Dionex ASE 100 Bedienungsanleitung

ASE 100®

ACCELERATED SOLVENT EXTRACTOR

OPERATOR'S MANUAL

Document No. 031842

Revision 01

May 2002

Printed in the United States of America.

This publication is protected by federal copyright law. No part of this publication

may be copied or distributed, transmitted, transcribed, stored in a retrieval system, or

transmitted into any human or computer language, in any form or by any means,

electronic, mechanical, magnetic, manual, or otherwise, or disclosed to third parties

without the express written permission of Dionex Corporation, 1228 Titan Way,

Sunnyvale, California 94088-3603 U.S.A.

DISCLAIMER OF WARRANTY AND LIMITED WARRANTY

THIS PUBLICATION IS PROVIDED “AS IS” WITHOUT WARRANTY OF

ANY KIND. DIONEX CORPORATION DOES NOT WARRANT,

GUARANTEE, OR MAKE ANY EXPRESS OR IMPLIED

REPRESENTATIONS REGARDING THE USE, OR THE RESULTS OF THE

USE, OF THIS PUBLICATION IN TERMS OF CORRECTNESS, ACCURACY,

RELIABILITY, CURRENTNESS, OR OTHERWISE. FURTHER, DIONEX

CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION

AND TO MAKE CHANGES FROM TIME TO TIME IN THE CONTENT

HEREINOF WITHOUT OBLIGATION OF DIONEX CORPORATION TO

NOTIFY ANY PERSON OR ORGANIZATION OF SUCH REVISION OR

CHANGES.

TRADEMARKS

AutoSeal™ is a trademark and ASE®100 is a registered trademark of Dionex

Corporation.

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

Company.

PRINTING HISTORY

Revision 01, May 2002

Doc. 031842-01 5/02 i

Contents

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

2.1.3 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

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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ii Doc. 031842-01 5/02

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

Contents

Doc. 031842-01 5/02 iii

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

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

ASE 100 Accelerated Solvent Extractor

iv Doc. 031842-01 5/02

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

Contents

Doc. 031842-01 5/02 v

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

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

ASE 100 Accelerated Solvent Extractor

vi Doc. 031842-01 5/02

Doc. 031842-01 5/02 1-1

1 • Introduction

1.1 Overview

The ASE®100 Accelerated Solvent Extractor is a system for extracting either

organic or inorganic compounds from a variety of solid and/or semisolid samples.

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.

Figure 1-1. ASE 100 Accelerated Solvent Extractor

ASE 100 Operator’s Manual

1-2 Doc. 031842-01 5/02

The ASE 100 is designed to minimize the amount of solvent used without

sacrificing the speed of extraction or ease of operation. Samples are extracted one

at a time, and the extraction process is typically completed in 15 to 25 minutes.

All functions are controlled from the ASE 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:

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.

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 additional

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 cell size. For details, see Section 2.1.3.

_Before beginning an extraction, specify the new cell size on the SETUP screen

(see Section C.1.3).

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

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