Dionex ASE 150 Operator's Manual
ASE® 150
Accelerated Solvent Extractor
Operator's Manual
Document No. 065207
Revision 02
September 2008
©2008 by Dionex Corporation
All rights reserved worldwide.
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 of Dionex Corporation. ASE 150 is a registered trademark
of Dionex Corporation.
Acrobat, Adobe, and Adobe Reader are registered trademarks of Adobe Systems,
Incorporated.
C-2000 and Hastelloy are registered trademarks of Haynes International, Inc.
PEEK is a trademark of Victrex PLC.
Perlast is a registered trademark of Precision Polymer Engineering, Ltd.
Teflo n and Viton
are registered trademarks of E. I. duPont de Nemours & Company.
PRINTING HISTORY
Revision 01, April 2008
Revision 02, September 2008
1 • Introduction
1.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.2 About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.2.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.2.2 Safety Messages and Notes . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.3 Safety and Regulatory Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.4 Safety Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2•Description
2.1 Operating Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.1.1 Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Contents
2.1.2 Sample Cells and Rinse Cells . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1.3 Collection Vessels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.1.4 Solvent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.5 Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.2 Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3 ASE 150 Extraction Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.4 Method Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
2.5 Preprogrammed Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
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ASE 150 Operator’s Manual
3 • Operation and Maintenance
3.1 Preparing to Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .25
3.1.1 Selecting and Preparing Solvent . . . . . . . . . . . . . . . . . . . . . . . .25
3.1.2 Filling the Solvent Reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . .29
3.1.3 Preparing the Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31
3.1.4 Installing the Cell Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
3.1.5 Filling the Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .37
3.1.6 Installing the Collection Vessel . . . . . . . . . . . . . . . . . . . . . . . . .39
3.1.7 Installing the Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
3.2 Running . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
3.2.1 Selecting the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
3.2.2 Selecting the Cell Size . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42
3.2.3 Verifying the Cell Type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .43
3.2.4 Starting the Run and Checking the Oven Status . . . . . . . . . . . .43
3.2.5 Installing the Sample Cell in the Cell Holder . . . . . . . . . . . . . .44
3.2.6 Completing the Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .45
3.3 Performing Post-Run Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46
3.3.1 Cleaning the Sample Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46
3.3.2 Processing Extracts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .46
3.4 Stopping a Run . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47
3.5 Rinsing/Priming the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .48
3.6 Editing a Custom Method (Methods 1 through 24) . . . . . . . . . . . . . . . .49
3.7 Developing a New Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .52
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3.8 Performing Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.8.1 Daily Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.8.2 Periodic Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.8.3 Annual Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
3.9 Shutting Down . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
4 • Troubleshooting
4.1 Error Messages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
4.2 Liquid Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
4.3 Gas Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
4.4 Stopped System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
Contents
5•Service
5.1 Replacing Tubing and Fittings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
5.2 Replacing the Cell End Cap Seal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
5.3 Replacing the Cell End Cap O-Ring . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
5.4 Removing the Right-Side Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
5.5 Replacing Pump Check Valve Cartridges . . . . . . . . . . . . . . . . . . . . . . . 75
5.5.1 Before Beginning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
5.5.2 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
5.5.3 Removing the Check Valves and Cartridges . . . . . . . . . . . . . . 76
5.5.4 Installing New Check Valve Cartridges . . . . . . . . . . . . . . . . . . 77
5.5.5 Reinstalling the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . 77
5.5.6 Cleaning the Check Valves . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
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ASE 150 Operator’s Manual
5.5.7 Reinstalling the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78
5.5.8 Completing the Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . .78
5.6 Replacing Pump Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79
5.6.1 Before Beginning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79
5.6.2 Removing the Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .79
5.6.3 Replacing the Piston High-Pressure Seal . . . . . . . . . . . . . . . . .79
5.6.4 Replacing the Piston Air Seal . . . . . . . . . . . . . . . . . . . . . . . . . .81
5.6.5 Reinstalling the Pump and Completing the Procedure . . . . . . .83
5.7 Replacing the Pressure Relief Valve . . . . . . . . . . . . . . . . . . . . . . . . . . .84
5.8 Rebuilding the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .86
5.8.1 Removing the Static Valve from the System . . . . . . . . . . . . . .88
5.8.2 Disassembling the Static Valve Body . . . . . . . . . . . . . . . . . . . .90
5.8.3 Installing the New Seals . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .92
5.8.4 Reassembling the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . .93
5.8.5 Reinstalling the Static Valve . . . . . . . . . . . . . . . . . . . . . . . . . . .97
5.9 Replacing the Source Needle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .99
5.10 Replacing the Main Power Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . .102
A • Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103
A.1 Electrical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103
A.2 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .103
A.3 Physical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104
A.4 Pneumatic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104
A.5 Front Panel Display and Keypad . . . . . . . . . . . . . . . . . . . . . . . . . . . . .104
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Contents
A.6 Sample Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104
A.7 Collection Vessels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104
A.8 Interior Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105
B • Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107
B.1 Facility Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 107
B.2 Installation Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
B.2.1 Connecting the Nitrogen Gas Source . . . . . . . . . . . . . . . . . . . 108
B.2.2 Connecting the Drain Hose . . . . . . . . . . . . . . . . . . . . . . . . . . . 110
B.2.3 Checking the Oven Voltage Switches. . . . . . . . . . . . . . . . . . . 110
B.2.4 Connecting the Power Cord . . . . . . . . . . . . . . . . . . . . . . . . . . 111
B.2.5 Checking Pressure Readings. . . . . . . . . . . . . . . . . . . . . . . . . . 112
B.2.6 Connecting the Solvent Reservoir. . . . . . . . . . . . . . . . . . . . . . 113
B.2.7 Installing the Waste Bottle . . . . . . . . . . . . . . . . . . . . . . . . . . . 115
B.2.8 Adjusting the Cell Holder . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
B.2.9 Selecting Setup Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118
B.2.10 Rinsing the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
C • User Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125
C.1 Operational Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
C.1.1 Menu Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
C.1.2 Status Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127
C.1.3 Setup Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128
C.1.4 Method Editor Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
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ASE 150 Operator’s Manual
C.2 Diagnostic Screens . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
C.2.1 Diagnostics Menu. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
C.2.2 Sensors Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .132
C.2.3 Regulators Screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .133
C.2.4 Hydrocarbon Sensor Screen. . . . . . . . . . . . . . . . . . . . . . . . . . .134
C.2.5 Extraction Counters Screen . . . . . . . . . . . . . . . . . . . . . . . . . . .135
C.2.6 Moduleware Screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .136
D • Reordering Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . .137
E • Theory of ASE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .141
E.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .141
E.2 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .143
E.3 Method Optimization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .145
E.3.1 Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .145
E.3.2 Extraction Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .148
E.4 Method Development . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .151
E.5 Selectivity in ASE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .152
E.6 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .157
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1.1 Overview
1 • Introduction
The ASE
®
150 Accelerated Solvent Extractor is a system for extracting either
organic or inorganic compounds from a variety of solid or semisolid samples at a
variety of pH values. The ASE 150 can be used with organic solvent, aqueous
buffer, water, and small amounts of mineral acids. The ASE 150 accelerates the
traditional extraction process by using solvent at elevated temperatures and
pressures. Pressure is maintained in the sample cell to maintain the heated solvent
in a liquid state during the extraction. After heating, the extract is rinsed from the
sample cell into a collection vessel and is ready for analysis.
Solvent
Reservoir
Sample Cell
and Oven
Location
Waste
Figure 1-1. ASE 150 Accelerated Solvent Extractor
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Collection Vessel
ASE 150 Operator’s Manual
The ASE 150 is designed to minimize the amount of solvent used without
sacrificing the speed of extraction or ease of operation. Samples are extracted one
at a time, and the extraction process is typically completed in 15 to 25 minutes.
All functions are controlled from the ASE 150 front panel.
Built-in safety diagnostics monitor the system during operation. If a problem
occurs, the front panel displays an error message that identifies the problem. In
addition, the method currently running is aborted and basic system functions are
shut down until the situation is corrected.
1.2 About This Manual
1.2.1 Overview
The electronic version (i.e., PDF file) of the ASE 150 operator’s manual
contains numerous hypertext links that can take you to other locations
within the file. These links include:
• Table of contents entries
• Index entries
• Cross-references (underlined in blue) to sections, figures, tables, etc.
If you are not familiar with how to navigate PDF files, refer to the Help
system for Adob
Chapter 1
Introduction
Chapter 2
Description
Chapter 3
Operation and
Maintenance
Chapter 4
Troubleshooting
Chapter 5
Service
Appendix A
Specifications
2 Doc. 065207-02 9/08
e® Acrobat® or Adobe Reader® for assistance.
Introduces the ASE 150; explains the conventions used in
this manual, including safety-related information.
Describes ASE 150 operating features and the extraction
process.
Provides operating instructions and routine preventive
maintenance procedures.
Lists error messages and how to troubleshoot them; lists
operating problems and how to resolve them.
Provides step-by-step instructions for routine service and
parts replacement procedures that the user can perform.
Provides specifications and installation site requirements.
1 • Introduction
Appendix B
Installation
Appendix C
User Interface
Appendix D
Reordering
Information
Appendix E
Theory of ASE
Describes how to install the ASE 150.
Illustrates and describes the display screens on the ASE
150 front panel.
Lists spare parts for the ASE 150.
Describes the theory behind performing extractions with
ASE.
1.2.2 Safety Messages and Notes
This manual contains warnings and precautionary statements that can
prevent personal injury and/or damage to the ASE 150 when properly
followed. Safety messages appear in bold type and are accompanied by
icons, as shown below.
Indicates an imminently hazardous situation which, if not avoided, will
result in death or serious injury.
Indicates a potentially hazardous situation which, if not avoided, may
result in death or serious injury.
Indicates a potentially hazardous situation which, if not avoided, may
result in minor or moderate injury. Also used to identify a situation or
practice that may seriously damage the instrument, but will not cause
injury.
Indicates that the function or process of the instrument may be
impaired. Operation does not constitute a hazard.
Messages d’avertissement en français
Signale une situation de danger immédiat qui, si elle n'est pas évitée,
entraînera des blessures graves à mortelles.
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ASE 150 Operator’s Manual
Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures graves à mortelles.
Signale une situation de danger potentiel qui, si elle n'est pas évitée,
pourrait entraîner des blessures mineures à modérées. Également
utilisé pour signaler une situation ou une pratique qui pourrait
gravement endommager l'instrument mais qui n'entraînera pas de
blessures.
Warnhinweise in Deutsch
Bedeutet unmittelbare Gefahr. Mißachtung kann zum Tod oder
schwerwiegenden Verletzungen führen.
Bedeutet eine mögliche Gefährdung. Mißachtung kann zum Tod oder
schwerwiegenden Verletzungen führen.
Bedeutet eine mögliche Gefährdung. Mißachtung kann zu kleineren
oder mittelschweren Verletzungen führen. Wird auch verwendet, wenn
eine Situation zu schweren Schäden am Gerät führen kann, jedoch
keine Verletzungsgefahr besteht.
Notes
Informational messages also appear throughout this manual. These are
labeled NOTE and are in bold type.
NOTE NOTES call attention to certain information. They alert
the user to an unexpected result of an action, suggest
how to optimize instrument performance, etc.
4 Doc. 065207-02 9/08
1.3 Safety and Regulatory Information
The ASE 150 was manufactured by Dionex Corporation at the following location:
527 Lakeside Drive, Sunnyvale, CA 94088-3603 U.S.A. The ASE 150 is designed
for solvent extraction applications and should not be used for any other purpose.
Operation of an ASE 150 in a manner not specified by Dionex may result in
personal injury.
If you have a question regarding appropriate usage, contact Dionex before
proceeding. In the U.S., call 1-800-346-6390 and select the Technical Support
option. Outside the U.S., call the nearest Dionex office.
1.4 Safety Labels
The cTUVus Mark safety label and the CE Mark label on the ASE 150 indicate
that the ASE 150 is in compliance with the following standards.
EMC Susceptibility and Emissions
• EN 61326-1:2006
1 • Introduction
Safety
• CAN/CSA-C22.2 No. 61010-1:2004
• EN 61010-1:2001
• UL 3101-1/10.93
• UL 61010-1:2004
The symbols below appear on the ASE 150 or on ASE 150 labels.
Alternating current
Primary protective conductor terminal
Secondary protective conductor terminal
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ASE 150 Operator’s Manual
Power supply is on
Power supply is off
Hot surface
Indicates a potential hazard. Refer to the operator’s manual for
an explanation of the hazard and how to proceed.
6 Doc. 065207-02 9/08
2.1 Operating Features
Figure 2-1 illustrates the main operating features of the ASE 150 Accelerated
Solvent Extractor.
2 • Description
1
4
2
6
3
5
7
8
9
Figure 2-1. ASE 150 Operating Features
Solvent Reservoir
1
2
Sample Cell
3
Oven
Control Panel
4
5
Door OPEN Lever
Waste Bottle
6
Needle UP/DOWN Switch
7
Collection Vessel
8
(250-mL bottle shown)
Drip Tray
9
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ASE 150 Operator’s Manual
Solvent Reservoir
A 2-liter solvent reservoir is installed in a recess on top of the ASE 150. The
recess contains a plastic liner that collects any solvent leaks or spills that may
occur and directs them through a drain tube to the rear panel. A drain hose
connects to the drain tube and is routed to a waste container.
Sample Cell
Before a sample is run or a rinse cycle is performed, a sample cell or rinse cell
must be installed in the cell holder on the inside of the cell door. To access the cell
holder, push down on the
Oven
The oven is located behind the cell door. This area also houses the AutoSeal™
tips, which seal the cell during a run.
Control Panel
The ASE 150 control panel includes a display screen and a membrane keypad,
which are used to control ASE 150 operation.
OPEN lever and then pull open the door.
Waste Bottle
The waste bottle is a 250-mL collection bottle that is sealed with a special built-in
cap assembly.
Needle Up/Down Switch
The UP/DOWN toggle switch controls the position of the source and vent needles.
When the needles are in the “down” position, they pierce the collection vessel
septum. The source needle allows the extract to flow from the sample cell into the
collection vessel. The vent needles allow displaced gases to escape to the waste
bottle and the system vent.
Drip Tray
A pull-out drip tray is installed below the oven to collect any liquid leaks that may
occur during a run or rinse cycle.
Collection Vessel
After each extraction, the collection vessel (either a 250-mL collection bottle or a
60-mL collection vial) contains solvent and the analytes extracted from the
sample.
8 Doc. 065207-02 9/08
2 • Description
Safety Shields
The doors on the waste and collection vessel compartments are safety shields that
protect operators in the rare case of a bottle or vial breakage. The doors must be
closed for safe operation.
2.1.1 Control Panel
Use the control panel screen and buttons to control ASE 150 operation.
The screen displays status and operating information. You can edit any
field on the screen that contains a blinking cursor. A field without a
blinking cursor is for display only.
STATUS
SETUP
METHOD EDITOR
DIAGNOSTICS
START
RINSE
STOP
Figure 2-2. ASE 150 Control Panel
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MENU
ASE 150 Operator’s Manual
Button Function
START
RINSE
MENU
STOP
Starts the currently selected method. The LED starts flashing
when the oven is within 1 °C of the set point, indicating it is
okay to load the sample cell into the oven. During the method
run, the LED is lighted, but does not flash. When the method
finishes running (or is aborted), three beeps are emitted and
the LED turns off. See Section 2.4
for details about methods.
Starts a rinse cycle in which about 5 mL of solvent is pumped
through the system. During the rinse cycle, the LED is
lighted. When the rinse cycle is complete (or is aborted),
three beeps are emitted and the LED turns off.
Note: Always install a rinse cell and a collection vessel
before starting a rinse cycle. See Section 3.5
for instructions.
Interrupts the currently running method or rinse cycle and
displays the
ABORT screen. Pressing the button lights the
LED. The LED turns off when you select an option on the
ABORT screen. See Section 3.4 for details.
Exits the screen currently displayed and returns to the screen
one level up in the hierarchy. For example, if the
EDITOR
the
screen is displayed, pressing MENU returns you to
MENU screen. See Figure C-1 for an overview of the
METHOD
screens.
When the cursor is in an editable field, pressing
MENU
discards any change and reverts to the previously selected
parameter.
Selects the field the cursor is currently pointing to. On the
MENU or DIAGNOSTICS screen, this selects and displays a
different screen. On other screens, pressing
ENTER moves
the cursor from the left margin to the first field in that line
that can be edited; it also changes the normal cursor into the
blinking editing cursor.
When the cursor is in an editable field, pressing
ENTER saves
the parameter currently displayed in the field.
Table 2-1. ASE 150 Control Panel Button Functions
10 Doc. 065207-02 9/08
Button Function
Moves the cursor, in the direction of the arrow, to the next
selectable line on the display (if any).
When the cursor is in an editable field, pressing an arrow
button displays the next or previous parameter or numeric
value allowed for the field.
Note: Pressing and holding down an arrow button moves the
cursor continuously through the allowed settings.
Table 2-1. ASE 150 Control Panel Button Functions (Continued)
2.1.2 Sample Cells and Rinse Cells
NOTE Appendix D contains part numbers for cells, bottles,
vials, and other accessories.
Sample Cells
Cell Material Sizes Available (mL) Used For
Stainless steel 1, 5, 10, 22, 34, 66, and
100
Zirconium 66 and 100 Extraction of basic or acidic
2 • Description
Extractions with solvents
matrices, and extractions with
solvents
Sample cells consist of a cell body and two interchangeable caps, which
are screwed onto each end of the cell body. The cell body and end caps
are made of the same material. Inside each end cap is a frit in the same
material as the cell, as well as a PEEK™ seal. During a run, the cell end
caps are compressed by the oven to form a tight seal between the caps and
the cell body.
Always tighten the cell end caps by hand. Use of a wrench or other
tool can damage the cell, as well as the seals inside the cell end caps.
Each cell end cap contains an external O-ring. Teflon® O-rings
(P/N 049457, pkg. of 50) are standard. Use Viton® O-rings (P/N 056325,
pkg. of 50) for dioxins and other high temperature applications.
If Viton external O-rings are installed on the cell end caps, do not use
acetone or other ketones.
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Rinse Cells
Rinse cells are similar in appearance to sample cells, but are blue in color.
During a rinse cycle, solvent passes directly through the rinse cell and
into the collection vessel. For more information about rinse cycles, see
Section 3.5
The rinse cell size must be matched to the size of the sample cell, as
indicated in the table below.
Use this rinse cell: With this sample cell:
Short (P/N 060174) 1 mL, 5 mL, 10 mL, 22 mL, 34 mL
Medium (P/N 060175) 66 mL
Long (P/N 060176) 100 mL
Ordering Sample Cells in Other Sizes
To perform a run with a cell in a different size than the size originally
ordered, order the cells from Dionex. You will also need to order the
Startup Kit appropriate for the new cell size. For cell and Startup Kit part
numbers, see Appendix D
.
.
Note that installation of a different sample cell size will require a few
additional changes:
• Reposition the cell holder to accommodate the new sample cell size,
if required. For instructions, refer to Section B.2.8
.
• Before beginning a run, specify the new cell size on the SETUP screen
(see Section C.1.3
12 Doc. 065207-02 9/08
).
2.1.3 Collection Vessels
The following collection vessels are available:
Collection Vessel Part Number Quantity
60-mL clear vials 048784 Pkg. of 72
60-mL amber vials 048781 Pkg. of 72
60-mL clear graduated vial, Class A 068226 1
60-mL clear graduated vial, Class B 068248 1
250-mL clear bottles 056284 Pkg. of 12
250-mL clear graduated bottle, Class A 068225 1
250-mL clear graduated bottle, Class B 068249 1
Before each run, carefully inspect all collection vessels for chips,
scratches, or cracks. If a collection vessel shows any sign of damage,
do not use it.
Use each nongraduated collection vessel once only. Graduated
collection vessels may be used multiple times, provided they are
undamaged.
La présence de fêlure ou d’égratignures sur les flacons de collecte
doit être vérifiée avant chaque extraction. N’utilisez jamais un flacon
endommagé.
Les flacons non gradués sont à usage unique. Les flacons gradués
peuvent être réutilisés tant qu’ils sont intacts.
Untersuchen Sie vor jedem Lauf alle Sammelgefäße auf
Abplatzungen, Kratzer oder Risse. Wenn ein Sammelgefäß eine
Beschädigung aufweist, sollten Sie es nicht mehr verwenden.
Graduierte Sammelgefäße können mehrfach verwendet werden,
vorausgesetzt sie weisen keine Beschädigung auf.
2 • Description
Use each collection vessel cap and septum once only. This prevents
solvent leaks caused by piercing the septum in the cap multiple times.
An adapter (P/N 066392) is required to install a 60
-mL vial in the
collection vessel area. The adapter is included in the Startup Kits for
1
-mL, 5-mL, 10-mL, 22-mL, and 34-mL sample cells.
The collection vessel caps (used with all bottles and vials) contain a
solvent-resistant septum. During a run, the needle mechanism is lowered
so that the needles pierce the septum, creating a liquid flow path from the
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ASE 150 Operator’s Manual
sample cell to the collection vessel. After a run, the collection vessel
contains solvent and the analytes extracted from the sample.
2.1.4 Solvent Reservoir
The ASE 150 Ship Kit (P/N 066399) includes a 2-liter glass bottle with
shatterproof plastic coating (P/N 045901) and a bottle cap assembly
(P/N 068077) with tubing and fittings for the inlet and outlet connections.
For instructions on how to install the solvent reservoir, see Section 3.1.2
Use only Dionex solvent reservoirs. These are glass bottles with a
shatterproof plastic coating. To prevent operator injury, make sure the
pressure applied to the bottles does not exceed 0.07 MPa (10 psi).
Utilisez uniquement des réservoirs à solvant Dionex. Ce sont des
réservoirs en verre à revêtement incassable en plastique. Veillez à ce
que la pression exercée sur ces réservoirs ne dépasse pas 0,07 MPa.
Verwenden Sie ausschließlich die Lösemittelbehälter von Dionex.
Dabei handelt es sich um Glasbehälter mit einer splittersicheren
Plastikbeschichtung. Vergewissern Sie sich, daß der Druck, der auf
die Behälter ausgeübt wird, 0,07 MPa nicht übersteigt.
.
Never fill the solvent reservoir or disconnect the tubing connections
to the solvent and gas connectors during a run or rinse cycle. At these
times, the solvent reservoir is pressurized. If you remove the bottle
cap, the ASE 150 may not operate to specification.
2.1.5 Waste Bottle
A 250-mL collection bottle (without the cap) is used to collect system
waste. Three vent lines, one from the pressure relief valve and two from
the needle mechanism, are connected to the built-in waste bottle cap. The
waste bottle collects the small amounts of condensed solvent vented
through these lines.
A vent outlet line is also connected to the waste bottle cap; gas is vented
out this line to the rear panel. The ASE 150 Ship Kit (P/N 066399)
provides vent tubing (P/N 053514) that you can connect to the vent outlet
on the rear panel (see Figure 2-3
NOTE Check the waste bottle daily and empty whenever
necessary.
14 Doc. 065207-02 9/08
) and then route to a vent hood.
2.2 Rear Panel
Figure 2-3 illustrates the rear panel of the ASE 150.
2 • Description
Power
1
2
3
6
4
5
1
Oven Voltage
2
Switches
Model Data
3
Label
Nitrogen Gas
4
Inlet
5
Vent Outl et
Drain
6
Figure 2-3. ASE 150 Rear Panel
• The POWER switch provides on/off control of the main power for the system.
The power receptacle also includes the fuse holder. For instructions on how to
replace the fuses, see Section 5.10
.
• The oven voltage switches must be set to match the voltage from the power
source at the ASE 150 installation site. For instructions on how to set the
switches, see Section B.2.3
.
• The model data label lists fuse and power information, as well as the ASE 150
serial number. You will be asked to provide the serial number when ordering
replacement parts for the system.
• The NITROGEN connector is connected to a nitrogen supply regulated to
between 0.97 and 1.38 MPa (140 and 200 psi); 1.03 MPa (150 psi) is
recommended. For installation instructions, see Section B.2.1
.
• The VENT connector provides a connection for the vent outlet line. For
installation instructions, see Section B.2.1
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.
ASE 150 Operator’s Manual
• The drain directs solvent spills from the bottle area on top of the ASE 150 to
the rear panel. A drain hose connects to the fitting. For installation
instructions, see Section B.2.2
.
2.3 ASE 150 Extraction Process
Preparing to Run an Extraction
The following steps are required before the ASE 150 can perform an extraction.
Refer to Chapter 3
• Fill the solvent reservoir.
• Prepare the sample and load it into the sample cell.
• Install the waste bottle and collection vessel.
• Select or create a method.
• Press the START button.
• Verify that the STATUS on the STATUS screen is OVEN READY (see Figure 2-5)
and the LED on the
for detailed instructions for each step.
START button is flashing.
• Install the sample cell in the cell holder and close the cell door.
• Press the START button.
16 Doc. 065207-02 9/08
2 • Description
Performing the Extraction
After you complete the preparation steps described on page 16 and press START
the second time, the ASE 150 performs the extraction. The extraction process
consists of six main steps.
1. Fill the cell with solvent—the
pump is turned on and the
static valve is closed (see
Figure 2-4
). Solvent is pumped
into the sample cell until the
cell pressure reaches
10.35 MPa (1500 psi).
Thereafter, the static valve
opens occasionally to maintain
the pressure at 10.35 MPa
(1500 psi).
2. Heat the cell (equilibration)—
the temperature in the cell is
heated to the set point
specified in the method.
Solvent
Bottle
Oven
Pump
Pressure
Relief
Valve
Purge Valve
Sample
Cell
Static Valve
3. Static extraction—the cell
remains filled with the solvent
at the temperature set point.
Waste
Bottle
Figure 2-4. Extraction Process Schematic
Collection
Vessel
Nitrogen
4. Rinse with fresh solvent—the static valve opens and the extract flows into the
collection vessel. Fresh solvent is pumped through the cell.
5. Purge solvent from the system—the purge valve opens and gas purges the
remaining solvent from the cell into the collection vessel.
6. Relieve pressure—the pressure relief valve opens and residual pressure is
released from the cell.
NOTE Static extraction and rinsing can be repeated multiple
times.
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ASE 150 Operator’s Manual
Monitoring the Progress of a Run
To monitor the progress of a run, press MENU, move the cursor to STATUS (if
necessary), and press
ENTER. The STATUS screen appears (see Figure 2-5).
STATUS STATIC
METHOD PCB
PRESSURE
TEMP 100C
Figure 2-5. Status Screen Example
The
STATUS screen operating parameters are updated in real time.
• STATUS—the current system status. During a run, the status field displays the
following status states (in the order given): Oven Wait, Oven Ready, Load,
Preheat (optional), Fill, Heat, Static, Rinse, Purge, Relief, Unload, and Idle.
• METHOD—the name or number of the current method.
• VOL—the approximate volume of solvent (in mL) delivered by the pump
since the method started running.
VOL
1565PSI
TIME
75mL
2:25
• PRESSURE—the current sample cell pressure reading.
• TEMP—the temperature specified in the method.
• TIME—the elapsed time since the method started running.
18 Doc. 065207-02 9/08
2.4 Method Control
A method determines how the ASE 150 performs the sample extraction. Methods
are defined on the
METHOD EDITOR screen (see Figure 2-6).
2 • Description
METHOD
TEMPERATURE
STATIC TIME
RINSE VOLUME
Figure 2-6. Method Editor Screen (Initial View)
The following method parameters define the method. See Section C.1.4
detailed descriptions of the method parameters.
1
100C
5MIN
60%
for
• TEMPERATURE—the temperature at which to heat the cell.
• STATIC TIME—the number of minutes to maintain the cell contents (sample
and solvent) at the temperature set point.
• RINSE VOLUME—the amount of solvent to rinse through the sample cell after
the static extraction.
• PURGE TIME—the amount of time the cell is purged with nitrogen.
• STATIC CYCLE—the number of times the static extraction and rinse cycles are
performed.
• CELL TYPE—the type of cell to use (stainless steel or zirconium).
Two types of methods are available:
• Preprogrammed methods are application-specific methods created by Dionex.
These methods cannot be changed or deleted by the user. For a list of the
parameters for each preprogrammed method, see Section 2.5
.
• Custom methods are user-programmable methods. All custom methods
initially contain the default method parameters. You can modify these
methods as required. For instructions on how to edit a custom method, see
Section 3.6
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.
ASE 150 Operator’s Manual
2.5 Preprogrammed Methods
To help you quickly produce results with the ASE 150, Dionex provides nine
preprogrammed methods. These methods are designated by three-letter
abbreviations (see the table below).
Preprogrammed Method Method Name
Semivolatiles BNA
Total Fat (crude) FAT
Chlorinated Herbicides HRB
Organochlorine Pesticides OCP
Organophosphorous Pesticides OPP
Polychlorinated Biphenyls PCB
Dioxins and Furans PDF
Polymer Additives PPE
Total Petroleum Hydrocarbons TPH
The remainder of this section lists the recommended solvent and the operating
conditions for each preprogrammed method. You cannot edit or delete a
preprogrammed method.
BNA (Semivolatiles) Method Parameters
Solvent MeCl2/Acetone (1:1, v/v)
Temperature 100 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
20 Doc. 065207-02 9/08
2 • Description
FAT (Total Fat) Method Parameters
Solvent Hexane/Acetone (4:1)
Temperature 125 °C
Static Time 5 min
Rinse Volume 100%
Purge Time 60 sec
Static Cycle 3
Cell Type Stainless steel
HRB (Chlorinated Herbicides) Method Parameters
Solvent MeCl2/Acetone (1:1) with 1%
H
3PO4
Temperature 100 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
OCP (Organochlorine Pesticides) Method Parameters
Solvent Hexane/Acetone (1:1, v/v)
Temperature 100 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
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ASE 150 Operator’s Manual
OPP (Organophosphorous Pesticides) Method Parameters
Solvent MeCl2/Acetone (1:1, v/v)
Temperature 100 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
PCB (Polychlorinated Biphenyls) Method Parameters
Solvent Hexane
Temperature 100 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
PDF (Dioxins and Furans) Method Parameters
Solvent Toluene
Temperature 200 °C
Static Time 5 min
Rinse Volume 60%
Purge Time 100 sec
Static Cycle 1
Cell Type Stainless steel
22 Doc. 065207-02 9/08
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