Argonaut Technologies QUEST 205 User manual

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ARGONAUT
TECHNOLOGIES
Part Number 102965
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.......
Quest 205 . User Manual Revision
B 12/03/98
1 Introduction ................................................................................................................................. 1-7
Quest205 Product Description
................................................................................................. 1-8
. . ...............................................................................................................
Quest205 Specifications.. 1-9
..................................................................................
Quest205 Limited Warranty Agreement 1-10
WarrantyTerm
.......................................................................................................................... 1-10
Who Is Protected?
..................................................................................................................... 1-10
......................................................................................................................
What Is Covered? 1-10
..............................................................................................................
What Is Not Covered? 1-10
........................................................................................................
Preparation and Installation 1-12
How to Get Warranty Service
..................................................................................................... 1-12
..............................................................................................................
InterferenceInformation 1-12
.................................................................................................................
Immunity Information 1-13
.............................................................................................................................................
Safety -1-13
......................................................................................................................
Laboratory Safety 1-14
MaterialSafetyData Sheets(MSDS)
.......................................................................................... 1-14
.....................................................................................................................
Contact Information 1-15
.................................................................................................................
2 Quest 205 Installation 2-1
....................................................................................................................
InstallationProcedure 2-1
..............................................................................................................................................
Parts 2.1
...................................................................................................................
User-Supplied Items 2-1
...................................................................................................................
InstallationGlossary 2.2
Settingup the Quest 205 Synthesizer
...................................................................................... 2-2
Connecting the Interface Harnessto the Controller Unit
..................................................... 2-3
Connecting the BottleCap Assembly
...................................................................................... 2-3
........................................................................
Connecting the Reactor Unit Manifold Tubes 2-4
..........................................................................................................
Installingthe Waste Tank 2-6
Settingthe Manifold ControlValves
....................................................................................... 2-6
....................................................................................
Connecting Gasto the Controller Unit 2-7
Connecting a SingleGas Source
........................................................................................... 2-7
Connecting Two GasSources
................................................................................................ 2-7
.........................................................................................
Connecting Power to the Quest205 2-8
Installingthe SolventBottle
...................................................................................................... 2-8
...................................................................................................................
3 Quest 205 Overview 3-1
.....................................................................................................................................
Reactor Unit 3-1
............................................................................
ReactionVessel Bank and ReactionVessels
3-2
....................................................................................................................
ReactionVessels 3-2
..............................................................................................................
ReactionVessel Bank 3-2
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Quest 205 . User Manual Revision
B 72/03/98
Heatingand Cooling .................................................................................................................. 3-2
..................................................................................................
Heatingand CoolingBlocks 3-2
..........................................................................................................................
Reaction Mixing 3-3
. .
...................................................................................................................................
Agitation 3-3
...............................................................................................................................
Magnet Bar 3-3
Fluidic System
............................................................................................................................. 3-3
ManifoldControl Valves
....................................................................................................... 3-4
....................................................................................................
Metered Gas Needle Valve 3-5
Utility Ports
.......................................................................................................................... 3-5
Upper Manifold
...................................................................................................................... 3-6
Luer Ports
................................................................................................................................. 3-6
Lower Manifold Drain Valves
.............................................................................................. 3-7
.............................................................................................................................. Waste Tank 3-7
SampleCollection
................................................................................................................... 3-7
ControllerUnit
................................................................................................................................ 3.8
LCD Screen and Keypad
............................................................................................................ 3-8
LCD Screen
.............................................................................................................................. 3-8
Keypad
..................................................................................................................................... 3.9
Mode Button
............................................................................................................................ 3-9
Forward and Back Buttons
.................................................................................................. 3-10
Parameter SettingButtons
.................................................................................................. 3-10
START/STOPButton
.......................................................................................................... 3.10
Agitator Control Buttons
..................................................................................................... 3.11
Agitation Needle Valve
........................................................................................................ 3-11
ControllerUnit Gas and Power Connections
....................................................................... 3-12
SystemGas
........................................................................................................................... 3-12
ElectricalOutlet
..................................................................................................................... 3-12
Power Switch
........................................................................................................................ 3-12
InterfaceHarness
......................................................................................................................... -3-12
SolventBottle Assembly
............................................................................................................. -3-13
............................................................................................................
4 Operatingthe Quest205 4-1
...................................................................................... Preparingthe Quest205 for a Synthesis 4-1
Remove Used Reaction Vessels
................................................................................................ 4-1
...............................................................................................
InstallingNew ReactionVessels 4-4
ShuttingOffIndividualReaction Vessels
............................................................................... 4-6
Waste Tank
.................................................................................................................................. 4-7
.......................................................................................................................... Startinga Reaction 4-7
......................................................
Settingthe Reaction Temperature, Time, and Aptation 4-8
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...
Quest 205 . User Manual Revision
B 12/03/98
..........................................................................................
Settingthe Agitation Parameters 4.8
................................................................................................................
TemperatureControl 4-10
..................................................................................
Enteringthe TemperatureSet-Point 4-12
Chillingthe ReactionVessels
.............................................................................................. 4-13
Upper Manifold MembraneSwitch
....................................................................................... 4-14
ParallelSolvent Addition and Vessel Draining
.................................................................... 4-14
....................................................................................................
ParallelSolventAddition 4-14
Drainingthe ReactionVessels
............................................................................................ -4-16
Changinga SolventBottle
................................................................................................... 4-17
Adding Solventor Reagents Throughthe Luer Ports
......................................................... 4-18
................................................................................................
Adding Solventor Reagents 4-18
Adding Liquid Solventor Reagents to an Air-SensitiveChemistry
............................. 4-19
ReactionVessel Bank-to-Bank Transfer
................................................................................. 4-20
Providing a GasSweep Over the Reaction Vessels
............................................................. 4-21
Collection of Liquid Reaction Products
.................................................................................... -4-22
DrainingSynthesisProductsto CollectionFlasks
............................................................... 4-22
5 Maintenance
............................................................................................................................. 5-1
Post SynthesisCleaning
................................................................................................................ 5-1
...................................................................................................................
Manifold Maintenance 5.3
........................................................................................................................................
6 Glossary 6-1
...............................................................................................
7 ControllerUnit Display Screens 7-1
Sign-OnScreen
................................................................................................................................ 7-1
Firmware Version Screen
............................................................................................................... 7-2
AgitationControlScreen
............................................................................................................... 7-3
.
Set Temperature Screen ................................................................................................................. 7-5
........................................................................................................
Monitor Temperature Screen 7-6
..................................................................................................................
Other Functions Screen 7-7
.................................................................................................................
Contrast ControlScreen 7.9
Self Test Screen
.............................................................................................................................. 7-10
Restore DefaultsScreen
................................................................................................................ 7-11
...........................................................................................................
Start/Stop HeatersScreen 7-12
8 Reactor Unit PlumbingSchematic
............................................................................................ 8-1
9 Accessories
................................................................................................................................... 9-1
Quest 205 Magnet Stirrer (P/N 900200)
.................................................................................. 9-1
.................................................................... Quest 205 Magnet Extraction Bar (P/N 102288) 9-1
.........................................................................................
Quest205 Flask Rack (P/N 900199) 9-1
...................
Quest 205 RestrictorTubing (P/N 900201) and InsertionTool (P/N 900202) 9-1
.............................................................................
Quest 205 WeighingFunnel (P/N 900196) 9-2
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Quest 205 . User Manual Revision
B 12/03/98
Quest 205 Addition Funnel (P/N 900197) ............................................................................... 9-2
Quest 205
RV Tapered Caps (P/N 900203) ........................................................................ 9-3
............................................................................................. Quest 205 RV Rack (P/N 900204) 9-3
............................................................ Quest 205 Hex Ball Driver 3/32" Tool (P/N 900205) 9-3
Quest 205
Hex Ball Driver 7/ 64" Tool (P/ N 900206) ........................................................... 9-3
...........................................................................
Quest 205 Bubbler Accessory (P/N 900125) 9-4
............................................................................. Quest 205 TransferCannula (P/N 900207) 94
.................................................................
Quest 205 Multi-FlaskAdapter Kit (P/N 900209) 9-5
.............................................................
Quest 205 SPE Cartridge Adapter Kit (P/N 900210) 9-5
Quest 205 SeptumLuer Plugs (P/N 900145)
.......................................................................... 9-6
10 User Tutorial
.............................................................................................................................. 10-1
Overview
........................................................................................................................................ 1 0-1
Instrument and SolutionPreparation
........................................................................................ 10-2
....................................................
RV Removal, Instrument Cleaning, and RV Installation 10-5
Reductive Amination
................................................................................................................... 10-6
Fillingthe Dead Volume Between the
RV frit and the Lower Manifold Drain Valve .... 10-6
Addition of Reagentsof RVs
................................................................................................... 10-7
Addition of NaBH4 Solutionto eachRV
............................................................................... 10-9
Product Work Up and Collection
............................................................................................ .10-11
In-Line Purification: Bank to Bank TransferCannulation (optional)
............................. 10-11
Off-Line Purification: 60 mL or 75 mL SPE cartridge (optional)
.................................... 10-12
............................................................................................................ Cleaning and Maintenance 10-13
Systemswithout the Automated SolventWash Option
.................................................. .I 0-14
Systemswith Automated SolventWash
............................................................................. 10-14
Product Analysis
......................................................................................................................... 10-16
SpectroscopicData
.................................................................................................................. 10-17
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Quest 205 - User Manual
Quest 205 User Manual.
Part Number 102965
Rev
B 12/03/98
Argonaut Technologies
887 Industrial Rd., Suite G
San Carlos, CA 94070
All rights reserved. Printed in the Unitec
d States.
Revision B 12/03/98
Argonaut Technologiesreservesthe right to make changes in any products herein to improve
reliability, fimction,or design. Argonaut Technologiesdoes not assume any liability arising out of the
applicationor use of any product or circuitdescribed herein; neither does it convey any license.
-
Quest is a trademark of Argonaut Technologies. Other product names in this document are registered
trademarksor trademarks of their respective holders.
Argonaut Technologies
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Quest 205 - User Manual
Revision 6 72/03/98
1 Introduction
This manual will assist with operating and maintaining the Quest 205 Synthesizer
and is organized into the following sections.
Section
1, Introduction: Contains general information on the Quest 205
Synthesizer, brief description of the instrument, warranties, and safety
information.
Section 2, Quest 205 Installation: Provides instructions on installing the Quest
205 Synthesizer.
Section
3, Quest 205 Overview:Defines the Quest 205 hardware parts and
provides
an overview of how these parts work together.
Section 4, Operatingthe Quest 205: Provides step-by-step instructions for
performing solid phase or solution phase reactions.
Section 5, Maintenance:Provides step-by-step instructions on maintenance
procedures for optimum instrumentperformance.
Section
6, Glossary: Definesterms specific to the Quest 205 Synthesizer.
Section
7, Controller Unit Display Screens:Provides a list of the possible display
screens and how to changeparameters on the appropriate screens.
Section
8, Reactor Unit Plumbing Schematic
Section
9, Accessories:Describes accessories available for the Quest 205
Synthesizer. Includes installation and use instructions.
Section 10,User Tutorial: Provides
an introductionto the instrument by guiding
the user through a parallel solution phase reaction, work-up and purification.
Argonaut Technologies
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Quest 205 - User Manual Revision
B 12/03/98
Quest 205 Product Description
WARNING: The Quest 205 Synthesizer is designed for use in chemical syntheses,
including potentially hazardous chemical reactions and should be operated in a fume hood.
Potential hazards of chemical synthesis include but are not limited to burns, explosions,
and exposure to carcinogens and toxic chemicals. Always wear eye protection and suitable
gloves.
The Quest 205 Synthesizerruns in parallel up to 10liquid or solid phase organic
chemistry reactions. The unique design of the Quest 205 incorporates
heating/cooling,agitation,and the inert environmentneeded to
run these
reactions. The mechanical featuresof the Quest 205 also provide for simple
operation of the instrument.
The Quest 205 consistsof four main parts: the Reactor Unit, the Controller Unit,
the Solvent Bottle Assembly, and the Reactor InterfaceHarness.
The
Reactor Unit containsthe manual solvent and gas control valves and
components for heating, cooling, agitation,as well as holds the Teflon Reaction
Vessels. Solventsmay be added to the Reaction Vessels (RVs) in parallel using
the manual rotary valves. Reagents are added via luer ports located at the top of
each Reaction Vessel.
The
Controller Unit contains the controlsto set the reaction temperature, heating
duration, and agitationconditions. The ControllerUnit also contains connections
for system power and gas, and interfaceconnectionsfor the Reactor Unit. A
serial computerport is included on the ControllerUnit to download firmware
upgrades.
The
Solvent Bottle Assembly consists of the solvent bottle, plastic bottle safety
carrier, and a Bottle Cap Assembly. The Bottle Cap Assembly can either
pressurize or vent the solvent bottle. The Solvent Bottle Assembly connects to
the Quest Reactor Unit and providesthe solvent for parallel deliveryto the
Reaction Vessels for resin washing and system cleaning.
The
Interface Harness linksthe Control Unit to the Reactor Unit. Solvent, drain
gas, metered gas, agitationpressure, and temperature control information are
supplied and/or communicatedthrough the harness. The solvent, drain gas, and
metered gas movements are directed via the Reactor Unit's manual control
valves. The agitation and heating parameters are set using the Controller Unit
components.
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Quest 205 - User Manual Revision
8 12/03/98
See System Overviewfor a detailed description of the Quest 205 Synthesizer
Quest 205 Specifications
Reactor Assembly
(wxdxh)
Weight
Controller Unit
(wxdxh)
Weight
1
- 10disposable Reaction Vessels with frit
100mL transparent Teflon
Proprietary vertical oscillation mechanism
-40°C to 130°C
+ 5%
(requiresrecirculating chiller for
temperaturecontrol below ambient)
Accommodates 14/20, 19122,24140,29126,
and 29142 pear-shaped or round flasks
19" (48 cm)
x 19"(48 cm) x 30" (76 cm)
75 lbs (34
kg)
10" (25 cm) x 16.5"(42 cm) x 12"(30 cm)
20 lbs (9 kg)
15°Cto 35OC Ambient Temperature
30-70% Relative Humidity
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.. . -
Quest 205 - User Manual
Revision B 72/03/98
Quest 205 Limited Warranty Agreement
Warranty Term
The standard Warranty Agreementbegins on the ship date of the Quest 205
Synthesizer and terminates 1 year from that date, unless other contractual
agreements have been made.
Who Is Protected?
This warranty may be enforced by the original purchaser only.
What Is Covered?
Argonaut Technologieswarrants the Quest 205 Synthesizerand Options against
defects in materials and workmanship for the term of the Warranty Agreement.
Argonaut Technologieswill use reasonable efforts to repair or replace the
product, at its sole discretion, at no charge provided that Argonaut Technologies
is notified in a timely manner of defects within the warranty period.
Additional expenses coveredby the Warranty are:
1. Labor and materials for covered items.
2. Shipping of repaired systems and accessories back to the Customer after
service.
3. Shipmentcosts for repair parts sent to the Customer for Customer 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.
What Is Not Covered?
Argonaut Technologiesmakes, and the Customer 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 obligationsunder this agreement for consequential, exemplary,
or incidental damages even if it has been advised of the possibility of such
damages.
Argonaut Technologies
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Quest 205 - User Manual
Revision 0 12/03/98
Argonaut Technologiesdoes not warrant and will not be held responsible for loss
or damagesresulting from a cause other than defects in material or workmanship,
including:
1. Damage caused by servicingor modification by the Customer other than what
is recommended in the customer servicingand maintenancedocumentation 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 failureto perform routine preventative maintenance as
specified in the Quest
205 User Manual.
4. Damage causedby non-conformance to recommended instrument operation
procedures.
5. Any product onwhichthe serialnumber has been defaced, modified, or
removed.
6. Damage caused by shipmentof the product. (Claims must be presented to the
carrier.)
7. Any accessoriesused in connectionwith the product, which are not covered
under warranty.
Additional expensesnot covered by the Warranty are:
1. Removal or installationof the system or accessories.
2. Costs associated with installation,including adjustment of user controls.
3. Shipmentcosts to return systemsor accessoriesto the factory for repair.
4. Shippingboxes or packaging used to return systems and accessories to the
factory for repair.
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--
-
Quest 205 - User Manual
-
Revision B 12/03/98
Preparation and Installation
Unless other contractual agreementshave been arranged, it is the responsibility of
the Customer to unpack the equipment, move the equipment to its location, and
perform the installation as described in the provided manual. Contact the local
Argonaut Technologies Representative for pricing of installation services by a
qualified Argonaut TechnologiesRepresentative.
NOTE: It is the Customer's responsibilityto retain the original system packaging.
Howto Get Warranty Service
Argonaut Technologieshas a fully staffed technical support hot line to help the
Customer repair minor problems over the phone, or by
FAX or e-mail. Major
repairs that cannot be handled over the phone are repaired at the nearest Quest
205 repair center. Argonaut Technologies does not perform on-site repair of the
Quest 205 Synthesizerunless other contractual agreements have been pre-
arranged.
To establish the Quest 205 warranty, the warranty return card, provided in the
shipping box, must be filled out and mailed after installation is complete.
To qualify for warranty repair, first contact the appropriate repair center detailed
in this chapter, ContactInformation.
Interference Information
This equipment generatesand uses radio frequency energy and, if not installed
and used in strict accordancewith the manufacturer's instructions, may cause
interferenceto radio and television reception. The equipment has been type
tested and found to comply with the limits for a Class
B computing device in
accordance with the requirements set forth in the European Standard EN
55011:1997. Class
B equipment is equipment suitable for use in domestic
establishments and in establishmentsdirectly connected to a low voltage power
supply network which suppliesbuildings used for domestic purposes. However,
there is no guarantee that interferencewill not occur in a particular installation. If
this equipment does cause interferenceto radio or television reception,
determined by turning the equipment off and on, the user is encouraged to try to
correct the interferenceby one or more of the following measures:
Argonaut Technologies
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Quest 205 - User Manual
Revision B 12/03/98
Reorient the receiving antenna
.
Relocate the equipment with respect to the receiver
Move the equipmentaway from the receiver
Plug the equipment into a differentoutlet so that the Controller Unit and the
Reactor Unit are on differentbranch circuits
Immunity Information
This equipmenthas been type tested and found to comply with the Requirements
of the GenericImmunity Standard: EN50082-111997.
If the equipmentis used in a manner not specifiedby the manufacturer, the
protection provided by the equipment may be impaired.
Safety
This equipmenthas been tested and found to comply with the requirements as set
forth in the EuropeanImmunity Standard:EN50082-111997.
The following hazard symbolsare found on the Quest 205 Synthesizer:
This symbol indicates a hot surface. Use
cautionwhen working near or on the
Reactor Assembly. When heating, the
Reactor Unit becomes hot. Allow it to cool
before attemptingto access Reaction
Vessels.
This symbol indicates a shock hazard. Use
care when working around an area with this
symbol.
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Quest 205 - User Manual
-
Revision B 12/03/98
Laboratory Safety
Every laboratory has specificpractices and policies designed to protect personnel
from potential hazards, both obvious and hidden. When working with a Quest
205 Synthesizer,the manufacturerrecommends that the following safety
equipment be readily available:fire extinguisher, eye wash station, safety shower,
eye protection, lab coat, and hand protection. Adherence to these
recommendations, as well as the other requirements presented in this manual, will
help to ensure both the successful installation and safe use of the Quest 205.
WARNING: If the equipment is used in a manner not specified by the manufacturer, the
protection provided by the equipment may be impaired.
This equipment has been type tested and found to be in accordance with the
requirements for Laboratory Instruments set forth in the European Standard
EN 6 1010-1 : 19931A2:1995. Copies of the TUV certificates are available upon
request fiom Argonaut TechnologiesInc.
Material Safety Data Sheets (MSDS)
The MSDS associatedwith each chemical used with the Quest 205 Synthesizer
must be kept at the user's facility for easy reference by employees.
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Quest 205 - User Manual
Contact Information
North America:
Argonaut Technologies
887Industrial Road, Suite G
San Carlos, CA 94070
Toll free number for
U.S. and Canada:
Phone: [phone]
Fax: [phone]
E-Mail: support@,arnotech.com
Revision B 12/03/98
Web Page address:http://www.argotech.com
Europe:
Argonaut Technologies A.G.
St. Jakobsstrasse 148
Postfach 43
4132 Muttenz 2, Switzerland
Phone: [phone]
Fax: [phone]
Japan:
Argonaut TechnologiesK.K.
MK Komachi Bldg. 4-2-1
Kojimachi ChiyodaKu
Tokyo 102,Japan
Phone: [phone]
Fax: [phone]
E-Mail: stanabe@,arnotech.com
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 on the previous page.
Argonaut Technologies
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Quest 205 - User Manual Revision
B 12/03/98
2 Quest 205 Installation
Installation Procedure
Installation of the Quest 205 Synthesizerinvolves connecting the systemto a gas
source and making some simple tubing connections. The process typically takes
less than 1hour.
Parts
. Quest 205 Reactor Unit
Quest 205 Controller Unit
Accessory Kit
Voltage Kit (power cord)
Solvent Bottle Safety Carrier (4L capacity for Domestic Instruments or 2.5L
capacity for International Instruments)
User-Supplied Items
If using a single gas source:
55-60 psi house nitrogen supply or other high-purity (>99.98%) inert gas
If using dual gas source:
40-60 psi house nitrogen supply or other high purity (>99.98%) insert gas
55-60 psi clean, dry compressed air
One 100-120or 200-240
VAC, 50-60 Hz grounded outlet capable of supplying
10amps.
Recirculating chiller (optional, required for temperatures below ambient)
Solvents and reagents
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Quest 205 - User Manual
. - -
Revision B l2,/03/98
Installation Glossary
Bulkheadfitting: The femalethreaded ports found on the front of the Controller
Unit and on variousplaces of the Reactor Unit.
Ferrule: The yellow, conical-shaped piece which mates to the PPS fitting. Used
for Teflon tube connections.
InterfaceHarness: The bundle of tubing and electrical wires that connects the
ControllerUnit to the Reactor Unit.
PPS fitting: The tan colored threaded fittings made from PPS and used for
Teflon@*tubing connections.
*Teflonis a registered trademark of DuPont
Teflon tubing: The semi-transparent, semi-rigidtubing (0.125 inch [3.175 mm]
O.D.) used for gas and liquid connections.
Tygon tubing: The flexibletubing with a slight yellow color to it. Used for gas
connectionswithin the Quest 205 ControllerUnit.
Setting up the Quest 205 Synthesizer
1. Clear a space about 2-114 feet (70 cm) wide by 2 feet (60 cm) deep in a fume hood
for the Quest 205 Reactor Unit.
2. Clear a space on the lab bench adjacent to the fumehood for the Quest 205
ControllerUnit.
3. Carefullyunpack the instrument and place the Reactor Unit in the hood and the
ControllerUnit on the lab bench next to the hood. Remove any packaging material
from the units.
4. The Interface Harness is already connected to the Reactor Unit. Free the harness
from any packing material and lay it out sothe free end is placed in front of the
Controller Unit.
NOTE: It is recommended that the following safety equipment be readily available: fire
extinguisher, eyewash station, safety shower, eye protection, lab coat, and hand protection.
Argonaut Technologies
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