Argonaut Technologies QUEST 210 User manual

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TECHNOLOGIES
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Argonaut Technologies Revision
06/24/98
Quest
210
Manual Addendum
-
Auto Solvent Wash Option.
Part Number 102531
Rev A
6/
19/98
Copyright
0
1998by Argonaut Technologies
887
Industrial Rd., Suite
G
San Carlos, CA 94070
All rights reserved. Printed
in
the United States.
Argonaut Technologies reserves the right to make changes in any products herein to improve
reliability, function, or design. Argonaut Technologies does not assume any liability arising out of the
application or use of any product or circuit described herein; neither does it convey any license.
Quest 210 is a registered trademark of Argonaut Technologies. Other product names in this
document are registered trademarks or trademarks of their respective holders.
~~IEST
2
10
ORGANIC SYNTHESIZER
-
AUTOMATED SOLVENT
WASH
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Revision
06/24/98
......
...
Argonaut Technologies
Table
of Contents
..............................................................
1
QUEST
210
LIMITED WARRANTY AGREEMENT
4
.....................................................................................................................
1
.
1
WARRANTY
TERM
4
1.2 WHOISPROTECTED
..................................................................................................................
4
...................................................................................................................
1.3
WHATISCOVERED 4
...........................................................................................................
1.4 WHATISNOTCOVERED 4
.............................................................................................
1.4.1 Preparation and Installation
5
..........................................................................................
1.5 HowToGETWARRANTYSERVICE 5
1.5.1 ContactInformation
.....................................................................................................
5
2
LABORATORY SAFETY
...........................................................................................................
6
2.1 MATERIALSAFETYDATASHEETS(MSDS)
.............................................................................
6
3
STATEMENT OFPURPOSE
......................................................................................................
6
......................................................................
4
AUTOMATED SOLVENTWASH OVERVIEW
6
...............................................................................................................
5 SITE REQUIREMENTS
7
.............................................................................................................
5.1 SPACEREQUIREMENTS 7
....................................................................................................
5.2 ELECTRICALREQUIREMENTS 7
5.3 GASREQUIREMENTS
.................................................................................................................
8
5.4 WASTEREQUIREMENTS
............................................................................................................
8
..................................................................................................
5.5 VENTILATIONREQUIREMENTS 8
6
INSTALLATION
...........................................................................................................................
9
6.1 INSTALLATIONPARTS
...............................................................................................................
9
......................................................................................................
6.2 INSTALLATIONPROCEDURE 9
7
AUTOMATED SOLVENTWASH OPERATIONALCHECKOUT
.....................................
13
7.1 AUTODETECTION
OF
AUTOMATEDSOLVENTWASHCONFIGURATION
.................................
13
7.2 MANUALOPERATIONVERIFICATION
......................................................................................
13
8
USING THE AUTOMATED SOLVENTWASH OPTION
....................................................
14
8.1 SET-UP
.....................................................................................................................................
14
.................................................................................................
8.1.1 ASWM Set-up Procedure 15
.....................................................................
8.2 DETERMINING
THE
SOLVENTDELIVERYTIMES 15
.............................................................................................
8.2.1 Delivery Timing Procedure 15
.......................................................................
8.3
THEAUTOMATEDSOLVENTWASHPROGRAM 16
8.3.1 Programming anAutomated Solvent WashProcedure
...................................................
16
8.4 WASHTIMING
PPLRAMSMENU
...............................................................................................
18
8.4.1 Adjusting WashTimingParams Procedure
....................................................................
18
8.5 STARTING
THE
AUTOMATEDSOLVENTWASHPROGRAM
......................................................
19
8.5.1 Automated Solvent WashStart UpProcedure
.................................................................
19
..............................................................................................................
8.6
Rm
TIMEFEATURES 20
...............................................
8.6.1 Mod?fyinga Running Automated Solvent WashProgram
20
....................................................................
8.7 COMPLETING
AN
AUTOMATEDSOLVENTWASH 21
......................................................................................
8.7.1 Solvent Bottle Depressurization
22
9
PLUMBING DIAGRAMS
...........................................................................................................
23
..............................................
9.1 QUEST210ASW CONTROLLERUNITPLUMBINGSCHEMATIC 24
...........................................................................
9.2 QUEST21
0
ASWM PLUMBINGSCHEMATIC 25
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Argonaut
Technologies
Figures
Revision
06/24/98
Figure
I
-
Recommended Set-up of a Quest 210 with the Automated Solvent WashOption 7
Figure
2
-ASW Controller UnitRear View 10
Figure 3
-
ASW
Controller UnitFront View
I I
Figure
4
-Automated Solvent WashModule (ASWW Front Panel
I I
Figure
5
-
Bottle CapAssembly
12
Figure
6
-
Firmware VersionScreen 13
Figure
7
-
A
UTO
SOL
VENT WASHMenu - Program
1
selected 16
Figure
8
-
AUTOSOLVENT WASHMenu -first line displayed 17
Figure 9
-
"PressMODE to Exit'' Menu 18
Figure 10
-
WASHTIMEPARAMS Menu 18
Figure 11
-
"ToStart At" Menu 19
Figure 12
-
Screens Displayed During Operation 2
0
Figure 13
-
Editing An Active Parameter 20
Figure 14
-
Program Pause Menu 21
Tables
Table 1-Automated Solvent WashOption Parts 9
Table
2
-
ASWM Solvent Bottle Locations 12
Table
3
-
ASWMSet-up 15
Table
4
-
Solvent WashProgram
-
Lines
1-4
17
QrlEsr
21
0
ORGAMC
SYNTHESIZER
-
AUTOMATED
SOLVENT
WASH
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Revision
06/24/98
Argonaut Technologies
1.1 Warranty Term
The standard warranty agreement begins on the ship date of the Quest
2
10
Automated Solvent Wash
Option and terminates 1year from that date unless other contractual agreements have been arranged.
1.2
Who
Is
Protected
This warranty may be enforced by the original purchaser only.
1.3
What
Is
Covered
Argonaut Technologies warrants the Quest
21
0
system and Options against defects in materials and
workmanship for the term of the Warranty Agreement. Argonaut Technologieswill use reasonable
effortsto repair or replace the product, at its sole discretion, at no charge provided that Argonaut
Technologies is notified in a timely manner of defectswithin the warranty period.
Additional expenses covered by warranty are:
1.
Labor and materials for covered items.
2.
Shipping of repaired systems and accessories back to the customer after service.
3.
Shipment costs for repair parts sent to the customer for repair.
Consumable products or the like are only warranted to conform to the quantity and content stated on
the label at the time of delivery.
1.4
What
Is
Not Covered
Argonaut Technologies makes and Buyer receives no other warranty expressed or implied and all
warranties of merchantability and fitness for a particular purpose are expressly excluded. Neither
party shall have any liability with respect to its obligations under this agreement for consequential,
exemplary, or incidental damages even if it has been advised of the possibility of such damages.
Argonaut does not warrant and will not be held responsible for loss or damages resulting from a cause
other than defects in material or workmanship, including:
1.
Damage caused by servicing or modification by the customer other than what is recommended in
the customer servicing and maintenance documentation, or which has not been recommended by
a qualified Argonaut Technologiestechnical support representative.
2.
Damage caused by neglect, accident or any natural disaster, including earthquake, lightning,
flood, or fire; electrical surges or use of improper power sources.
3.
Damage caused by failure to perform routine preventative maintenance as specified in the user
operation manual.
4.
Damage caused by non-conformance to recommended instrument operation procedures.
5.
Any product on which the serial number has been defaced, modified, or removed.
6.
Damage caused by shipment of the product (claims must be presented to the carrier).
7.
Any accessories used in connection with the product, which are not covered under warranty.
Additional Expenses not covered by warranty are:
1.
Removal or installation of the system or accessories.
2.
Costs associated with installation, including adjustment of user controls.
3.
Shipment costs to return systems or accessories to the factory for repair.
4.
Shipment boxes or packaging used to return systems or accessories to the factory for repair.
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Argonaut Technologies Revision
06/24/98
1.4.1
Preparation and Installation
Unless other contractual agreements have been arranged, it is the responsibility of the customer to
unpack, move the equipment to its location and perform the installation as described in this manual.
Contact your local Argonaut Technologies Representative for pricing of installation services by a
qualified Argonaut Technologies Representative.
Note: It is the customer's responsibilityto retain original system packaging.
1.5
How
To
GetWarranty Service
Argonaut Technologies has a fully staffed technical support hot line to help you repair minor
problems over the phone, FAX or email. Major repairs that cannot be handled over the phone are
repaired at the nearest Quest 210 repair center. Argonaut Technologies does not perform on site repair
ofthe Quest unless other contractual agreements have been pre-arranged.
1.5.1
Contact Information
Be sure to have the serial number of your Quest ready when you call. It can be found on the
waste tray bracket on the Reactor Unit.
North America:
Argonaut Technologies
887 Industrial Road, Suite G
San Carlos, CA. 94070
Toll free number for USA and Canada: 888.598.1350
PHONE: 650.598.1350
FAX: 650.598.1359
Web Page address: http://www.argotech.com
Europe: Japan:
Argonaut TechnologiesA.G. Argonaut Technologies K.K.
St. Jakobsstrasse 148 MK Komachi Bldg. 4-2- 1
Postfach 43 Kojimachi Chiyoda-Ku,
4132 Muttenz 2, Switzerland Tokyo 102,Japan
PHONE: 41.61.465.9898 PHONE: 81.3.3234.4321
FAX: 41.61.465.9899 FAX: 81.3.3234.1359
Note: If you have any questions or comments regarding the content of this manual or
instrument installation requirements, please contact Argonaut Technologies at the phone
numbers or e-mail addresses provided above.
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Revision 06/24/98 Argonaut Technologies
Safety is everyone's concern. Your laboratory has specificpractices and policies designed to protect
personnel from potential hazards, both obvious and hidden. When working with a Quest
2
10 with the
Automated Solvent Wash Option we recommend thatthe following safety equipment be readily
available: Fire extinguisher, eye wash station, safety shower, eye protection, lab coat, and hand
protection. Adherence to these recommendations, aswell asthe other requirements presented in this
manual, will help to ensure both the successful installation and safe use of our equipment.
-
--
WARNING:
If
the equipment is used in a manner not specified by the manufacturer, the
protection provided by the equipment may be impaired.
2.1
Material Safety Data Sheets (MSDS)
The MSDS associated with each chemical used with this instrument must be kept at your facility for
easy reference by employees.
3
STATEMENT
OF
PURPOSE
This manual will assist in installation and use of the Quest
210
Automated Solvent Wash Option.
This manual was designed to be used in conjunction with the standard Quest Manual. When used in
this manner, this addendum will help to simplify installation and ensure that the Automated Solvent
Wash Option operates as designed.
WARNING: The Quest
210
Organic Synthesizerwith Automated Solvent Wash is designed to
be used for chemical synthesis including potentially hazardous chemical reactions. The
potential hazards of chemical synthesis include but are not limited to burns, explosions, and
exposure totoxic chemicals and carcinogens.Always wear eye protection, protective clothing
and suitable gloves. Operate the instrumentin a fume hood.
In addition to the features of the standard Quest, the Auto Solvent Wash Option provides the benefit
of programmable wash cyclesusing up to four solvents. The Automated Solvent Wash Option
consists of two main assemblies:
ASW Controller Unit
-
The Controller Unit for a Quest 210 with the Automated Solvent Wash
Option contains additional softwareto allow programming of wash cycles. Additional hardware
in the ASW Controller Unit includes dual inlet gas connections, a new distribution manifold,
additional solenoid valves to control the valves in the Automated Solvent Wash Module (ASWM)
and a connection for the Automated Solvent Wash Module harness. Refer to section 9.1 for a
plumbing schematic for the Controller Unit.
Automated Solvent Wash Module (ASWM)
-
The ASWM can hold up to four solvent bottles
with Bottles CapAssemblies. These solvent Bottle Cap Assemblies are identical to the one used
on the standard Quest. The ASWM also contains the tubing and valves that control the
automated delivery of the four solvents to the Reactor Unit. Four Toggle switches on the front
panel allow for manual delivery of solvents with a fifth toggle switch for purge gas (inert gas used
to clear lines after solvent delivery). A harness connects the ASWM to the Controller Unit and
provides the operating gas pressures for the ASWM valves. Refer to section
9.2
for a plumbing
schematic for the ASWM.
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Argonaut Technologies
The following information provides space, electrical, gas, waste, and ventilation requirements for the
Automated Solvent Wash Option. Adherence to the following will result in trouble free installation.
5.1
Space
Requirements
The space requirements for the ASW Controller Unit remain the same as the standard Quest and can
be found in the Quest User Manual. The
ASWM
requires bench space that is
17
inches wide,22
inches deep and
18
inches tall within a fumehood. This bench space must be capable of supporting
58
pounds and be located between the Reactor and Controller units. See Figure
1
for the recommended
set-up of a Quest
210
with the Automated Solvent Wash Option.
*tor
Unit
,Automated Solvent Wash Module
,ASW
Controller Unit
Figure
1
-Recommended Set-up of a Quest
210
with the Automated Solvent Wash Option
Note: The ASW Controller Unit must be placed external to the fume hood. Sensitive electronic
assemblies could be degraded and/or damaged if placed in an environmentwith a high level of
chemical vapors.
5.2
Electrical Requirements
The electrical requirements for the ASW Controller Unit are the same as for the standard Quest and
can be found in the Quest manual. Since the ASWM is controlled pneumatically there are no
additional electrical requirements.
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Revision
06/23/98
Argonaut
Technologies
5.3
Gas Requirements
The ASW Controller Unit can be configured to operate on either a single inert gas source or a
combination of inert gas and compressed air. On the rear panel of the ASW Controller Unit are two
gas inlet ports. One port requires a regulated
40-60
PSI source of high-purity (>99.98%) inert gas.
This gas is used for delivering solvents and creating the inert reaction environment in the Reactor
Unit. The second port requires
a
regulated
55-60
PSI source of clean, dry compressed air. This gas is
used to operate the agitation system in the reactor and control valves in the ASWM. When
compressed air is used it is recommended that a dryer be installed on the compressed air line to
prevent water from entering the system plumbing. Each source should be able to connect to
!4
inch
ODtubing. Included, as part of the Automated Solvent Wash Option, is a Gas Supply Assembly to
allow connection of the ASW Controller Unit to the gas source(s).
Note: Powering the agitation and control valves with compressed airwill significantly reduce
- -
the amount of inert gas consumed bv the Quest.
5.4
Waste Requirements
A Quest
210
with the Automated Solvent Wash Option uses the same Glass Waste Tank forwaste
collection as the standard Quest. Depending on the automated wash program it may be necessary to
attach a line from the Glass Waste Tank valve to a larger waste container. Refer to State and Local
regulations on the handling and disposal of hazardous waste.
5.5
Ventilation Requirements
Depending on the chemistry, a Quest
2
10
Organic Synthesizer with the Automated Solvent Wash
Option can generate volatile waste. The ASWM must be placed directly in a fume hood before use.
This allows for the proper venting of any hazardous vapors providing optimal laboratory safety. If a
Quest
2
10
with the Automated Solvent Wash Option is installed outside a fume hood a method to
evacuate any hazardous vapors created during operation is required (i.e. snorkels, adjustable hood).
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.-irgonaut Technologies
6.1
InstallationParts
Table 1outlines the parts provided to install the Auto Solvent Wash Option:
Part
Ouantitv
I
Part Descri~tion
I
Part Number
/
Note
-
..-
.
-
.I
,
1
I
ASW Controller Unit
1
300382 or
I
When installed as part of an
/
(ASWM) with
4
bottle cap assemblies
300390
;;;;:;;turn
of original
Controller Unit required.
300383 When installed as an upgrade,
3 Bottle Cap Assemblies are
1
1
1
10
FT Gas Supply Assembly
%-28
peek fitting and ferrule 100020
/
Ferrule swaging tool (%-28plugand
1
100083 and
I
1
I
I I
When installed as an upgrade,
I
I
300453
1
100019 and
/
1
2
4
%28 union)
0.125 inch OD Teflon tubing with
Table
1
-Automated Solvent Wash Option Parts
100200
300462
fittings
I
4
4
6.2
Installation Procedure
1. Place the ASW Controller Unit (Part Number 300382 or 300390) on a bench outside and
adjacent to a fume hood. Place the ASWM (PartNumber 300383) inside the fume hood closest to
the Controller Unit. Place the Reactor Unit inside the fume hood next to the ASWM and within 3
feet of the ASW Controller Unit. See Figure
1
for the recommended set-up of a Quest 210 with
the Automated Solvent Wash Option.
Hose clamp
4L
solvent bottle safety carriers
Note: If the Automated Solvent Wash Option is being installed as an upgrade, disconnect the
reactor umbilicus, power cord and the gas supply line from the original ControllerUnit. Set
aside the original Controller Unit for return to Argonaut Technologies.
102559
/
100353
(
(
For domestic use only)
2.5L solvent bottles with safety
carriers
Bottle Cap Assembly Vent lines
2.
To supply the ASW Controller Unit from a single inert gas source continue with step A. To
supply the ASW Controller Unit from both an inert gas source and compressed air continue with
step B. Refer to Figure
2
for the location of gas inlets on the rear panel of the ASW Controller
Unit.
Package of 10 Polyethylene
1
SolventiReagent Inlet Filter 900073
102553 and
102552
300319
3 safety carriers are provided.
(
For non-domestic use only)
When installed as an upgrade,
3 safety carriers are provided.
When installed as an upgrade,
3 vent lines are provided.
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Revision
06/25/98
Argonaut
Technologies
A. Attach the single end of the Gas Supply Assembly
(Part
Number 300453) to an inert gas
source capable of providing a regulated output between 55-60 PSI. The other end of the
Gas Supply Assembly has a tee with two quick disconnect fittings attached. Connect one
quick disconnect fitting to the inert gas inlet and the other fitting to the compressed air
inlet on the rear of the ASW Controller Unit. To attach these fittings push them over the
appropriate inlet port until an audible click is heard. Continue the installation at step
3.
Note:
If
either gas source is greater than five feet from the
ASW
Controller Unit additional gas
supply tubing will be required for dual gas operation.
B.
Remove the tee and quick disconnect fittings from the end of the Gas SupplyAssembly
(Part Number 300453). Cut the remaining 10
ft
piece of tubing in half. Install one quick
disconnect fitting onto the end of each piece of tubing to create two inlet lines. Attach the
open end of the first inlet line to an inert gas source capable of providing a regulated
output between 40-60 PSI. Attach the quick disconnect fitting on the opposite end to the
inert gas inlet on the rear panel of the ASW Controller Unit. Attach the open end of the
second inlet line to a compressed air source capable of providing
a
regulated output
between 55-60PSI. Attach the quick disconnect fitting on the opposite end to the
compressed air inlet on the rear panel of the ASW Controller Unit. To attach these
connectors push them over the appropriate inlet port until an audible click is heard.
Figure
2
-
ASW
Controller Unit Rear View
3.
Refer to Figure
2
for the location of components on the rear panel of the ASW Controller Unit.
Ensure the onioff switch is set to OFF and connect the power cable to the electrical socket on the
rear of the Controller Unit. Connect the free end of the power cable to an appropriate power
outlet as specified in the Quest User Manual.
4. See Figure
3
for the location of the ASWM interface harness connection on the front of the ASW
Controller Unit. Attach the ASWM Interface harness to the fiont of the Controller Unit by lining
up the surfaces and rotating the locking collar in a clockwise direction until tight.
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Argonaut Technologies Revision 06/24/98
-
ASWM Interface
Harness connection
1
Lower Manifold
Pressure connection (port
6)
Figure
3
-
ASW Controller Unit Front View
The remaining connection that differentiates the ASW Controller Unit from the standard
Controller Unit is an additional port on the front panel. In figure
3
this port is labeled "Lower
Manifold Pressure connection (Port 6)". Locate the tubing labeled "MEM" in the Reactor Unit
Umbilicus. If the "MEW tubing already has
a
ferrule and fitting attached, identical to tubing one
through five, then continue with step
7.
If no fitting or ferrule is attached to the "MEM" tubing
continue with step
6.
Slidethe fitting (PartNumber 100019)on the "MEW tubing with the threads closest to the end
of the tubing. Slide the yellow ferrule (Part Number 100020)onto the tubing sothat the smaller
OD is closest to the threads of the fitting. Align the flat edge of the ferrule to the end of the
"MEM" tubing. Create a ferrule swaging tool by screwing the %-28plug into the %-28 union
(PartNumbers 100083 and 100200) included with the Automated Solvent Wash Option. Screw
the "MEM" fitting into the ferrule swaging tool. Tighten the fitting finger tight and continue for
?4
turn. Remove the fitting from the swaging tool, you will notice the surface ofthe ferrule
closest to the fitting will be slightly flattened.
Connect the "MEM" tubing with ferrule and fitting into port 6 on the ASW Controller's front
panel. Make the connection finger tight. Complete the remaining tubing and cable connections
from the Reactor Unit Umbilicus to the ASW Controller Unit. These connectionsare identical to
the standard Quest and are described in the Quest User Manual.
See Figure 4 for the location of the ports on the front of the ASWM. Connect the BTL PRESS
line from the Reactor Unit Umbilicus to the Bottle Pressure port on the front of the ASWM.
Connect the SOLVENT line from the Reactor Unit umbilicus to the SOLVENT port on the front
of the ASWM. Connect one end of the 0.125 inch OD Teflon tubing with fittings (Part Number
300462) to the VENT port on the front of the ASWM and the other end to the UTILITY 2 port on
top ofthe Reactor Unit. Use the two hose clamps (Part Number
1
O2559)to hold the vent tubing
tightly to the Umbilicus.
ASWM Interface Harness
d
A B
C
D
Purge Bottle Pressure
1111
1
0
Vent
\
Solvent
Toggle Valves
Figure
4
-
Automated SolventWash Module (ASWM) Front Panel
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Revision
06/24/98
Argonaut Technologies
Note:
If
this Automated Solvent Wash Option is being installed as part of an initial Quest
install refer totheQuest User Manual for additional information concerning setup of the
Reactor Unit.
9.
If the Automated Solvent Wash Option was received as an upgrade to an existing Quest continue
with step 10, otherwise proceed with step 11.
10.
Three Bottle CapAssemblies are included when the Automated Solvent Wash Option is shipped
as an upgrade to an existing Quest 210. Use the Bottle Cap Assembly originally shipped with the
Quest as the fourth assembly. To connect the fourth Bottle Cap Assembly locate the solvent
tubing marked DS and the pressure tubing marked DP in the ASWM. Connect the tubing to the
corresponding ports on the fourth bottle cap assembly per Figure
5.
o+
Pressure
tubing
I
0
1
Solvent tubing
Figure
5
-
Bottle CapAssembly
Note: The tubing attached to the Bottle Capassemblies in the ASWM arelabeled with two
characters. Thefirst character, either A,
B,
C,
or
D
describes the bottle cap assembly it
attaches to. Thesecond Character, either
P
orS describes whether it is solvent or pressure
tubing.
Note: to allow for flexibility in locating the solvent bottle vents, additional tubing assemblies
(part number
300319)
areprovided for connection to theVent ports on the Bottle Cap
Assemblies.
1
1.
Place four solvent bottles in the safetycarriers and remove the clear cap from the top of the each
carrier. Place each solvent bottle with carrier into the ASWM. ~ndividuall~remove the solvent
bottle caps, insert a Teflon bottle seal and attach a Bottle CapAssembly. The Bottle Cap
Assemblies are labeled A, B,
C,
and D. Table
2
identifies where in the ASWM each of the
solvent bottles should be placed and which Bottle Cap Assembly should be attached. If installing
solvents bottles the first time, refer to "Manual Operation Verification" for the recommended
solvents to use forthat orocedure.
1--
-
~
Bottle CapAssembly
I
Location in the ASWM
(as viewed from the front)
A
- -
B
C
Table
2
-
ASWM Solvent Bottle Locations
Left
Front
-
-
-
.
-
.
-
..
.
Right Front
Left Rear
I
-
-
-
.
-
-
.
.
.
.
Note: For all customers outside of North America solvent bottles are provided.
D
Q~JEsT.?
10
ORGANIC
SYNTHESIZER
-
A
UTOWTED
SOISJIINT
WASH
Right Rear
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Argonaut Technologies Revision
06/24/98
12.
Using Figure
5
as a guide, turn the valves on the top of the Bottle Cap Assemblies towards the
vent port. This completes the installation of the Automated Solvent Wash Option. Before using
the Automated Solvent Wash Option it is recommended that you perform the Automated Solvent
Wash Operational Checkout.
WARNING: Always vent the bottle prior to unscrewing the Bottle CapAssembly.
WARNING: Always place the solvent bottles in the plastic Safety Carrierwhen working with
the Quest.
Once the Automated Solvent Wash Option installation is complete, performing the Operational
Checkout will insure that the system has been properly installed and functions correctly. The first
procedure verifies the configuration of the ASW Controller Unit. The second procedure will verify
manual operation of the Automated Solvent Wash Option by demonstrating that a specific bottle will
deliver solvent when selected.
WARNING
-
Always wear eye protection and appropriate clothingwhen operatingthe Quest.
7.1
Auto Detection of Automated SolventWash Configuration
1.
Turn ON the ASW Controller Unit and the gas supply.
2.
On power up, the Quest firmware will determine ifthehardware and software necessary for Auto
Solvent Wash are present.
3.
Pressing the Mode Key, located on the front of the Controller Unit, once will display the
Firmware revision screen.
If
the firmware version screen includes the line "with Auto Solv.
Wash" as shown in Figure
6,
then the Controller Unit is properly configured.
QUEST 210
-----
with Auto Solv. Wash
Date: Jun 12,
1998
Figure
6
-
Firmware Version Screen
Note: The firmware revision screen can also be accessed from the OTHER FUNCTIONS menu.
7.2
Manual Operation Verification
Note:
It
is recommended that methanol be used as the solvent when performing the Manual
Operation Verification procedure.
1.
See Figure
4
for the location of the toggle valves on the ASWM. Verify that the
5
toggle valves
on the ASWM front panel are all in the off (down) position.
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On side A of the Reactor Unit install ten 5ml Reaction Vessels (RVs), turn the Control Valves to
SOLVENT
and VENT, and set the MANIFOLD toggle valve to the open (down) position. On
side B of the Reactor Unit set both Control Valves and the MANIFOLD toggle valve to the
CLOSED position. Ensure all Lower Manifold drain levers on both sides ofthe Reactor Unit are
in the closed (up) position and rotate the Reactor Unit soyou are facing side A.
On the ASWM, pressurize bottle A by turning the valve on top of the Bottle CapAssembly
toward the tubing labeled BTL PRESS. Allow ten minutes for the bottle to pressurize before
delivering solvent.
On the ASWM front panel, flip the toggle valve labeled
A
to the open (up) position. Within 30
seconds solvent should be flowing into the RVs on side A of the Reactor Unit. After delivering
approximately 4ml tothe RVs return toggle valve A to the closed position. Verify the flow of
solvent stops.
On the ASWM, flip the purge toggle valve to the open position. Observe that the remaining
solvent in the delivery tubing is forced into the RVs followed by purge gas. Return the Purge gas
toggle valve tothe closed position.
Depressurize
ASWM
solvent bottle A by turning the valve on the top of the Bottle Cap Assembly
towards the vent port.
Insure the Glass Waste Tank is installed on the Reactor Unit. Attach the parallel drain lever (Part
Number 300296, included with all Quests) and flip the Lower Manifold drain levers to the open
position. Drain the reaction vessels on side A of the Reactor Unit by turning the left Control
Valve to
DRAIN
GAS and the right Control Valve to CLOSED.
Repeat steps
2
through
7
for ASWM bottle positions
B,
C and D. If any of the above steps do not
produce the expected results, the installation should be reexamined.
Note: Contact Argonaut Technologiesif after reexaminingthe installation process any of the
above steps still does not producethe expected results. Refer to the section 1.5.1 for contact
information on how to reach an Argonaut Technologies Technical Support Representative.
At this point, the functions ofASWM have been fully tested in the manual mode. Toverify the
operation ofthe Automated Solvent Wash Option it is recommended that you complete the "Using
the Automated Solvent Wash Option" procedure.
8
USING
THE
AUTOMATED
SOLVENT
WASH
OPTION
This section explains how to use the Automated Solvent Wash Option by providing step by step
instructions on how to perform an automated solvent wash. An automated solvent wash consists of
filling the Reaction Vessels (RVs) with solvent, agitating the solvent and then draining the RVs
automatically. It also serves as the final system verification. The following procedures assumethe
system has been fully tested in manual mode. If you have not tested the system in manual mode
complete the procedures described in section 7.0.
8.1
Set-up
The following four solventswere chosen for this procedure since they represent the most commonly
used solvents. Any solvents may be used but delivery times will have to be adjusted based on the
viscosity
of
the solvent chosen.
QUEST
210
ORGANIC:SYNTHESIZER
-
AUTOMATEDSOLVENTWASH
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Argonaut Technologies Revision
06/24/98
8.1.1
ASWM Set-up Procedure
Place the specified solvent bottles with safety carriers into the ASWM positions noted in Table
3.
Remove the solvent bottle cap on the bottle in position A and insert the Teflon bottle seal. Install
a new polyethylene SolventIReagent Inlet Filter onto the Solvent Bottle Cap pick-up line. Screw
Bottle Cap Assembly
A
onto the bottle in position A.
Repeat step
2
for bottle position B,C, and D.
Turn the valves on top of each Solvent Bottle Cap Assembly toward the tubing labeled BTL
PRESSURE.
0.44 27
sec
Table
3
-
ASWM Set-up
8.2
Determining the SolventDelivery Times
Determining the solvent delivery time ensures the appropriate volume of solvent is delivered to the
RVs. Due to differences in solvent viscosity the delivery times will be different for various solvents.
The best method to measure solvent delivery times is to manually deliver solvent tothe RVs using the
Toggle Valves on the front of the ASWM and a stop watch.
Warning: Insure proper solvent deliver times before operating the Automated Solvent Wash
Option. Inappropriate solvent delivery times can cause over filling of the RVs creating cross
contamination between RVs, upper manifold clogs and solvent overflow into the ASWM.
8.2.1
Delivery Timing Procedure
Install ten
5
ml RVs onto side A of the Reactor Unit. Turn the Reactor Unit Control Valves on
side A to SOLVENT and VENT. Set the MANIFOLD toggle valve to the open (down) position
and close the Lower Manifold Drain Valves.
Using a stopwatch, start timing the delivery for solvent A when you flip the Toggle Valve for
solvent A on the ASWM. Stop the stopwatch when the appropriate volume is delivered to the
RVs(use
4
ml's for this procedure). Return Toggle Valve A tothe closed position to stopthe
flow of solvent. The time on the stopwatch represents the delivery time for the specific solvent
and volume dispensed from bottle
A.
Flip the Purge Toggle Valve on the front of the ASWM to the ON position. This will purge any
remaining solvent in the delivery line. Notice that purging the delivery line adds additional
solventto the RVs. Return the Purge Toggle Valve to the OFF position. During an Automated
SolventWash Program purging is automatically performed after each delivery of solvent.
Insure the Glass Waste Tank is installed on the Reactor Unit. Attach the parallel drain lever and
flip all the Lower Manifold drain levers to the open position. Drain the RVS on side A of the
Reactor Unit,
turn
the left Control Valve to DRAIN GAS and the right Control Valve to
CLOSED.
Repeat steps
1-4
for the solvents in position B, C, and
D
to determine delivery times for all four
solvents. As a reference, the delivery times determined in our laboratories is shown in Table
3.
Your actual delivery times may be different.
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Revision
06/24/98
Argonaut Technologies
8.3
The Automated Solvent Wash Program
The Automated Solvent Wash firmware can support up to
60
wash programs. A single program can
have up to
25
lines, however, the total number of lines cannot exceed
120
in all wash programs added
together. Automated Solvent Wash programs are entered using the menu driven software of the ASW
Controller Unit. Using the AUTO SOLVENT WASH menu the User enters the following
information:
1.
Program number.
2.
Reaction volume.
3.
Reaction location.
4.
Number of repetitive washes of a specific solvent.
5.
Wash solvent.
6.
Solvent addition time in seconds.
7.
Agitation time.
.8. Pulsed or not pulsed draining.
9.
Drain time.
8.3.1
Programming an Automated SolventWash Procedure
1.
Push the MODE key on the Controller Unit until the AUTO SOLVENTWASH menu is
displayed. A flashing cursor is aligned to the right of Pgm: (program). Use the PARAMETER
SETTING keys
(+
or
-)
to increment or decrement the program number until Pgm
1
is displayed.
The screen should now look like Figure
7.
--AUTO SOLVENT WASH-
5ml
Side:A&B
#
R
S Add
Mix
Pul
Empty
Program---
Figure
7
-
AUTO SOLVENTWASH Menu
-
Program
1
selected
2.
Move the flashing cursor to the reaction volume parameter by pressing the right arrow key once.
Use the PARAMETER SETTING keys
(+
or
-)
to increment or decrement the reaction volume
until
4
ml is displayed. An Asterisk will be displayed next to the reaction volume if it is different
than the volume entered in the Set Temperature menu. For information on the Set Temperature
menu refer to the Quest User Manual.
3.
Move the flashing cursor to the Side parameter by pressing the right arrow key once. Use the
PARAMETER SETTING keys
(+
or
-)
to change the Side parameter until A is displayed.
4.
Move the flashing cursor tothe Draining Method parameter by pressing the right arrow key once.
To select a draining method the PARAMETER SETTING keys
(+
or
-)
are used to choose either
Pul or Dm. When pulsed draining is selected,the gas pressure to drain the RVs is pulsed to
overcome minor flow restrictions. When
Dm
is selected the drain gas is not pulsed. Setthe
draining method to Pul. Pulsed draining is the default setting and is the recommended draining
method.
5.
Push the right arrow soft key again to enter the first line of the Automated Solvent Wash
program. See figure 8, the following parameters are displayed on the first line of the solvent wash
program:
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Argonaut Technologies Revision
06/24/98
--AUTO SOLVENT WASH-
Pgm:
1
5ml
Side:A&B
#
R
S
Add
Mix
Pul
1)
3xA
60
5:OO
25
Figure
8
-
AUTO SOLVENTWASH
Menu
-
first line displayed
A.
#:
Line number of the solvent wash. The default entry forthis parameter is
1
representing
the first line ofthe program.
B.
R: Number of repetitive washes for the selected solvent. The default entry for this parameter
is
3
representing
3
repetitions of this line of the program.
C.
S: Solvent position selected. The default entry for this parameter is A representing the
Solvent in bottle A.
D.
Add: Solvent delivery time in seconds. The default entry for this parameter is 60
representing a delivery time of 60 seconds.
E. Mix: Agitation time in minutes and seconds. The default entry for this parameter is 5:00
representing an agitation time of
5
minutes and 0 seconds.
F. Pul: Pulsed draining time in seconds. The default entry for this parameter is 25 representing a
draining time of 25 seconds. If
Dm
is selected instead of Pul the default time would be 50.
Enter the values listed in Table
4,
line
1
into the first line of the Automated Solvent Wash
program. Use the right arrow soft key to align the cursor over the parameter to be changed and
press the PARAMETER SETTING (+or-) keys to incrementldecrementthe value. *For entries
under the Add parameter use the measured delivery times for the respective solvents.
Table
4
-
SolventWash Program
-
Lines
1-4
After entering the Pul parameter press the right arrow key once to add a second line to the
Automated Solvent Wash program. The software creates a copy of the first line and enters it as
the next line of the program. Enter the values listed in Table
4,
line
2
into the second line of the
program.
After entering the Pul parameter press the right arrow key once to add a third line to the
Automated Solvent Wash program. The software creates
a
copy of the second line and enters it
asthe next line of the program. Enter the values listed in Table
4,
line
3
into the third line ofthe
program. Another method to add or delete
a
line into the Automated Solvent Wash program is by
pressing the mode key. Press the mode key to display the menu shown in Figure
9.
QUEST
2
10
ORGANIC
SYNTHESIZER
-
A
IJTOMATEL) SOI.VENT
WASH
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