Dionex ASE 100 Operator's Manual
ASE 100
®
ACCELERATED SOLVENT EXTRACTOR
OPERATOR'S MANUAL
© 2002 Dionex Corporation
Document No. 031842
Revision 01
May 2002
©2002 by Dionex Corporation
All rights reserved worldwide.
Printed in the United States of Amer ica.
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
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
2.2 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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v
ASE 100 Accelerated Solvent Extractor
vi
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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
1-1
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
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.
1-5
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
b
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
2-1
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
2-3
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
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
In
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
MENU
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
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.
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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2-5
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
A
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.
2-7
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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2-9
ASE 100 Operator’s Manual
2-10
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
START
START
button.
STATUS
button is flashing.
to begin the run.
is
OVEN READY
(see Figure 2-5) and the LED
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2-11
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
2-12
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2.4 Method Control
2•Description
A
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)
2-13
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%
H
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
2-15
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
2-16
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