

6. Check that the cell door is closed.

7. Remove the lower trim panel of the ASE 100:

a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each h and under th e top edg es of t he

bottle holders, near the

WASTE

and

COLLECTION

labels (see

Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e tri m panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

Doc. 031842-01 5/02

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

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ASE 100 Operator’s Manual

8. Remove the right side panel of the ASE 100: a. U sing a Phillip s screwdriver, remove the two screws on the inner

front panel, near the needle assembly (see Figure 5-5).

b. Insert a screwdriver into the hole located beneath the top screw

hole (see Figure 5-5). Push the screwdriver in until the right side panel slides back about 1/2 inch.

damage to the panel, do not let the panel fall onto the workbench.

c. R emove the right side panel from the system and s et it aside.

9. Remove the left side panel of the ASE 100: a. U sing a Phillips screwdriver, remove the two screws in the uppe r

left section of the inner front panel (see Figure 5-10).

b. Gently slid e the left side panel back ward as far as it can travel

(about 1/2 inch). Pull the panel to the left and remove it from the system.

Be careful not to damage the mounting tabs on the left side panel.

To prevent scratches or other

5-24

Figure 5-10. Removing the Left Side Panel

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10. Locate the static valve in the lower left corner of the component panel (see Figure 5-11). The stainless steel solvent outlet line is connected to the top of the static valve. (The other end of the solvent ou tlet line is connected to the lower AutoSeal tip.)

Remove the fitting that connects the solvent outlet line to the static valve. Carefully feed the tubing through the small round opening in the component panel (see Figure 5-11) and into the left side of the instrument.

NOTE Many tubes and wires are connected to both sides of the

component panel. Be careful not to disconnect or unseat any of the connections.

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Figure 5-11. Solvent Outlet Line–Static Valve Connection

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11. The stainless steel solvent outlet line is connected to the lower AutoSeal tip (see Figure 5-12). From there, the solvent outlet line is routed through a vertical guide .

5-26

Figure 5-12. Lower AutoSeal Tip–Solvent Outlet Line Connection

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12. Loosen the three Phillips screws that secure the cover to the vertical guide. Slip the solvent outlet line out the left side of the cover (see Figure 5-13).

Figure 5-13. Removing the Solvent Outlet Line from the Vertical Guide

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13. Lift the lower AutoSeal tip out of the support tube located on top of the air cylinder shaft (see Figure 5-14).

14. Note the indentation alo ng the top e dge of the s upport tub e, where it meets the lower AutoSeal tip (see Figure 5-14). Insert the tip of a small flathead screwdriver into the indentation and twist the screwdr iver just enough to raise and loosen the lower AutoSeal tip.

15. Remove the old solvent outlet line. Remove the lower AutoSeal tip from the outlet line.

16. Screw the lower AutoSeal tip onto the end of the new solvent outlet line (P/N 059821). While holding the solvent line securely with a 1/4-inch wrench, use a 3/8-inch open-end wrench to tighten the AutoSeal tip.

17. Reinstall the AutoSeal tip in the support tube on top of the air cylinder.

18. Route the new solvent outlet line through the vertical guide and reinstall the Phillips screw s in the guide.

19. Connect the other end of the new solvent outlet line to the top of the static valve. Make sure that there is adequate clearance above and below the solvent line. During operation, the solvent line must be a ble to move up and down freely.

5-28

Figure 5-14. Support Tube for Lower AutoSeal Tip

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20. Reinstall the left side panel: a. Hold the panel against the l eft side of the system. Eng age the

small tabs on the to p and bottom of the panel wit h t he sl ots in the chassis. Pull the panel forward until it locks into place.

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

21. Reinstall the right side panel: a. Hold the panel against the right side of the system. Engage the

small tabs on the to p and bottom of the panel wit h t he sl ots in the chassis. Pull the panel forward until it locks into place.

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

22. Carefully align the lower trim panel with the edges of the instrument, and then

gently push the panel into place.

23. Reinstall the waste bottle.

24. Turn on the ASE 100 main power switch.

25. Reconnect the gas source at the ASE 100 rear panel and turn on the gas

supply.

5.10 Replacing the Lower AutoSeal Tip

1. Make sure the ASE 100 power is turned on. (This ensures that the AutoSeal mechanism is lowered.)

2. Toggle the needle switch to the remove the bottle from the bottle holder and set it aside.

3. Turn off the gas supply. Disconnect the gas source at the ASE 100 rear panel and let the s ystem vent.

4. Turn off the ASE 100 main power switch.

5. Check that the cell door is closed.

6. Unscrew the waste bottle from the bottle cap and set the bottle aside.

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position. If a collection bottle is installed,

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7. Remove the lower trim panel of the ASE 100: a. Stand directly in front of the ASE 100, with both hands facing

palm upwards.

b. Hook the first two fi ngers of each hand under th e top edg es of t he

bottle holders, near the Figure 5-3).

c. Brace your thumbs against the bottom of the cell door and the

control panel. Pul l for war d unti l the to p of th e trim panel pops off the ball stu ds that secure it to the system.

d. Note the small round depressions on t he le ft and r ight s ides of the

trim panel, near the bottom (see Figure 5-4). Place your index fingers in these depressions and pull forward until the bottom of the trim panel pops off.

e. Pull the trim panel comple tely of f, e xpos ing t he inne r front pa nel ,

and set the trim panel aside.

8. Remove the left side panel of the ASE 100:

WASTE

and

COLLECTION

labels (see

a. U sing a Phillips screwdriver, remove the two screws in the uppe r

left section of the inner front panel (see Figure 5-10).

b. Gently slid e the left side panel back ward as far as it can travel

(about 1/2 inch). Pull the panel to the left and remove it from the system.

Be careful not to damage the mounting tabs on the left side panel.

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Doc. 031842 -01 5/02

Dionex ASE 100 Operator's Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Contents

1.1 Overview

1.2 About This Manual

1.2.1 Typefaces

1.2.2 Saf et y Me ss ages and Notes

1.3 Safety Labels

2.1 Operating Features

2.1.1 Control Panel Screen

2.1.2 Contro l Panel Keypad

2.1.3 Extrac tion Cells and Rinse Cells

2.1.4 Collection Bottle

2.1.5 Solvent Bottle

2.1.6 Waste Bottle

2.2 Rear Panel

2.3 Extraction Process

2.4 Method Control

2.5 Preprogrammed Methods

3.1 Preparing to Run an Extraction

3.1.1 Selecting and Preparing Solvent

3.1.2 Filling the Solvent Bottle

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 Bottle

3.1.7 Rinsing/Priming the System

3.2 Editing a Custom Method (1–24)

3.3 Guidelines for Method Development

3.4 Running an Extraction

3.5 Post-Extraction Procedures

3.5.1 Cleaning the Cells

3.5.2 Processing Extracts

3.6 Aborting a Run

3.7 Routine Maintenance

3.7.1 Daily Maintenance

3.7.2 Periodic Maintenance

3.8 Shutdown

4.1 Error Messages

4.2 Liquid Leaks

4.3 Gas Leaks

4.4 System Stops

5.1 Replacing the Seal in the Cell End Cap

5.2 Replacing the Cell O-Ring

5.3 Removing the Right Side Panel

5.4 Cleaning and/or Replacing Pump Check Valves

5.4.1 Removing the Pump

5.4.2 Rem oving the Check Valves

5.4.3 Cleaning the Check Valves

5.4.4 Reinstalling the Inlet Check Valve

5.4.5 Reinstalling the Outlet Check Valve

5.4.6 Reinstalling the Pump

5.4.7 Completing the Procedure

5.5 Replacing the Piston Seal

5.5.1 Removing the Pump

5.5.2 Replacing the Piston Seal

5.5.3 Reinstalling the Pump

5.5.4 Completing the Procedure

5.6 Replacing the Relief Valve

5.7 Replacing the Static Valve

5.8 Replacing the Source Needle

5.9 Replacing the Solvent Outlet Line

5.10 Replacing the Lower AutoSeal Tip