Argonaut Technologies QUEST 210 User manual

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UAL
Part Number 900114
ARGONAUT
TECHNOLOGIES
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Quest 210 Manual Synthesizer - User Manual
Part Number 900
114
Revision 1.O, 5 September 2000
Copyright 02000by Argonaut Technologies
All rights reserved.
Argonaut Technologies
887 Industrial
Rd., Suite G
San Carlos, CA 94070
Printed in the United States.
The information in this document has been carefully checked and is
believed to be entirely reliable. However, no responsibility is
assumed for inaccuracies. Statements in this document are not
intended to create any warranty, expressed or implied. Argonaut
reserves theright to make changes in any products herein to improve
reliability, function, or design. Argonaut does not assume any
liability arising out of the application oruse of any product
described herein; neither does it convey any license under its patent
rights nor the rights of others. Inclusion in this document does not
imply that any particular feature is standard on the instrument. The
information in this document is subject to change at any time.
Quest and pFrit are registered trademarks of Argonaut
Technologies, Inc. Teflon is a registered trademark of DuPont.
Tygon is a registered trademark of Norton Performance Plastics.
Other product names in this document are registered trademarks or
trademarks of their respective holders.
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Limited Warranty
All individual instrument parts, consumables and the like are subject
to the provisions of the Seller Limited One
(1) Year Warranty as
outlined below. Resin consumable products or the like are only
warranted to conform to the quantity and content stated on the label
at the time of delivery. All instrument system products are provided
subject to the provisions of the SELLER Limited One
(1) Year
Warranty,
a copy of which is available to Buyer and which is
incorporated herein in its entirety by this reference.
SELLER'S LIMITED ONE
(1) YEAR WARRANTY IS
EXCLUSIVE AND IN LIEU OFALL OTHER WARRANTIES,
AND SELLER MAKES NO OTHER WARRANTIES, EXPRESS
OR IMPLIED, EITHER IN FACT OR BY OPERATION OFLAW,
STATUTORY OR OTHERWISE, AND SELLEREXPRESSLY
EXCLUDES AND DISCLAIMS ANY WARRANTY OF
MERCHANTABILITY OR FITNESS FOR A PARTICULAR
PURPOSE.
Limitation of Liability
Buyer agrees that SELLER's liability to Buyer in any way
connected with the sale andlor license of products or services to
Buyer, regardless of the form of action, shall in no event exceed the
price paid by Buyer for such products or services. Under no
circumstances will SELLER be liable for any damages resulting
from SELLER's failure to meet any delivery schedule, even if
SELLER has been advised of the possibility of such damages. IN
NO EVENT WILL SELLER BE LIABLE FOR COSTS OF
PROCUREMENT OFSUBSTITUTEPRODUCTS OR SERVICES,
LOST PROFITS, OR ANY SPECIAL INDIRECT,
CONSEQUENTIAL OR INCIDENTAL DAMAGES, HOWEVER
CAUSED AND ON ANY THEORY OFLIABILITY, ARISING IN
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Exclusions
ANY WAY OUT OFTHE SALE AND/OR LICENSE OF
PRODUCTS OR SERVICES TO BUYER. THIS LIMITATION
SHALL APPLY EVEN
IF SELLER HAS BEEN ADVISED OF
THEPOSSIBILITY OF SUCH DAMAGES AND
NOTWITHSTANDING ANY FAILURE OFESSENTIAL
PURPOSE OFANY LIMITED REMEDY.
This limited warranty covers normal use. Exclusions from this
limited warranty may include:
Servicing or modification by anyone other than a qualified
Argonaut Technologies Service Representative;
Non-conformance to recommended instrument operating
procedures as noted throughout this manual;
Failure to perform routine preventative maintenance;
Any natural disaster, including earthquake, lightning, tornado,
flood, or fire; electrical surges or the use of improper power
sources.
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Warranty
Argonaut Warranty Agreement
Limited Warranty
Limitation of Liability
Exclusions
Contents
List
of Figures
1 Introduction
Interference Information
Immunity Information
Quest
2 10Overview
Automated Solvent Wash Option
Gaseous Reaction and Concentration Manifold Option
2 Safety
User Attention Words
Warning Labels
Safety Class
System Safety
Safety Equipment
Operating Environment
Material Safety Data Sheets (MSDS)
3 System Overview
Reactor
Reaction Vessels
Luer Ports
Heating and Cooling
Reaction Mixing
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Agitator Magnets
Solvent/Gas Delivery System
Upper and Lower Manifolds
Manifold Control Valves
Low Pressure Gas Valve
Bubbler Port
Solvent Bottle Assembly
Product Collection
AutoWash Port
Waste Tray and Waste Reservoir
Controller
LCD Screen
Display Screens
Keypad
MODE Button
FORWARD and BACK Buttons
VALUE SETTING Buttons
HEAT ONIOFFButton
AGITATOR Control Buttons
Mix Speed Valve
Controller Gas and Power Connections
Gas
Electrical Outlet
Power Switch
4 Quest 210 Installation
SitePreparation
Installation Requirements
Space
Gas
Electrical
Refrigeration
Materials
Components
Installation Glossary
Installation Procedure
Interface Harness Connections
SolventBottle Cap Assembly
Reactor Manifold Tubes
Waste Reservoir
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Manifold Control Valves
Gas Connection
Single Gas Source
Dual Gas Source
Bubbler
Power Connection
SolventBottle
ASW Option Installation
Overview
Installation Requirements
Space
Electrical Supply
Gas Supply
Waste Facilities
Ventilation
Installation Procedure
Location
Gas Connections
Power Connection
Controller and Reactor
ASW Module
SolventBottles
Installation Verification
Configuration
Manual Functions
Delivery Times
Automated Functions
6 Preparation For Synthesis
General
Line Power
Removing Reaction Vessels
Installing Reaction Vessels
Waste Reservoir
SolventBottle
Gas
7 Operation
Filling the Dead Volume
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Reagent and Solvent Delivery
Upper Manifold Membrane Valve
Parallel Delivery
Individual Delivery
Programming
Agitator Bar
Adjusting
Values
Starting and Stopping
Mix Speed
Temperature Control
Heating
Cooling
Draining Reaction Vessels
Non-Metered Draining
Metered Draining
Product Collection
8 Usingthe ASW Option
Programming
Program Number
Solvent Volume
Reactor Side
Draining Method
Variables
Wash Times
Washing
Monitoring The Wash
Editing Active values
Completion
Solvent Sparging
9 Cleaning & Maintenance
10 Tutorial
Overview
Summary of the Procedure
Preparation
Equipment Requirements
Reagent Requirements
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Reagent Preparation
Reductive Amination
Adding Reagent
Adding Sodium Borohydride
Product Work-Up and Collection
On-line Solid Phase Extraction
Off-Line Solid Phase Extraction
Cleaning and Maintenance
Manual Cleaning
Cleaning with the Automated Solvent Wash Module
Product Analysis
Tabulated Results and Structures
Spectroscopic Data
A Glossary
B Controller Screens
Start-upScreen
Firmware Version Screen
Menus
Agitator Values
Set Temperature
TemperatureMonitor Screen
Other Functions Menu
Set Contrast Menu
Self-Test Screen
Restore Defaults Screen
StartBtop Heaters Screen
C Specifications
Quest 210
Automated Solvent Wash Option
D Parts & Accessories
Quest 2 10Synthesizer
E Service
Contact Information
Index
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. ..
Vlll
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........................................
Figure 1 : Quest 210 Reactor 3-14
...................................
Figure 2 : Quest 210 Reactor Labels 3-19
Figure 3
: Manifold Control Valves (SolventDelivery Configuration) ........ 3-19
..........................................
Figure 4 : Quest Controller 3-23
...................................
Figure 5 : LCD Screen and Keypad 3-24
...........................................
Figure 6 : MODE Button 3-26
.............................
Figure 7 : FORWARD and BACK Buttons 3-26
.................................
Figure 8 : VALUE SETTINGButtons 3-27
....................................
Figure 9 : HEAT ONIOFF Button 3-27
................................
Figure 10 : AGITATOR ControlButtons 3-28
........................................
Figure 11 : Quest 210 Reactor 4-35
...............................................
Figure 12 : Controller 4-36
.....................
Figure 13 : Controller . Interface Harness Connections 4-37
............................
Figure 14 : SolventBottle Cap . Female Ports 4-38
.............................
Figure 15 : Manifold Control Valves Closed 4-39
.....................................
Figure 16 : Controller . Gas Inlets 4-40
Figure 17
: Recommended Set-Up of a Quest with the ASW Option .......... 5-46
................................
Figure 18 : ASW ControllerFront View 5-50
Figure 19
: Automated SolventWash module (ASW) Front Panel ............ 5-51
......................................
Figure 20 : Bottle Cap Assembly 5-51
..............................
Figure 21 : ASW SolventBottle Locations 5-52
..............................
Figure 22 : Quest Firmware Version Screen 5-54
Figure 23
: Representative SolventDelivery Times ........................ 5-57
.....................................
Figure 24 : Quest Start-up Screen 6-59
.................................
Figure 25 : Grasping the Top of the RV 6-60
Figure 26
: Breaking the RV free of the Lower Drain Manifold .............. 6-61
..........................
Figure 27 : The RV free of the Lower Manifold 6-61
.........................
Figure 28 : Inserting the 5 mL RV InsertionTool 6-64
...........................................
Figure 29 : Seatingthe RV 6-65
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Figure 30 : Properly Installed Reaction Vessels ........................... 6-65
Figure 31
: Controller Panel .......................................... 6-66
Figure 32
: Manifold Control Valves . Closed and Vent .................... 6-68
Figure 33
: Manifold ControlValves . Solvent Delivery and Low Pressure Gas . 6-69
Figure 34
: Manifold Control Valves . Both Closed ........................ 6-69
Figure 35
: Manifold Control Valves . Both Closed ........................ 7-72
Figure 36
: Pressurizing the Solvent and Venting the RVs .................. 7-74
......................................
Figure 37 : Purging the Manifold 7-74
Figure 38
: Sealing the Manifold ...................................... 7-75
.......................................... Figure 39 : Venting the RVs 7-75
Figure 40
: Purging the RVs .......................................... 7-77
Figure 41
: Blanketing RVs with Nitrogen ............................... 7-78
Figure 42
: Both Valves Closed ....................................... 7-78
Figure 43
: Example Agitator Cycle Plot ................................ 7-80
Figure 44
: Agitating Menu ........................................... 7-80
Figure 45
: Agitator Control Buttons ................................... 7-82
Figure 46
: SetTemperature Menu ..................................... 7-84
Figure 47
: Temperature Monitor Screen . Heating ........................ 7-85
Figure 48
: Temperature Monitor Screen . Cooling ........................ 7-86
Figure 49
: Auto SolventWash Menu with Program 1 Selected .............. 8-92
Figure 50
: Auto Solvent Wash Menu with First Line Displayed ............. 8-93
Figure 51
: Automated SolventWash Program . Lines 1-4 .................. 8-94
Figure 52
: Pressing MODE to Exit Menu ............................... 8-95
Figure 53
: Wash Time Params Menu .................................. 8-96
Figure 54
: To Start At Menu ......................................... 8-98
Figure 55
: Four Screens Displayed During Operation ..................... 8-99
Figure 56
: Editing An Active Value .................................. 8-100
Figure 57
: Program Pause Menu ..................................... 8-101
Figure 58
: Drain Path of Lower Manifold .............................. 9-107
Figure 59
: Reductive Amination to form Corresponding Secondary Amine . . 10-109
Figure 60
: Equipment Required ..................................... 10-111
Figure
6 1 : Reagents Required ...................................... 10-1 12
Figure 62 : Structures of Aniline and Benzaldehyde Reagents ............. 10-113
................................ Figure 63 : Reagent Addition Scheme 10-114
...............
Figure 64 : Results of SolutionPhase Reductive Amination 10-124
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Figure 65 : Structures of Amine Products .............................. 10-125
........................ Figure 66 : Quest Control Panel and LCD Screen B-131
........................ Figure 67 : Quest 210 Controller Start-up Screen B-131
........................ Figure 68 : Start-up Screen and Button Functions B-132
Figure 69
: Firmware Version Screen .................................. B-132
Figure 70
: Agitator Value Menu ..................................... B-133
Figure 71
: Agitator Value Menu and Button Functions ................... B-133
Figure 72
: SetTemperature Menu .................................... B-134
Figure 73
: Set Temperature Menu and Button Functions .................. B-134
Figure 74
: Temperature Monitor Screen ............................... B-135
............. Figure 75 : Temperature Monitor Screen and Button Functions B-135
Figure 76
: Other Functions Menu - Button Functions .................... B-136
Figure 77
: Set Contrast Menu ....................................... B-137
.
Figure 78 : Set Contrast Menu Button Functions ........................ B-137
Figure 79
: Self-Test Screen ......................................... B-138
Figure 80
: Self-TestScreen Button Functions ........................... B-139
Figure 81
: Restore Defaults Screen ................................... B-139
Figure 82
: StartIStopHeater Menu Screen ............................. B-140
Figure 83
: Self-Test Screen Button Functions...........................B-140
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INTRODUCTION
T
his manual is intended to assist you with the operation and
maintenance of the Quest 210 Organic Synthesizer. It is
organized intothe following chapters:
Chap t er 1 : I n t ro d uc t i on . Provides general information on
the Quest 210 Organic Synthesizer with a brief description of the
instrument.
C h ap t er 2 : Safety . Warnings and precautions appropriateto
the safe use of the Quest 210 and associated equipment.
Chapter 3: System Overview. Definition of the Quest
210 instrument and an overview of its operation.
Chapter 4: Quest 210 Installation. Step-by-step
instructions for installing the Quest 210.
Chapter 5: ASW Option Installation. Step-by-step
instructions for installing the Automatic Solvent Wash Option
(available separately).
Chapter 6: Preparation For Synthesis. Proceduresto
be followed prior to each use of the Quest 210.
C h ap t er 7 : 0 perat i on . Procedure for carrying out synthesis
with the Quest 210.
Chapter 8: Using The ASW Option. Cleaning the
Quest 210 with the Automatic Solvent Wash option, for optimum
instrument performance.
Chapter 9: Cleaning & Maintenance. Step-by-step
instructions for manual cleaning and maintenance of the Quest 210.
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IZITR0L)I:CTIoZ
Interference Information
Chapter 1 0 : Tutoria I. Step-by-step instructions, using a set
of actual examples, for reductive amination to form corresponding
secondary arnines.
Appendix A: Glossary of Terms.
Appendix
B: Controller Screens. A list ofthe
Controller screens and menus.
Appendix C: Specifications.
Appendix
D: Parts and Accessories.
A p p e n d i x E : Se r v i ce . Contact information for service and
sales.
INTERFERENCE INFORMATION
,11111..1.11..1s,a...,I....,,,.,,,...,....,...s...B
This equipment generates and uses radio frequency energy and, if
not installed and used in strict accordance with the manufacturer's
instructions, may cause interference to radio and television
reception. It 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 550 1 1 : 1997.
Class
B equipment is suitableforuse in domestic establishments and
in establishments directly connected to a low voltage power supply
network supplying power to buildings used for domestic purposes.
However, there is no guarantee that interference will not occur in a
particular installation.
If this equipment does cause interference to
radio or television reception, which can be determined by turning
the equipment off and on,theuser isencouraged to try to correctthe
interference by one or more of the following measures:
Reorient
the receiving antenna
Relocate the equipment with respect to the receiver
Move the equipment away from the receiver
Plug the equipment into a different outlet sothat the controller
and receiver are on different circuits
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INTRODUCTION '
Immunity Information
IMMUNITY INFORMATION
111111~~~~~mmm~rsm~mmm~nmmmmmmms11ammmmmm~~~mmmm~~~
This equipment has been type tested and found to comply with the
Requirements of the Generic Immunity Standard: EN50082-111997.
If the equipment is used in a manner not specified by the
manufacturer, the protection provided by the equipment may be
impaired.
QUEST 210 OVERVIEW
.......... ....*...........*.................,,..,,*
The Quest 21 0 Organic Synthesizer is designed for use
in chemical synthesis including potentially hazardous
chemical reactions.The potential hazardsof chemical
synthesis include but are not limitedto burns, explosions,
and exposureto toxic chemicals and carcinogens.
Always wear eye protection, suitable gloves, and
appropriate clothing. Operate the instrument in a fume
hood.
The Quest 210 Organic Synthesizer allows you to perform up to 20
solution or solid phase organic chemistry reactions in parallel. The
unique design of the Quest
2 10incorporates heating and cooling,
agitation, and the inert environment needed for organic synthesis.
The system's ease of use and intuitive operation allow new users to
quickly integrate the Quest 210 into their syntheses.
The Quest 210 consists of four main parts:
Reactor
Interface Harness
Controller
Solvent Bottle Assembly
Re act 0 r Compounds are synthesized on the Reactor. With two
banks of 10reaction vessels, the Reactor can synthesize up to 20
compounds in parallel. Each bank of reaction vessels has an
integrated heatinglcooling block for reaction heating and cooling.
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The Reactor also has rotary controls for solvent and gas delivery.
Using these controls, solvents or reagents can be added to the
reaction vessels in parallel. Luer ports located on top of each
reaction vessel allow for the individual addition of reagent or
solvents. Agitation is accomplished
by moving a magnetic bar
located between the two banks of reaction vessels vertically up and
down. Magnets placed in the vessels are attracted to the magnetic
agitator bar and follow its movement, effecting mixing of reaction
vessel contents.
Interface Harness TheReactorisconnectedtothe
Controller by the Interface Harness. ~eflon@tubing in the harness
delivers gas and solvent to the Reactor. The harness also contains the
wiring for the heaters and thermocouple for each bank of reaction
vessels. The Interface harness consists of the following lines:
SolventDelivery lines: Delivers solvent from the solvent
bottle(s) to the Reactor. Solventis delivered in parallel to each
bank of reaction vessels.
High Pressure Gas line: Delivers 30 psig (3.1 bar) gas from the
Controller to the Reactor. This supplies the pressure to drain
liquid from the reaction vessels and to dry solid phase resin.
Low PressureGas line: Delivers 10psig (1.7 bar) gas from the
Controller to the Reactor, This line connects to the Low Pressure
Gas valve which controls the gas flow for blanketing, draining,
and purging the reaction vessels with inert gas.
Agitator Gas lines: Two 30 psig lines (3.1 bar) deliver gas to the
pneumatically controlled Agitator Bar.
Electrical wiring: Provides voltage forthe heaters, and electrical
connections for the temperature sensors for each reaction vessel
bank.
C o n t r o l l e r The Controller enables fine control of solvent and
gas delivery, and the temperature of the RVs in the Reactor. It has a
LCD screen and buttons for programming the reaction temperature,
time, and agitator conditions using the system's firmware. It also
provides connections for system power and 30-40 psig (3.1-3.8 bar)
gas.
Solvent, high pressure gas, and low pressure gas deliveries are
controlled using the mechanical Control Valves on the Reactor. The
User programs the Controller with the agitator and heating values.
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INTRODUCTION '
Quest 210 Overview *
The Controller firmware implements the agitator and temperature
program for the synthesis.
Solvent Bottle Assembly The Solvent Bottle Assembly
consists of the Solvent Bottle Cap Assembly and a solvent bottle
(user-supplied in North America). The Caphas four Teflon lines,for
pressure, venting, delivery, and solvent pick
up. A two-position
valve on top of the Solvent Bottle Cap Assembly allows the user to
vent and pressurize the solvent bottle. The Solvent Bottle Assembly
connects to the Interface Harness for solvent or reagent delivery to
the Reactor.
> NOTE
Solvent, high pressure gas, and low pressure gas deliveries are
controlled using the mechanical Control Valveson the Reactol: The
userprograms the Controller with the agitator and heating values.
AUTOMATEDSOLVENTWASHOPTION
The optional Automated Solvent Wash (ASW) provides the benefit
of programmable wash cycles using up to four solvents. The ASW
consists of a Quest Synthesizer Controller with additional software
forprogramming wash cycles, additional gas connections, and a new
distribution manifold.
GASEOUSREACTION AND CONCENTRATIONMANIFOLDOPTION
The Gaseous Reaction and Concentration Manifold (GRCM)
accessory is available separately.It enables the Quest 210 to perform
gaseous reactions and concentration by evaporation.
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