Synthos 3000 Reference Manual

-EASURE
WHATISMEASURABLE
ANDMAKEMEASURABLE
THATWHICHISNOT
'ALILEO'ALILEI
Synthos 3000
Microwave Synthesis
Reference Manual
Anton Paar GmbH assumes no liability for technical or printing errors or omissions in this document.
Nor is any liability assumed for damages resulting from information contained in the document.
Anton Paar GmbH reserves the right to content changes. This also extends to changes to delivery
volumes or any features of delivered parts.
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as such. They are the property of their respective owner.
Published by Anton Paar

Printed: Anton Paar, Austria
Copyright © 2006 Anton Paar GmbH, Graz, Austria
Address: Anton Paar GmbH

Anton-Paar-Str. 20
A-8054 Graz / Austria – Europe
Tel: +43 316 257-0
Fax: +43 316 257-257
E-Mail: info@anton-paar.com
Web: www.anton-paar.com
Date: 12.2006
Document number C49IB08A

1 Introduction ..................................................................................................................................... 5
2 Symbols ........................................................................................................................................... 6
2.1 Symbols in the Instruction Manual .......................................................................................... 6
2.2 Safety Symbols Applied to the Instrument .............................................................................. 6
3 Safety Instructions .......................................................................................................................... 8
3.1 General Safety Instructions for Synthos 3000 ........................................................................ 9
3.2 Safety Instructions for Chemical Synthesis .......................................................................... 12
3.3 Unexpected Operation Behavior ........................................................................................... 14
4 Technical Description of Synthos 3000 ...................................................................................... 17
4.1 Working Principle .................................................................................................................. 17
4.2 Fields of Application .............................................................................................................. 18
4.3 Technical Description of the Instrument ................................................................................ 19
4.3.1 Microwave Heating ................................................................................................ 22
4.3.2 Magnetron Protection ............................................................................................ 22
4.3.3 Unpulsed Energy Control ...................................................................................... 22
4.3.4 Safety Features ..................................................................................................... 23
4.3.5 Cooling and Exhaust ............................................................................................. 26
4.3.6 Rotor Detection ..................................................................................................... 27
4.4 Technical Description of the IR Temperature Sensor Accessory .......................................... 30
4.5 Technical Description of the Pressure /Temperature Sensor Accessory .............................. 31
4.5.1 Pressure Measurement ......................................................................................... 33
4.5.2 Temperature Measurement ................................................................................... 34
4.6 Technical Description of the T-Probe .................................................................................... 36
4.6.1 Temperature Measurement ................................................................................... 37
4.7 Technical Description of the Safety Module SOLV ............................................................... 38
4.8 Technical Description of the Solvent Sensor Accessory ....................................................... 39
4.8.1 Installation ............................................................................................................. 39
4.8.2 Function Verification .............................................................................................. 41
4.9 Technical Description of the Magnetic Stirrer Device ............................................................ 45
5 Installation ..................................................................................................................................... 46
5.1Installation Requirements ..................................................................................................... 46
5.1.1 Exhaust System .................................................................................................... 46
5.1.2 Electrical Requirements ........................................................................................ 47
5.2 Installation Steps ................................................................................................................... 48
5.3 Connecting Accessories ....................................................................................................... 51
5.3.1 Printer .................................................................................................................... 51
5.3.2 Keyboard ............................................................................................................... 51
5.3.3 External Computer ................................................................................................ 51
5.4 Activating / Deactivating Rotors, Sensors and Accessories ................................................. 52
5.5 Microwave Power Calibration ............................................................................................... 53
6 Software ......................................................................................................................................... 58
6.1 General Information .............................................................................................................. 58
6.2 Basic Software Structure ...................................................................................................... 60
6.3 The Main Menu ..................................................................................................................... 61
6.4 Library Menu ........................................................................................................................ 62
6.4.1 Sample Menu ........................................................................................................ 63
6.5 Review .................................................................................................................................. 69
6.5.1 Review - Displayed Diagrams ............................................................................... 70
6.6 Setting Up the Instrument ..................................................................................................... 74
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6.6.1 Configuration ......................................................................................................... 75
6.6.2 Printer Setup ......................................................................................................... 76
6.6.3 Serial Port Setup ................................................................................................... 78
6.6.4 Safety Cooling ....................................................................................................... 79
6.6.5 Rotors .................................................................................................................... 80
6.6.6 Sensors ................................................................................................................. 81
6.6.7 Accessories ........................................................................................................... 82
6.7 Service .................................................................................................................................. 83
6.7.1 Software Update .................................................................................................... 84
6.7.2 Power Calibration .................................................................................................. 84
6.7.3 Power Check ......................................................................................................... 85
6.7.4 Temperature Sensor Calibration with the Calibration Accessory .......................... 86
6.7.5 Temperature Sensor Calibration with the Calibration Unit ..................................... 94
6.7.6 Temperature Sensor Check with the Calibration Accessory ............................... 109
6.7.7 Temperature Sensor Check with the Calibration Unit ...........................................110
6.7.8 Temperature Sensor Settings ...............................................................................112
6.7.9 IR Sensor Calibration with the Calibration Accessory ..........................................114
6.7.10 IR Sensor Calibration with the Calibration Unit ....................................................118
6.7.11 IR Sensor Check with the Calibration Accessory ................................................ 122
6.7.12 IR Sensor Check with the Calibration Unit .......................................................... 124
6.7.13 Solvent Sensor Settings ...................................................................................... 125
6.7.14 Exhaust Unit Installation ...................................................................................... 127
6.7.15 Library Maintenance Tool .................................................................................... 127
6.7.16 Advanced Service Routines ............................................................................... 129
6.8 Info ...................................................................................................................................... 130
6.9 AP Softprint ......................................................................................................................... 131
7 Troubleshooting .......................................................................................................................... 132
7.1 Software .............................................................................................................................. 132
7.1.1 Error Message Menu - List of Error Codes .......................................................... 132
7.1.2 Pop-up Error Messages in the Case of an "Alarm" ............................................. 134
7.1.3 Pop-up Messages During System Check ............................................................ 138
7.1.4 Pop-up Error Messages During System Check ................................................... 139
7.1.5 Pop-up Error Messages Under Various Conditions ............................................. 143
7.1.6 Pop-up Error Messages During "Power Calibration" ........................................... 147
7.1.7 Pop-up Error Messages During "Temp. Sensor Calibration" and "Temp. Sensor
Check" ................................................................................................................. 149
7.2 Rotor 16 and Rotor 8S ........................................................................................................ 151
7.3 Sensors .............................................................................................................................. 152
8 Rotor 48MF50 .............................................................................................................................. 153
8.1 Technical Description of Rotor 48 ....................................................................................... 153
8.1.1 Vessels for Rotor 48 ............................................................................................ 155
8.2 Limitations of Operation ...................................................................................................... 156
8.2.1 Number of Vessels .............................................................................................. 156
8.2.2 Temperature profiles ............................................................................................ 157
8.2.3 Power Profiles ..................................................................................................... 157
8.2.4 Fan Settings ........................................................................................................ 157
8.3 Prior to the First Reaction ................................................................................................... 158
8.4 Performing a Reaction ........................................................................................................ 159
8.4.1 Adding Reagents and Solvents ........................................................................... 159
8.4.2 Closing the Vessels ............................................................................................. 160
8.4.3 Loading Rotor 48 ................................................................................................. 163
8.4.4 Performing a Synthesis Run ................................................................................ 165
8.4.5 Unloading Rotor 48 ............................................................................................. 167
8.5 Cleaning and Maintenance ................................................................................................. 170
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8.5.1 Cleaning of the Reaction Vessels ........................................................................ 170
8.5.2 Cleaning After Every Run .................................................................................... 171
8.5.3 Checking After Every Run ................................................................................... 174
8.5.4 Standard Cleaning and Maintenance Procedures ............................................... 175
8.5.5 Procedures After the Rupture of a Safety Disk ................................................... 179
8.5.6 Procedures After a Vessel Explosion .................................................................. 185
8.6 Maintenance of the Pressure / Temperature Sensor M50 .................................................. 195
8.6.1 Replacing Seal and Safety Disk .......................................................................... 195
8.6.2 Replacing the Thermometer Capillary ................................................................. 200
8.6.3 Replacing the Immersion Tube ............................................................................ 202
9 Rotor 16MF100 / 16HF100 .......................................................................................................... 205
9.1 Technical Description of Rotor 16 ....................................................................................... 205
9.1.1 Vessels for Rotor 16 ............................................................................................ 207
9.2.1 To Prepare the First Run ..................................................................................... 209
9.3 Performing a Synthesis ....................................................................................................... 210
9.3.2 Assembling the Vessels .......................................................................................211
9.3.3 Loading Rotor 16 ................................................................................................. 220
9.3.5 Unloading Rotor 16 ............................................................................................. 223
9.4.5 Procedures After the Breakage of a Safety Disk ................................................. 244
9.4.7 Intensive Cleaning of Ceramic Vessels ............................................................... 253
9.5 Maintenance of the Pressure / Temperature Sensor Accessory ......................................... 255
9.5.1 Replacing Seal and Safety Disk .......................................................................... 255
9.5.3 Replacing the Immersion Tube ............................................................................ 263
10 Rotor 8SXF100 / 8SXQ80 ............................................................................................................ 265
10.1 Technical Description of Rotor 8S ....................................................................................... 265
10.1.1 Vessels for Rotor 8S ............................................................................................ 267
10.2.1 To Prepare the First Run ..................................................................................... 270
10.3 Performing a Synthesis ....................................................................................................... 271
10.3.2 Assembling the Vessels ...................................................................................... 272
10.3.3 Loading Rotor 8S ................................................................................................ 281
10.3.5 Unloading Rotor 8S ............................................................................................. 287
10.4.5 Procedures After the Rupture of a Safety Disk ................................................... 312
10.4.7 Intensive Cleaning of Ceramic Vessels ............................................................... 323
10.5 Maintenance of the T-Probe and the Immersion Tube with Seal XF / XQ .......................... 324
10.5.1 Replacing the Seal and Safety Disk .................................................................... 324
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11 Applications ................................................................................................................................ 332
11.1 General Information ............................................................................................................ 332
11.1.1 Basics of Microwave Heating .............................................................................. 333
11.1.2 Hazards During Microwave Synthesis ................................................................. 335
11.1.3 Reagents ............................................................................................................. 338
11.2 Performing Synthesis .......................................................................................................... 347
11.2.1 General ................................................................................................................ 347
11.2.2 Operation Without an Internal Temperature Sensor ............................................ 348
11.2.3 Operating With Sensors ...................................................................................... 348
11.2.4 Interpretation of Results ...................................................................................... 351
11.2.5 Power Reduction by the Instrument ................................................................... 351
12 Appendix ...................................................................................................................................... 353
12.1 Addresses ........................................................................................................................... 353
12.2 Packing the Synthos 3000 and the Rotors ......................................................................... 354
12.2.1 Packing the Instrument ........................................................................................ 354
12.2.2 Packing the Rotors .............................................................................................. 358
12.3 Technical Data of the Instrument ........................................................................................ 360
12.3.1 Synthos 3000 Microwave Oven ........................................................................... 360
12.3.2 Options ................................................................................................................ 362
12.3.3 Rotor 48MF50 ..................................................................................................... 362
12.3.4 Rotor 16 MF100 .................................................................................................. 363
12.3.5 Rotor 16 HF100 ................................................................................................... 363
12.3.6 Rotor 8SXF100 .................................................................................................... 364
12.3.7 Rotor 8SXQ80 ..................................................................................................... 364
12.4 List of Spare Parts .............................................................................................................. 365
12.5 Safety Certification .............................................................................................................. 366
12.6 CE Declaration of Conformity ............................................................................................. 368
12.7 Safety Declaration for Repair and Malfunction Report ....................................................... 369
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1 Introduction
1 Introduction
Synthos 3000 is a scale-up-instrument for microwave-assisted chemical

synthesis. It has different rotors for various fields of application in organic
synthesis chemistry employing closed vessels. Powerful microwave generators
(magnetrons) allow efficient heating of large amounts of solvents.
Fig. 1 - 1 Synthos 3000
Parallel rotors with up to 48 positions can be used to carry out temperature-

dependent processes in the microwave field, saving time. A specially designed
rotor with robust quartz glass vessels enables reactions under extreme pressure
and temperature conditions which are difficult to reach safely with conventional
systems.
The components are highly compatible with each other, making the system
suitable for a variety of different applications.
Synthos 3000 excels in:

• Easy operation
• Excellent reproducibility of results
• Direct scalability of reaction protocols up to the liter scale
• Maximum safety under extreme conditions
• Effective scale-up and high sample throughput
This makes Synthos 3000 a high-performance instrument for the production of

numerous compounds in pharmaceutical, biomedical and other organic-chemical
synthesis laboratories.
Synthos 3000 has been developed by Anton Paar GmbH as a result of its long-
standing experience and in close cooperation with the Karl-Franzens University
in Graz, Austria.
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2 Symbols
2 Symbols
2.1 Symbols in the Instruction Manual
Warning:
The "Warning" sign indicates a hazard.
It calls attention to an operating procedure, practice, etc. which could result in
injury or loss of life, if not correctly performed or adhered to.
Do not proceed beyond a "Warning" sign until the indicated conditions are
fully understood and met.
Important:
The "Important" sign indicates a hazard.
It calls attention to an operating procedure, practice, etc. which could result in
damage or destruction of the instrument or parts of it, if not correctly
performed or adhered to.
Do not proceed beyond an "Important" sign until the indicated conditions are
fully understood and met.
Hint:
The "Hint" sign calls attention to additional information, which might be
useful to the operator.
2.2 Safety Symbols Applied to the Instrument
Warning screen located on the front door of the instrument.
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2 Symbols
Warning screens located on the front side and on the right side panel of the
instrument.
Symbol located on the rotors: Refer to the manual!
Warning screen located on Rotor 48.
Symbol located on the calibration accessory: Caution - hot surface!
C49IB08A 7
3 Safety Instructions
Synthos 3000 has been tested and is listed for compliance with US, Canadian
and European standards by Intertek Testing Services, which is an accredited
testing lab. The instrument was found to be fully compliant with the Equipment
Safety Law. This indicates the high safety standard of the Synthos 3000 system.
Hint:
This instruction manual is supplied with Synthos 3000 and contains important
information and warnings that must be followed by the user to ensure safe
operation and to maintain the instrument in safe condition. This manual is
intended to supplement, not supersede, the normal safety code of conduct of
each individual country of operation.
The provided information does not cover every safety procedure that should be
practiced. Ultimately, the operator's organization bears responsibility for the
adherence to safety rules. Possible hazards that could harm the user or result in
damage to the instrument are clearly stated at appropriate places throughout this
instruction manual as well as in the reference manual.
C49IB08A 8
3.1 General Safety Instructions for Synthos 3000
Important:
Read this reference manual carefully before the first use of your instrument!
Make sure that all instructions are fully understood and met to ensure safe
and efficient operation of Synthos 3000.
Warning:
The instrument cavity is equipped with light emitting diodes (LED). Do not look
directly into the light with optical instruments as the LEDs are class 1M laser
products.
• All operators have to be sufficiently trained in the correct and safe use of this
instrument. Operators must be able to judge dangerous situations and take
the right measures to prevent accidents, injuries and damages.
• The operation of the pressure vessels may be liable to individual national

regulations. The operator is responsible for the correct installation, handling
and service of the pressure vessels and for sufficient training of the operating
staff.
• Do not use Synthos 3000 for any purpose other than described in this
instruction manual or the reference manual, respectively. Anton Paar GmbH
accepts no responsibility for injuries or damages caused by unauthorized
use of the instrument.
• Follow the installation instructions provided with this manual. The installation
has to be carried out by qualified personnel who are able to read, understand
and apply these instructions.
• This instrument is not designed for operation in an explosive atmosphere.
• Synthos 3000 is equipped with strong permanent magnets. Keep the

following items away from Synthos 3000: credit cards and other cards with a
C49IB08A 9
magnetic read-write band, pacemakers or similar items, magnetic storage

media such as floppy disks, DAT, ZIP, video cassettes, as they might be
damaged by the permanent magnets.
• Do not lift or carry the instrument by its door.
Warning:
Do not lean against the instrument or the door, respectively.
In case of a sudden pressure build-up inside the cavity (opening of a safety
disk, vessel breakage) the door will slightly open for less than a second and
noxious reaction gases may be released.
Warning:
This instrument features strong magnets to close the door.
People with pacemakers should keep a distance of at least 50 cm to the
instrument.
During operation (microwave energy "ON") an electromagnetic field is
generated by two transformers. Keep a safe distance of approx. 1 m to ensure
maximum safety.
• Under adverse conditions chemical syntheses may lead to violent,

spontaneous reactions in which gaseous reaction products and solvent
vapors may escape. Thus, the Synthos 3000 has to be installed in a fume
hood.
• The hood must be closed immediately after starting an experiment.
• Do not to store containers with flammable reagents or other ignitable

materials (e.g. soaked cleaning paper) close to the instrument.
• Indoor use only!
• Synthos 3000 should be supervised at all times during operation.
Warning:
- Never open the door during a running program!
- If you abort a reaction procedure, wait until the safety cooling has been
automatically stopped, i.e. the vessel temperatures are lower than the
above mentioned limits.
- After a mains power failure, wait for the vessels to cool down sufficiently
before taking the rotor out. If a failure does not allow you to activate the
safety cooling, it may take up to six hours for the vessels to cool down!
• In case of a safety disk breakage turn off the instrument after the cooling has
been finished, and remove the rotor. Clean the instrument and rotor parts
carefully and inspect them for visual damage. If the door shows deformations
or can no longer be closed tightly, an increased risk of microwave radiation
C49IB08A 10
leakage may consist. Do not continue to operate Synthos 3000 unless an

authorized service engineer has checked the instrument for microwave
radiation leakage.
• Never clean the rotor body and lid with organic solvents, especially
halogenated hydrocarbons or acetone.
• Never leave a rotor inside the Synthos 3000 oven when transporting the
instrument. This could damage the microwave cavity or the door.
Warning:
Do not open the instrument casing, as this would uncover live parts. Repair
work has to be carried out by authorized field service engineers or by
Anton Paar GmbH only.
• Anton Paar GmbH warrants proper function and safe operation only if no
unauthorized modifications have been made to mechanical or electronic
parts or software.
• When passing this instrument to other users, also hand over all
documentation and manuals.
C49IB08A 11
3.2 Safety Instructions for Chemical Synthesis
• Synthos 3000 is a scale-up instrument for use with optimized microwave

protocols. Using the instrument to develop new methods requires special
caution.
Warning:
Always wear goggles, protective gloves and appropriate protective clothing
when handling chemical reagents. Follow any special national safety
regulations.
• When performing a new synthesis for the first time, begin with small amounts
and diluted solutions.
• Never carry out syntheses in open vessels in the Synthos 3000.
Warning:
Do not use any sensors, accessories or consumption parts other than those
supplied by Anton Paar GmbH, as this might result in serious damage to the
instrument or injuries of users.
• Never operate Synthos 3000 without sufficient load. Never use less than 4
vessels, as surplus microwave energy may interact with rotor parts and
damage them.
• Do not mark plastic parts of pressure vessels or rotors of microwave systems

with pencils or markers containing conductive ink. A line of electrically
conductive substance on the surface of a plastic part may interact with the
microwave field, leading to local overheating of the plastic material up to
destruction of rotors.
• Make sure to apply reaction mixtures with adequate coupling efficiency. If

you use materials with poor microwave absorption properties, we
recommend using special heating elements.
• Allow the vessels to cool down to a vessel interior temperature below 60 °C

and to a vessel surface temperature (IR) below 50 °C before removing the
rotor. Hot and pressurized vessels are dangerous if removed from the
instrument.
• Vent the reaction vessels either inside the microwave cavity of Synthos 3000
with the exhaust unit activated or under a working fume hood. Noxious
gaseous reaction products may be released.
• Do not operate Synthos 3000 if a fault is suspected.
C49IB08A 12
• If there is a fault (e.g. opening of the safety disk) let the safety cooling run for
at least one hour then switch of the instrument. Refer to the reference
manual. Clean the instrument carefully and inspect it for visible damage. If
the door can no longer be closed tightly, there is a danger of increased
microwave radiation. Do not continue operating Synthos 3000.
• After a (very unlikely) explosion of a vessel, do not continue with synthesis

reactions. A service engineer has to perform an inspection and microwave
leakage test.
C49IB08A 13
3.3 Unexpected Operation Behavior
Synthos 3000 has been designed for safe operation even in case of incidents. In
case of safety disk- or vessel breakage, the microwave power is shut down
immediately due to the sudden overpressure release inside the cavity and the
safety door opening. Normally, the safety cooling is activated simultaneously.
Let the safety cooling run for at least one hour, then switch off the instrument and
proceed as described in the reference manual.
Although highly unlikely, it is still possible that a reaction procedure is terminated

in an abnormal way due to an instrument failure. In such a case it is vital to act
properly, thus strictly adhering to the instructions below.
Warning:
In case of unexpected operation behavior, NEVER open the door of
Synthos 3000!
Hot and pressurized vessels inside!
The opening of the door will deactivate a vital safety feature, which is
indispensable to ensure user safety.
After a power failure:
• Switch on the instrument again. If the safety cooling does not start
automatically, gently pull the door (Fig. 3 - 1). The door will still be held by its
safety hooks, while the door switches will trigger the safety cooling.
Do not use the door opener! Switch off the instrument after one hour of
safety cooling, as the cooling will not stop automatically.
Fig. 3 - 1 Manual activation of safety ccoling
• If the instrument cannot be switched on again, wait for the vessels to cool
down. Depending on the reached temperature, the type of vessels as well as
the number and loading of the vessels, it may take up to six hours for the
vessels to cool down!
Do not open the door earlier than after these six hours!
C49IB08A 14
Warning:
Before removing a rotor from a switched off instrument, make sure that rotor
and vessels have been cooled down completely! To do so, you can switch on
the instrument and check if the last run was finished completely (Review
menu).
If you are not sure whether rotor and vessels have cooled down, wait at least
six hours before removing the rotor.
After an exhaust unit failure:
• Wait for the vessels to cool down. If the exhaust unit fails during the run,
terminate the run by pressing the <Stop> button twice. Depending on the
reached temperature, the type of vessels as well as the number and loading
of the vessels, it may take up to six hours for the vessels to cool down!
Do not open the door earlier than after these six hours!
After a system failure:
• In very rare cases the instrument might reset during a run. After the
automatic restart the safety cooling is usually activated by default. If the
safety cooling does not start automatically, gently pull the door (Fig. 3 - 1).
The door will still be held by its safety hooks, while the door switches will
trigger the safety cooling. Do not use the door opener! Switch off the
instrument after one hour of safety cooling, as the cooling will not stop
automatically.
• If the safety cooling can not be started, wait for the vessels to cool down.
Depending on the reached temperature, the type of vessels as well as
number and loading of the vessels, it may take up to six hours for the vessels
to cool down! Do not open the door earlier than after these six hours!
In case of fire inside the microwave cavity:
• Switch off the instrument. Never open the door to extinguish the fire! The
emitted flue gas will cause the fire to die out rapidly. Thus do not activate
the safety cooling!
Warning:
Hot pressure vessels!
Overheating may result in rupture of safety disks or vessels! The design of the
oven cavity ensures user safety even in case of unexpected operation
behavior. This safeguard is only provided if the door is kept shut!
• As a precaution keep a fire extinguisher ready or call for corresponding

assistance.
• Due to the possibility of escaping fumes it is recommended to switch on the

fume hood(s) and to leave the lab. Look after the instrument temporarily.
C49IB08A 15
• After the fire is extinguished wait at least six hours before opening the door.
Waiting six hours ensures that rotor and vessels are cooled down sufficiently
and overpressure is diminished.
Important:
Always check rotor and vessels carefully for damage if a run has been
interrupted unexpectedly.
C49IB08A 16
4 Technical Description of Synthos 3000
The following chapters contain a short description of the working principle, fields
of application and the technical description of the instrument as well as of
available sensor accessories.
4.1 Working Principle
The reagents are weighed into the reaction vessels made of quartz or
fluoropolymers. The vessels are closed by a screw cap (Rotor 16 and Rotor 48)
or by a seal holder (Rotor 8S). The vessels are sealed either with a self-sealing
lip-type seal (Rotor 8S and Rotor 16) or a conical seal (Rotor 48). The pressure
vessels are inserted into the rotor, the closed rotor is placed into the Synthos 3000
oven and the door is closed.
A built-in microcontroller controls the reaction processes, stores a method library

and documents the reaction process.
Depending on the rotor type and accessories used, the operating pressure and
temperature can be recorded simultaneously and displayed.
The measured data is transmitted wireless from the rotor to the built-in
microprocessor. As soon as one of the predefined limits is reached, the
microwave energy is reduced or completely switched off. If necessary, cooling
intensity is increased.
In addition the surface temperature of the reaction vessels is measured using an

infrared sensor.
During the process, the integrated cooling system generates a slight cooling air
flow along reaction vessels and therefore protects rotor components against
excessive thermal stress of rotor and vessels. This has a positive effect on the
service life of the components.
C49IB08A 17
4.2 Fields of Application
The main field of application for Synthos 3000 is the synthesis of organic
compounds in the pharmaceutical, biomedical and agrochemical industry in the
50-250 g range using optimized methods.
The numerous accessories for Synthos 3000 also make it ideal for special
applications such as reactions under different atmospheres, extreme pressure
and temperature conditions and for carrying out cleaning and processes steps.
Compared with other microwave synthesis systems, Synthos 3000 provides the
highest safety standards, high quality accessories and excellent reproducibility of
the experiments. This is due to:
• unpulsed continuously adjustable microwave energy over the whole power

range
• direct scalability, from milliliters to liters without changing the reaction

parameters
• the highest available pressure and temperature limits
• innovative and practical rotor and vessel design
• efficient vessel cooling
• easy-to-operate program functions.
As well as conventional microwave-assisted synthesis, the following applications

can also be carried out:
• Reactions under pressure with individually applied reactant or inert gas

atmosphere
• Efficient high-temperature synthesis with low absorbing solvents utilizing

silicon carbide (SiC) heating elements
• Near critical water chemistry
• Protein hydrolysis
• Solid phase synthesis including cleavage and filtration in the same vessel
C49IB08A 18
4.3 Technical Description of the Instrument
The microwave cavity is sealed by a safety door, which can be opened easily by
pressing the door opener button.
Above the door is a graphic display and an acid- and water-repellent keypad.
To the right of the keypad is space to place the alphanumeric keyboard.
The main switch for the instrument is located at the front lower right corner of the
instrument.
Door opener button
Graphic display Keypad foil * (not visible)
Space for the

alphanumeric keyboard
Door
Mains switch
Fig. 4 - 1 Front view of Synthos 3000
C49IB08A 19
Turntable
Fig. 4 - 2 View into the opened microwave cavity

(without rotor on the left, with rotor on the right)
Exhaust unit
Fitting for exhaust hose
Electrical supply of the

exhaust unit
Mains supply
Fig. 4 - 3 Rear side of Synthos 3000, view of the exhaust unit
The exhaust unit and the appropriate electrical connections are located on the
rear side of the instrument together with the mains supply socket.
Ports for optional accessories, interfaces and the view angle control knob for the
graphic display are located on the right side of the instrument:
C49IB08A 20
3 1 4 5 6
2 7
Fig. 4 - 4 Electrical connections/ports on the right side of Synthos 3000
1 Serial RS 232C interface (COM1)

This port is used to connect Synthos 3000 to the serial
(RS 232C) interface of a PC via a serial link cable (0-Modem
cable, Mat.No. 70429). For computer with USB-port only an
USB to RS232 converter cable (Mat.No. 17562) is needed.
2 Serial RS 232C interface (COM2)

This port is for maintenance purpose only.
3 View angle control for the graphic display (VIEW ANGLE)

Use this knob to adjust the view angle of the graphic display
(LCD).
4 External alphanumeric keyboard (KEYB)

This port can be used to connect the alphanumeric keyboard.
5 Calibration port (CAL)

The temperature sensor accessories must be calibrated from
time to time. Use this port to connect the temperature
calibration accessory for calibration of the sensor accessories.
6 Auxiliary port for optional accessory (AUX)

This port can be used to connect auxiliary/optional accessories
(e.g. solvent sensor).
7 PRINTER
Parallel (Centronics) interface to connect printers.
C49IB08A 21
4.3.1 Microwave Heating
Microwave radiation is an electromagnetic radiation in the frequency range from

300 MHz to 300 GHz. Synthos 3000 comes with two microwave generators
(magnetrons) that generate microwave radiation at a frequency of 2.45 GHz.
Materials exposed to microwave radiation will react differently depending on their

dielectric constants. They may reflect the microwaves (e.g. metals) or allow the
permeation of radiation without being heated up (e.g. glass or plastics). Other
substances, i.e. water, can absorb microwave energy, whereas polar molecules
are stimulated to oscillate and dissolved ions can be moved through the
electromagnetic field. Both effects cause the substance to heat up.
These properties are the key to fast and efficient heating time of aqueous
solutions and other polar substances. In contrast to the conventional heating in
heating blocks or ovens (where the heat has to be transferred to the medium via
metal parts, air or vessels), microwave radiation heats up the medium directly,
which results in significant saving of time in many fields of application.
4.3.2 Magnetron Protection
In order to prevent damage of the magnetrons by reflected power and to increase

the service life of magnetrons, several features are installed in the instrument:
• Optimized waveguides for minimum reflected power

• Magnetron core temperature control
• Magnetron thermoswitch
• Soft start electronics
4.3.3 Unpulsed Energy Control
The unpulsed ("continuous") energy control contributes significantly to the

synthesis quality and operational safety of the system.
Fig. 4 - 5 Comparison of pulsed and unpulsed energy control
C49IB08A 22
Energy supply of conventional microwave instruments usually applies maximum

power in various duty cycles only. As a consequence, even at low power levels
samples are irradiated with maximum power, thus making it difficult to control
critical reactions.
Synthos 3000 supplies unpulsed microwave energy over the entire power
range.
This brings the following benefits:
• Uniform heating properties
• Enhanced reaction control
• Prevention of spontaneous reactions
• Shorter reaction times
4.3.4 Safety Features
The pressure / temperature (p/T) monitoring and unpulsed microwave energy

control ensure a high degree of operational safety. To ensure maximum protection
in the case of spontaneous reactions, Synthos 3000 has been equipped with
additional safety features.
Safety features:
• Monitoring of the pressure increase rate

• Built-in metal safety disks
• Use of special vessel jackets
• Effective rotor design
• Special construction of the instrument door
• Effective safety cooling
• Monitoring of the pressure increase rate
If a p/T sensor accessory (optional) or Rotor 8S is used, the pressure increase

rate can be limited to 0.1 - 3.0 bar/sec.
By reducing the limit of the pressure increase rate, spontaneous reactions can be
controlled very quickly by automatically reducing the microwave power in an early
stage of the reaction.
A possible rupture of the safety disk can be prevented in most cases.
C49IB08A 23
In addition, the sensor unit includes a second electronic protection circuit that
reacts as soon as the maximum pressure increase rate of 3.0 bar/s is exceeded.
In this case, microwave power is completely shut down (temporarily) and safety
cooling is activated.
• Built-in metal safety disks
Each pressure vessel is protected by a metal safety disk. If the pressure exceeds
the permitted pressure limit (due to spontaneous chemical reactions or thermal
runaways), the safety disk breaks and the pressure is released. This usually
prevents the pressure vessels from rupture.
Safety disk
Safety disk holder
Screw cap
Fig. 4 - 6 Screw cap (Rotor 16), safety disk and safety disk holder
• Use of special vessel jackets
The vessel jacket serves as a mechanical protection. Depending on the required

pressure stability, the vessel jacket is either made of PEEK (for operating
pressures up to 20 bar) or ceramics (for operating pressures up to 60 bar). The
quartz glass vessels for Rotor 8S (for operating pressures up to 80 bar) are vessel
jacket as well as reaction vessels; they are inserted directly into the protective
casing.
• Effective rotor design
The rotor surrounds the vessels and has been designed to ensure that the
microwave cavity is well protected in the case of safety disk or vessel rupture.
• Special construction of the instrument door
The instrument door is locked by means of a mechanical interlock. To unlock and

open the door, press the door opener button at the top of the instrument cover.
C49IB08A 24
Fig. 4 - 7 Door opener button
Permanent magnets effectively support the opening and closing mechanism of

the door. The instrument door is equipped with two strong safety hooks that allow
the door to open only a little slit.
In the case of overpressure in the microwave cavity the door is opened slightly to
release the overpressure and immediately closed by the magnets.
Safety hooks
Fig. 4 - 8 Instrument door with safety hooks
• Effective safety cooling
The safety cooling cools down the hot, pressurized vessels and exhausts any
reaction products that have escaped after the rupture of a safety disk or vessel.
The safety cooling system is activated:
• after termination of a program

• when starting up Synthos 3000 again after an interrupted reaction program
(e.g. due to a power failure)
• if the pressure increase rate has exceeded 3.0 bar/s
• if no cooling step has been programmed
C49IB08A 25
• Temperature sensor "magnetron"
Temperature sensors are assembled on each of the two magnetrons (microwave

generators). If overheating occurs, the magnetrons are shut down.
• Temperature sensor "exhaust unit"
This temperature sensor is directly built into the exhaust unit and protects it
against thermal overload.
• Temperature sensor "exhaust air"
This sensor detects the temperature of the exhaust air. If the temperature of the
exhaust air exceeds 130°C both microwave energy and cooling are switched off
and a fire alarm is shown on the display.
4.3.5 Cooling and Exhaust
Synthos 3000 includes an "exhaust unit" that is programmable in four intensity

steps and permanently carries off the reaction heat during the reaction in order to
reduce the thermal stress on the used materials.
Due to the permanent cooling during the process, a temperature gradient is built
up in the vessel which leads to strong convection behavior and constant
exchange between the liquid and the gaseous phase.
Any gases which may escape during the reaction are withdrawn by the exhaust
system.
After completion of reaction the vessels are automatically cooled down below an
appropriate temperature limit.
C49IB08A 26
Fig. 4 - 9 Integrated cooling unit
4.3.6 Rotor Detection
Modern sensor technologies are an indispensable part of powerful, innovative

instruments, such as Synthos 3000. The more accurate information about
physical parameters is provided, the more successful demanding technical
processes can be controlled. A wide range of additional sensors is available for
improved, reliable results and higher operational safety.
The standard version of Synthos 3000 includes optical sensors which are located
in the microwave cavity of the instrument:
• Position and protection lid recognition
A sensor located in the base of the oven cavity sends an infrared light beam onto
the bottom plate of the rotor. The bottom plate reflects the beam to the sensor,
which is electronically analyzed. The following information and/or functions are
processed:
• Automatic detection of the rotor type

This feature rules out errors caused by improper handling/operation.
• Monitoring the revolution of the rotor

This feature monitors the rotor's revolution (RPM revolution per minute),
which is important for uniform microwave heating. Local overheating is
avoided and the risk of spontaneous reactions is minimized.
C49IB08A 27
• Exact position detection

This function assigns the temperature measured by the IR sensor to
each pressure vessel. In this way, the temperature course of each
vessel can be followed and displayed.
• Rotor lid detection

A sensor located on the right inner wall of the microwave cavity sends
an infrared light beam to the rotor lid and (via a reflecting surface) back
to the sensor. This function prevents an inadvertent start of the reaction
program without the rotor lid (which is an indispensable safety
requirement).
Rotor lid detection
IR sensor
Position and rotor detection
Fig. 4 - 10 Rotor sensors
C49IB08A 28
Reflecting surfaces Light beam Reflection Rotor surface
Microwave cavity
Sensor Evaluation
Electrical Signal
Fig. 4 - 11 Working principle of the rotor sensors
C49IB08A 29
4.4 Technical Description of the IR Temperature

Sensor Accessory
The infrared sensor measures the temperature at the base surface of each
reaction vessel. Measured temperature values are assigned and recorded to the
corresponding vessel via the automatic position recognition. The temperature
measurement protects against overheating.
As the measurements are taken through a Fresnel lens on the bottom of the
microwave cavity, make sure that this Fresnel lens is always kept clean.
Reaction vessel
IR radiation Fresnel lens

Electronic
IR sensor module
Fig. 4 - 12 IR temperature sensor - working principle
Temperature measuring range 20 - 400 °C
For checking and calibrating the IR sensor see Chapter 6.7.9 or Chapter 6.7.10
and Chapter 6.7.11 or Chapter 6.7.12.
Important:
The IR sensor has to be checked (and recalibrated, if necessary) at least
once a year.
C49IB08A 30
4.5 Technical Description of the Pressure /

Temperature Sensor Accessory
This description applies for both, p/T sensor accessory for Rotor 16 and p/T
sensor accessory M50 for Rotor 48. These tools are optional, but recommended
to be used for optimum reaction control.
Electronics Receiver
Knurled nut
Fig. 4 - 13 Pressure / Temperature sensor - schematic description
C49IB08A 31
Thermometer Capillary
Immersion Tube
Vent Pipe
Seal
Seal Husk
Fig. 4 - 14 Pressure/Temperature Sensor M50 (Rotor 48)
Gas bulb thermometer with PEEK protection

capillary tube
Syringe connector
with O-ring
Venting screw
Immersion tube
Seal holder
Seal
Safety disk holder Seal husk
Safety disk M&H
Fig. 4 - 15 Pressure / Temperature Sensor Accessory (Rotor 16)
C49IB08A 32
4.5.1 Pressure Measurement
A hydraulic piston is installed in the sensor head above the seal of the reference
vessel. This piston takes up the reaction pressure via the seal and the seal holder.
The hydraulic system transfers the pressure of the reference vessel to the sensor
module, where it is measured continuously during the reaction and transferred
wireless (via IR) to the control electronics for the following purposes:
• Display and storage of the pressure graph

The pressure of the reference vessel can be displayed on the graphic display
during and after the reaction program (via the Review dialog). Values and
graph can be printed out for documenting purposes or sent to an external PC
after completion of the reaction run.
• Hardware monitoring of the pressure increase rate

The sensor head of the p/T sensor accessory includes a special
microprocessor for software-independent monitoring of the pressure rate. As
soon as the pressure increase rate reaches 3.0 bar/s or higher, the
electronic module responds as follows:
• Microwave generation will be completely shut down for a least 3 seconds.

• The cooling intensity of the exhaust unit will be increased temporarily to
level 3; (for max. 120 seconds, or until the pressure rate shows a negative
value for a defined period of time).
• After reaching normal pressure rate values the microwave power is
gradually increased until it has reached the default value.
• A pop-up message informs the customer about the pressure increase rate.
• Software-controlled pressure increase rate monitoring

During a reaction run, the software monitors the pressure increase rate in the
vessel. As soon as the pressure increase rate limit (selectable in the
method between 0.1 - 3.0 bar/s) has been reached or exceeded the
instrument responds as follows:
• If the pressure increase rate is 0.1 - 0.2 bar/s below the limit, the microwave
power is reduced.
• If the pressure increase rate limit is reached, the microwave power will be
cut off until the pressure rate is below the selected limit value; thereafter it
will gradually increase again.
• If, after cutting off the microwave power, the pressure limit has NOT fallen
below the limit value within 2 seconds, the intensity of the exhaust unit will
be increased to its highest level (level 3).
C49IB08A 33
• Control of pressure limit
• If the pressure exceeds the limit (20 bar for MF50 and HF100 and 40 bar
for HF100) by more than 5 bar as a result of a spontaneous reaction, the
experiment will be terminated. In this case the vessels and seals must be
cleaned and checked very carefully for signs of damage.
Pressure measuring range 0-86 bar
Accuracy ± 0.2 bar
4.5.2 Temperature Measurement
Important:
After (accidentally or on purpose) opening of the conical seal of the capillary
tube (knurled nut on the pressure sensor unit), the temperature sensor has to
be re-calibrated.
A hermetically sealed glass bulb is filled with gas. The gas in the bulb expands
with increased temperature during the reaction. This gas expansion causes an
increased pressure which is transferred to the pressure sensor via a capillary. The
pressure increase is converted to a corresponding temperature value. This
temperature value of the reference vessel is transmitted to the electronics module
and from there wireless (via IR) to the microwave oven. The temperature is
displayed graphically on the LCD as a “temperature over time” graph or as a
numeric value.
Using the optional calibration unit the immersion thermometer can be calibrated
to an accuracy of ± 1% within a measuring range of 0 to 280°C. (Refer to chapter
6.7.4, "Temperature Sensor Calibration with the Calibration Accessory" or chapter
6.7.5, "Temperature Sensor Calibration with the Calibration Unit".
Hint:
Calibration has to be done once a year, although it is recommended to
calibrate the temperature sensor at least twice a year.
Each p/T Sensor Accessory is shipped with a unique serial number that is printed
on an adhesive label and stored in the sensor electronics.
Synthos 3000 uses this information to identify the appropriate p/T Sensor
Accessory and to assign the correct calibration factors.
C49IB08A 34
Control of temperature limit
• If the temperature exceeds the limit (200 °C for MF50, 190 °C for MF100
and 240 °C for HF100) by more than 5 °C as a result of a spontaneous
reaction, the reaction run will be terminated. In this case the vessels and
seals must be cleaned and checked very carefully for signs of damage.
Temperature measuring range 0 - 280°C
Accuracy within a range of 0 - 200°C ± 1%
C49IB08A 35
4.6 Technical Description of the T-Probe
Hint:
The T-probe unit of Rotor 8S can be used for both pressure vessel types,
XF100 and XQ80 and is used together with immersion tube with seal XF or
immersion tube with seal XQ.
This optional accessory can be easily installed by the customer and it is
recommended to use for optimum reaction control
Safety disk holder Syringe connector with O-Ring
Safety disk X Venting screw
Seal XQ or XF
Seal husk
Immersion tube
Knurled nut
Fixing screw
Capillary
T-probe
Fig. 4 - 16 T-probe S and corresponding immersion tube
C49IB08A 36
4.6.1 Temperature Measurement
Important:
After (accidentally or on purpose) opening of the conical seal of the capillary
tube (knurled nut on the pressure sensor unit), the temperature sensor has to
be re-calibrated.
A hermetically sealed glass bulb is filled with gas. The gas in the bulb expands
with increased temperature during the reaction. This gas expansion causes an
increased pressure, which is transferred to the pressure sensor via a capillary.
The pressure increase is converted to a corresponding temperature value. This
temperature value of the reference vessel is transmitted to the electronics module
and from there wireless (via IR) to the microwave oven. The temperature is
displayed graphically on the LCD as a “temperature over time” graph or as a
numeric value.
Using the optional calibration unit the immersion thermometer can be calibrated
to an accuracy of ± 1% within a measuring range of 0 to 300 °C. Refer to chapter
6.7.4, "Temperature Sensor Calibration with the Calibration Accessory" or chapter
Hint:
Calibration has to be done once a year, although it is recommended to
calibrate the temperature sensor at least twice a year.
Each T-probe accessory is shipped with a unique serial number that is printed on
an adhesive label and stored in the sensor electronics.
Synthos 3000 uses this information to identify the appropriate T-probe accessory
and to assign the correct calibration factors.
• Control of temperature limit
• If the temperature exceeds the limit (260 °C for XF100 and 300 °C for
XQ80) by more than 5 °C as a result of a spontaneous reaction, the
reaction run will be terminated. In this case the vessels and seals must be
cleaned and checked very carefully for signs of damage.
Temperature measuring range 0 - 300°C
Accuracy within a range of 0 - 200°C ± 1%
C49IB08A 37
4.7 Technical Description of the Safety Module

SOLV
The safety module SOLV is a hardware accessory for Synthos 3000, which is
mandatory for safe operation using organic solvents.
It consists of mainly two membrane switches, which monitor the exhaust airflow
through the cavity in order to prevent the formation of dangerous concentrations
of solvent vapors inside the system. In case that the airflow is interrupted (e.g.
failure of the exhaust fan, blocking of the exhaust system), microwave power is
switched off immediately and the current run is interrupted.
The safety module SOLV is installed underneath the cavity, therefore later
upgrades in the field have to be done by authorized service engineers only.
C49IB08A 38
4.8 Technical Description of the Solvent Sensor

Accessory
Fig. 4 - 17 Solvent sensor accessory
The optional solvent sensor monitors the concentration of organic solvents in the
exhaust air channel of Synthos 3000. The sensor element is a metal oxide
semiconductor detector that changes resistance in correlation to the gas
concentration.
The factory-calibrated Solvent Sensor Accessory is mounted instead of the cover

on the exhaust channel at the rear side of the oven. It is electrically connected to
the "AUX" port. Use the latest software version to monitor the solvent
concentration and to trigger alarm functions, like increasing the speed of the
exhaust fan. The solvent sensor is not required for instrumental safety. This is
provided by the mandatory Safety Module SOLV.
4.8.1 Installation
Important:
Take care that Synthos 3000 is switched off before installing the Solvent
Sensor Accessory!
The Solvent Sensor Accessory measures the solvent concentration inside the
cavity, but it is not required for safe use of the instrument like the obligatory
Safety Module SOLV (SMS).
4.8.1.1 To Install the Solvent Sensor Accessory
1. Remove the safety bracket and the cover from the exhaust channel at the
rear of Synthos 3000 by loosening the two nuts.
2. Plug the sensor into the exhaust channel. The cable has to point to the left.
C49IB08A 39
3. Reassemble the safety bracket on the exhaust channel and fasten it with the
two nuts.
4. Attach the connector to the “AUX” port of the instrument and fix it with the
two screws for proper connection.
Sensor
Fig. 4 - 18 Installing the Solvent Sensor Accessory
cable
Fig. 4 - 19 Serial number label to mark the cable
C49IB08A 40
4.8.2 Function Verification
The function verification is only used for testing the sensor. For the function
verification you will need acetone and a 1 or 1.5 L bottle (any material), which can
be closed with a screw cap.
4.8.2.1 To Verify the Function
1. Check if the Solvent Sensor Accessory is installed and connected to the

instrument.
2. Switch on the instrument and wait until the Solvent Sensor Accessory has
reached a minimum temperature of 36 °C.
3. Open the Service - solvent sensor setting dialogue.
Fig. 4 - 20 Service - Solvent sensor settings
4. Check if the calibration constant is entered (available from the calibration

certificate or determined by performing the user calibration).
5. The "Value" is proportional to the measured solvent concentration in the

exhaust channel.
6. Open the door of Synthos 3000.
7. Remove the turn table and driving star.
8. Press <Fan 1 F4 > for the test mode. The exhaust unit is set to level 1.
9. Fill acetone into the bottle (0.5 mL acetone per 1L bottle volume). Close the
bottle with the screw cap and shake it for at least 30 seconds.
10. Hold the bottle upside down onto the exhaust holes in the cavity and open
the screw cap.
11. The signal on the display should reach a minimum value of 1000-1500. If
not, contact your local customer service.
C49IB08A 41
4.8.2.2 To Calibrate the Solvent Sensor Accessory
Important:
Calibration of the Solvent Sensor Accessory has to be done regularly.
Warning:
when handling solvents and observe the relevant national regulations.
For calibration of the Solvent Sensor Accessory it has to be put on a volumetric

flask. During the calibration in a volumetric flask the solvent sensor will be tested
in a standardized atmosphere to determine the sensitivity of the sensor during
use. After applying a certain amount of solvent, the signal of the sensor can be
stored as the new calibration factor.
Tools required for calibration:
- measuring cylinder (volume: approx. 1L, diameter: > 7 cm)

- solvent for calibration (acetone, hexane or methanol)
- solvent syringe (volume: 0.1 - 0.25 mL)
- adhesive tape
1. Switch off the instrument.
2. Remove the sensor in reverse order to the installation procedure. Refer to

chapter 4.8.1.1, "To Install the Solvent Sensor Accessory".
3. Connect the Solvent Sensor Accessory to the AUX port of Synthos 3000.
Cable of the Solvent

Sensor Accessory
Fig. 4 - 21 Connecting the Solvent Sensor Accessory to Synthos 3000
4. Switch on the instrument.
5. Use the arrow keys <Ï F4> and <Ð F5> to select the solvent sensor
settings menu in the service menu. Confirm by pressing <Enter F1>.
C49IB08A 42
6. Wait until the Solvent Sensor Accessory has reached a minimum

temperature of 36 °.
7. Close the measuring cylinder with the Solvent Sensor Accessory.
Fig. 4 - 22 Solvent sensor on a measuring cylinder
8. Use an adhesive tape for sealing. Take care for proper sealing.
Fig. 4 - 23 Sealing with an adhesive tape
9. Depending on your application inject one of the following solvents into the
measuring cylinder (through the adhesive tape):
• n-Hexane: 32 μL for 50 % lower explosion limit

• methanol/acetone: 56 μL for 50 % lower explosion limit
C49IB08A 43
n-Hexan or
Methanol/acetone
Fig. 4 - 24 Injecting the solvent
10. Shake the measuring cylinder and read out the highest signal value on the
display of the instrument.
Signal value
Fig. 4 - 25 Service - Solvent sensor settings
11. Remove the sensor from the measuring cylinder and vent the flask by
purging with an air stream.
12. Repeat these steps 2 times and enter the average value into the instrument
as your new "Calib. Constant".
13. A variation of the signal of +/- 200 between the different trials is within the
specified operation limits. If the limits excess the variation of +/- 200, contact
your local customer service.
C49IB08A 44
4.9 Technical Description of the Magnetic Stirrer

Device
Fig. 4 - 26 Magnetic stirrer device
The magnetic stirrer device is a useful tool for mixing the contents of the closed
reaction vessels inside Synthos 3000. Depending on the application, stirring
helps to obtain better recoveries or to attenuate spontaneous reactions by
avoiding local inhomogeneity inside the vessels.
The magnetic stirrer device is installed underneath the cavity and consists of
three plates with strong permanent magnets, which drive the magnetic stir bars
inside the reaction vessels.
Different rotation speeds (200, 400 and 600 rpm) are selected and controlled via
the software.
C49IB08A 45
5 Installation
5 Installation
The following chapter explains the requirements and the steps to be performed
for a successful installation of Synthos 3000.
5.1 Installation Requirements
5.1.1 Exhaust System
Important:
A reliable exhaust system with sufficient capacity (min. 300 m³/h) must be
provided when operating Synthos 3000.
Hazardous and noxious gases may build up if an appropriate and working
exhaust system is not provided at the place of installation. Synthos 3000 must
not be set in operation in this case.
Synthos 3000 must be installed in an operating fume hood and following

enquiries have to be fulfilled:
• Provide easy access to the instrument, especially to the connection ports on

the right hand side.
• A clean surface or workbench should be available next to the instrument for

manipulating the rotors.
• Provide sufficient clearance (10 cm) between the instruments side panel and
rear panel, respectively, and the laboratory walls for satisfactory circulation
of the cooling air.
• The exhaust tube must be routed with a sufficient bending tolerance to

prevent it from being squeezed or kinked.
• The utilized fume hood must be operating and switched on during the
experiments to withdraw vapors and gases, especially after venting actions.
• No reagents or samples should be placed on top or right next to the

instrument.
• The surrounding environment of the instrument must be kept scrupulously

clean.
• Any spills of chemicals, solvents, etc. must be removed IMMEDIATELY using

appropriate equipment.
• The valid Laboratory Safety Regulations and Occupational Safety

Regulations must be observed.
C49IB08A 46
5 Installation
5.1.2 Electrical Requirements
Warning:
Synthos 3000 must be connected ONLY to an approved standard socket with
protective conductor!
Before plugging in the cable, always make sure that the local mains supply
and frequency correspond to the values on the type plate of the instrument.
Synthos 3000 requires a constant supply of electrical current, corresponding to

the values listed below. The power supply must meet the local safety regulations.
Mains supply AC 230 V ± 10 %
Frequency 50 Hz ± 0.3 Hz or 60 Hz ± 0.3 Hz
Line protection (fuse) at least 16 A (USA and Canada: at least

20 A); tripping characteristics type "C",
according to IEC 898
Current supply at least 16 A (USA and Canada: at least

20 A); tripping characteristics type "C",
according to IEC 898
The rating of each Synthos 3000 instrument (voltage and frequency) is

printed on the type plate on the rear side of the instrument.
The instrument is delivered with an appropriate mains cable.
50 Hz instruments 2.5 meter, line power cable with CEE plug,

IEC 309 250 V, 16/20 A, 2-pole,
plus protective earth
60 Hz instruments 2.5 meter, line power cable with NEMA L6-

20R Twistlock plug, 208-240 V,
60 Hz, 20 A, 2-pole, plus protective earth
If your laboratory is equipped with another plug system, you have to provide a
suitable and approved connection cable.
C49IB08A 47
5 Installation
5.2 Installation Steps
For detailed information follow the instructions given on the video manual on CD.
1. Unpack Synthos 3000 and inspect it for possible signs of damage in transit.
Important:
Keep the packing material for transporting the instrument at a later time
(change of location, repair, upgrade etc).
2. Make sure that the door can be closed properly and the sealing surfaces of
the door are not damaged.
Warning:
Never operate Synthos 3000 if the door is damaged!
In this case the function of the safety features can no longer be guaranteed
and harmful microwave radiation may escape.
3. If the instrument has been transported at low temperatures (e.g. in winter),

please allow it to adjust to room temperature before switching it on!
4. Check if the voltage and frequency are in accordance with the ratings on the
instrument label.
Important:
When lifting Synthos 3000, only hold it by the outer edges of the base.
Never lift Synthos 3000 by the instrument door.
Never transport Synthos 3000 with a rotor inserted.
5. Check the proper installation of the foam seal between tube and exhaust
unit.
Fig. 5 - 1 Checking the proper installation of the foam seal
C49IB08A 48
5 Installation
6. Connect the exhaust hose to the exhaust unit by attaching it to the

connecting flange, which is located on the rear side of the instrument. Fix it
with the clamp. The foam piece in the exhaust hose reduces the noise
and should be positioned in the hose as shown in Fig. 5 - 2.
Fig. 5 - 2 Twisted foam for noise reduction in the exhaust hose
7. Lead the open end of the exhaust hose into an exhaust system or fume
hood. Make sure that there is a bypass between the hose of Synthos 3000
and the exhaust system.
Incorrect installation Correct installation
Fig. 5 - 3 Connection of the exhaust hose to an exhaust system
Warning:
Never run the system without the exhaust hose.
8. Check if the plug of the exhaust unit has been inserted properly into the
appropriate socket.
9. Connect the mains cable.

The socket is located on the rear side of the instrument.
10. Insert the mains cable plug into the wall socket.
Synthos 3000 has to be connected to an approved standard wall socket with
a ground conductor.
C49IB08A 49
5 Installation
11. Switch on the mains switch of Synthos 3000.

The mains switch is located at the front below the instrument door.
12. Adjust the view angle of the LCD after the software has started automatically.
The knob is marked "VIEW ANGLE" and located on the upper right-hand
side of Synthos 3000.
By turning the knob you can adjust the LCD for optimum readability.
13. Rotors and accessories of Synthos 3000 have to be activated and

configured via the software before use. For detailed information read chapter
"Software" in this reference manual.
C49IB08A 50
5 Installation
5.3 Connecting Accessories
5.3.1 Printer
Reaction data can be printed for documentation. All printer models with an
installed ASCII character set are suitable for printing text documents (without
graphs).
If you wish to print text and graphs, e.g. pressure / temperature curves, you may
connect any compatible printer. The printer port is located on the right side of the
instrument and marked "PRINTER".
5.3.2 Keyboard
An alphanumeric keyboard can be connected to Synthos 3000. This keyboard

allows you to edit methods and enter new ones. The appropriate port is marked
with "KEYB" and located on the right side of the instrument.
5.3.3 External Computer
Reaction data can be transferred to an external PC via a serial interface. The port
"COM1" is provided on the right side of the instrument. This RS232 interface is an
SELV (safety extra-low voltage) circuit that can only be connected to other SELV
or SELV-E circuits. Only use shielded cables with a length of less than 3 m for this
connection.
A standard terminal program can be used to store the run data as text file on an
optionally computer.
The free Excel Add-in "AP-Softprint for Synthos 3000" (available at AP-Website)
can be used to import the run data directly into a MS-Excel sheet, which simplifies
both, data collection and diagram generation.
For connection to a PC / notebook without serial interface, a serial-to-USB

converter is available.
C49IB08A 51
5 Installation
5.4 Activating / Deactivating Rotors, Sensors and

Accessories
Prior to the first reaction with Synthos 3000, proper instrument settings have to be
checked and the appropriate rotor types and accessories have to be activated in
the setup menu.
Hint:
All rotors, sensors and accessories for Synthos 3000 which are added or put
into operation must be activated and configured before first use.
You can also deactivate rotors, sensors or accessories which are no longer
required.
Starting from the main menu, press <Setup F3> to reach the setup menu.
The setup menu is used to change instrument settings. The arrow keys <Ï F4>
and <Ð F5> are used to select the desired options from the setup menu, which
are subsequently confirmed with <Enter F1>.
Fig. 5 - 4 Setup - menu
Refer to chapter 6.6, "Setting Up the Instrument".
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5.5 Microwave Power Calibration
The purpose of this calibration procedure is to adjust the microwave power

parameters to ensure accurate values for the applied power output.
Hint:
Microwave power must be calibrated before the first reaction and can be
repeated at periodical intervals.
Calibrate the microwave power at 800 W maximum as described below.
Required material:
• Immersion thermometer with a resolution of 0.1 °C

• Balance with a weighing capacity of at least 1000 g water in for example a
1 L volumetric flask.
• 1 L glass beaker with a diameter of approx. 180 mm
• Tap water (temperature approx. 20 °C)
The calibration is based on the knowledge of the specific heat capacity of water.
By heating up a certain amount of water with microwave energy, the apparent
power can be calculated from the water volume, the temperature of the water
before and after heating.
The power calibration consists of the following steps which are carried out
automatically by the software:
- Determining the apparent power output of the microwave generators

- Calculating a power factor
The list below is a short description of the power calibration procedure:
1. Switch on Synthos 3000.
2. Press <Service F4> to select the service menu.
3. Press <Ð F5> to select the power calibration option. Confirm by pressing
<Enter F1>.
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Fig. 5 - 5 Service - Power calibration
4. Fill 1000 g of tap water (approx. 20 °C) into a beaker (diameter approx.
180 mm).
5. Check if the amount of water in the beaker corresponds to the value shown
on the LCD. Possible deviations can be corrected by pressing <+ F2> or <-
F3>. Press <Next F4>.
Fig. 5 - 6 Power calibration - Entering mass of water
6. Select the target microwave power for the calibration. The recommended
power is 800 W. Changes can be entered via <+ F2> or <- F3>. Press <Next
F4>.
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Fig. 5 - 7 Power calibration - Selecting the target microwave power
7. Measure the temperature of the water. Use the <+ F2> or <- F3> key to enter
the measured temperature value, then press <Next F4>.
Fig. 5 - 8 Power calibration - Entering the temperature of the water
8. Open the door of Synthos 3000 and place the beaker on the turntable. Close
the door.
Fig. 5 - 9 Power calibration - Start heating for calibration
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9. Press the green <START> button and wait until the heating time (80 seconds
for 800 W) has elapsed. You can terminate the procedure at any time by
pressing the red <STOP> key.
Fig. 5 - 10 Power calibration - Heating up
10. After the time has elapsed and the red LED on the front panel has switched
off, the next menu step is displayed. Open the instrument door and remove
the beaker. Measure the water temperature with an immersion thermometer
while stirring (homogenizing) the water thoroughly. Enter the final water
temperature via <+ F2> or <- F3> and press the <Next F4> key.
Fig. 5 - 11 Power calibration - Measuring the temperature of the water
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Fig. 5 - 12 Power calibration - Entering the water temperature
The microwave power factor will now be calculated and displayed.
Fig. 5 - 13 Power calibration - Saving the power factor
11. Press <Save F1> to store the new power factor. Press <Repeat F4> to
repeat the power calibration once again. Press <Print F5> if you want to
print out the calculation for documentation purposes.
If the calculated power ratio is out of range (v1.52 or lower: 0.8 - 1.2; v2.0 or
higher: 0.7 - 1.3) saving is not possible.
In this case enter either 0.8 (if the power ratio was below 0.8) or 1.2 (if the
power ratio was above 1.2), press <Save F1> and repeat the calibration
procedure with the new settings (<Repeat F4>).
Press <ESC> to exit without any changes.
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6 Software
6.1 General Information
Synthos 3000 is a software-controlled instrument. Entry of program settings or

selection of various instrument parameters are easily done via softkeys on the
keypad. Information is provided via the graphic display. All operating elements are
integrated in the front panel of Synthos 3000. An external keyboard can be
connected to facilitate entry of alphanumerical data.
A hierarchical menu structure ensures convenient use of the software and easy
instrument operation.
The software starts automatically after switching on the instrument.
Hint:
Periodically check the Anton Paar website (www.anton-paar.com) for software
updates or contact our local distributor.
Install the updated software version according to chapter 6.7.1, "Software
Update".
The most important software features are:
• Fast and logical guidance through menu commands

• Multilingual user interface (v2.0 or higher)
• Display of all relevant reaction parameters as numeric data and graphs:
- Programmed and actually applied microwave power
- Individual IR temperatures of reaction vessels
- Internal temperature of the reference vessel
- Pressure measurement either inside the reference vessel (Rotor 16 and
Rotor 48) or simultaneously in all vessels (Rotor 8)
• Pressure rate monitoring
• Automatic reduction of the microwave power if preset limits are reached
(pressure, temperature, pressure increase rate)
• Method library which can be extended as required
• Automatic control of the exhaust unit (safety cooling)
• Documentation of process data via external PC or an optional printer
• Software-assisted calibration of microwave power and optionally available
sensors
• Service and maintenance programs
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The keypad consists of the following keys:
• 5 softkeys (F1 - F5)

Depending on the menu command, these keys have different functions. The
currently active function is shown on the display next to the key.
• ESC key
The <ESC> key is used to terminate a process and/or move back one step in
the menu hierarchy.
• Start button
The green <Start> button is used to start a selected method.
• Stop button
The red <Stop> button is used to interrupt or stop a microwave program.
Softkeys Keypad with signal lamp
Current software Assigned functions Start/Stop keys

version for softkeys
Fig. 6 - 1 Operating elements of the Synthos 3000 keypad
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6.2 Basic Software Structure
START
Fig. 6 - 2 Basic software structure
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6.3 The Main Menu
The main menu appears automatically after switching on the instrument. The
installed software version is shown in the lower left corner of the graphic display.
Fig. 6 - 3 Main menu
The following sections of the program or submenus are accessible via the
function keys:
• F1 Library
Allows you to select and modify methods or to create new methods. New or
modified methods can be saved for future use. Comments can be added to
the methods.
• F2 Review
For viewing and/or printing the stored process data as tables and diagrams
(power vs. time, temperature vs. time and pressure vs. time). The available
diagrams depend on the sensors used. The stored data can also be sent to
an external PC.
• F3 Setup
This key accesses a submenu containing different instrument settings.
• F4 Service
This key accesses a submenu containing maintenance and service
programs.
• F5 Info
Shows telephone number, fax number and contact e-mail address of
Anton Paar GmbH as well as the serial number of the instrument and the
usage information (v2.0 or higher).
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6.4 Library Menu
Starting from the main menu, press <Library F1> to reach the library menu.
Fig. 6 - 4 Library menu
The library menu is used to load stored methods and to create or edit methods
using the method editor.
The library menu consists of three areas:

• A list of the last four methods used ("Last")
This list is intended for routine operation, i.e. it provides fast retrieval and
access to frequently used methods.
• "Make New Sample" for creating new methods
• A method library in alphabetical order ("Library")

This list shows only methods stored for the activated rotors. (Refer to
chapter 6.6.5, "Rotors".)
To select a method use the arrow keys <Ï F4> or <Ð F5> and <Í F2> or
<ÎF3> and confirm your choice by pressing the <Enter F1> key.
To jump directly between these areas, use the arrow keys <Í F2> or <ÎF3>.
For various sample materials there may exist several methods using different
rotor types. Make sure to select the appropriate method for the rotor used. After
selecting a method, the sample menu will be opened.
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6.4.1 Sample Menu
Fig. 6 - 5 Sample menu
The program allows you to select the following functions:
• Start
Starts the selected method displayed in the sample menu.
• Edit
Edits the selected method displayed in the sample menu.
• Notes
This option is used to enter a comment or additional information. A flashing
notes field indicates information stored for this method.
• Spl Doc (Sample Documentation)

Use this option to enter additional information for each individual reaction
vessel. This information is visible during the run and stored in the run-data
only, BUT NOT in the method.
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6.4.1.1 Start
Biginelli
Fig. 6 - 6 Sample menu - Start
By pressing <Start F1> a startup routine is activated, which checks presence and
type of rotor in the microwave cavity and verifies whether the rotor has been
closed with the protection lid or not.
If optional sensors have been installed (e.g. a p/T sensor) and properly configured
in the instrument setup, the function of these sensors will also be checked.
If an error is detected during the testing procedure, an error message is shown

and the method start will be interrupted.
If no errors have been detected, the method can be started by pressing the green
<Start> button.
6.4.1.2 Edit
Depending on the installed rotors and accessories (sensor etc.), the actual
sample menu might look different.
Fig. 6 - 7 Sample menu - Edit
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• Press <+ F2> and <– F3> to create or change information or parameters for
a method. You can use them to enter characters, select options and
increase / decrease numerical values.
• The arrow keys <Í F4> and <Î F5> are used to jump between the entry
fields.
• Press <Exit F1> to exit the editing dialogue and select one of the following
options from the pop-up window:
- Save:
Press <Save F1> to save your changes by overwriting the (existing)
version. This function can be deactivated by locking the method in the
library maintenance tool (refer to chapter 6.7.15, "Library Maintenance
Tool").
- New:
Press <New F2> to store as a new method, the existing one remains
unchanged.
- Discard:
Press <Discard F3> to cancel your changes.
- Delete:
Press <Delete F4> if you wish to delete the method. This function can be
deactivated by locking the method in the library maintenance tool (refer to
chapter 6.7.15, "Library Maintenance Tool").
Explanation of the entry fields:
• Sample
This field is used to enter a sample name consisting of max. 23 characters
but only 18 will be shown in the library.
• Rotor
This field is used to select the rotor type you are going to work with.
Deactivated rotors are not displayed and therefore not selectable.
Hint:
After selecting the appropriate rotor type, the pressure and temperature limits
will be changed automatically.
Important:
The HEAT rotor type enables an operating mode that is exclusively for
testing purposes (e.g. for service).
Misuse of these instructions may result in damage to the Synthos 3000.
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• Vessels
This field is used to enter the number of vessels applied in the rotor.
Please follow the recommended loading patterns according to the respective
rotor type. Never use less than 4 vessels!
• Weight
This field is used to enter the weight of your sample material.
• P-Program / T-Program
Depending on the type of rotors and sensors, this field can be used to select
a power or temperature program:
- P-Program:
When using a P-program (power program), the instrument follows a
defined power profile and only deviates from this profile when limits such
as pressure, pressure increase rate or temperature are exceeded.
- T-Program:
When using a T-program (temperature program), the instrument follows a
defined temperature profile and only deviates from this profile when limits
such as pressure, pressure increase rate or temperature are exceeded.
Hint:
It is highly recommended always to use an immersing temperature sensor,
even when a power program is performed.
• Ph
This field indicates the "Phase“ or step of the power / temperature profile.
• Power / Temp
Power / temperature setpoint at the end of the ramp time.
• Ramp
Time period in which the previously defined power / temperature setpoint has
to be reached. Possible range 00:00 to 99:59 [minutes: seconds].
• Hold
Time period wherein the defined power / temperature setpoint has to be
held. Possible range: 00:00 to 99:59 [minutes: seconds].
Fan
This field is used for setting the intensity of the exhaust unit:
- Level 0: minimum intensity (special applications)
- Level 1: low intensity (used during heating)
- Level 2: medium intensity (for cooling)
- Level 3: highest intensity (for cooling)
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• p-rate
The limit of the pressure increase rate is entered in this field. The possible
range is between 0.1 - 3.0 bar/s.
If the pressure rate exceeds the predefined limit, the microwave generation
will be interrupted for a short period of time.
• IR
This field is used to enter the IR temperature limit.
• p
This field is used to enter the pressure limit for power controlled runs.
• P
This field is used to enter the power limit for temperature controlled runs.
• Drive
This field is used to chose the rotor drive mode.
Rot.: Constant rotation
Osc: Oscillation
• Stirrer
This field is used for setting the intensity of the stirrer unit in a range of 0 - 3.
Off: The magnetic stirrer is switched off.
1, 2 or 3: The magnetic stirrer rotates at varying speeds.
6.4.1.3 Notes
You can enter additional information or notes related to the method in the Notes
Editor. The following functions are available:
• Start F1
This function is used to start the method directly without going back to the
primary menu.
• Edit F2
This function is used to change existing information or to enter new ones
with the alphanumeric keyboard.
Leave the Edit mode by pressing the <Exit F1>.
• Sample F3
The <Sample F3> key will bring you back to the Sample menu.
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6.4.1.4 Spl Doc (Sample Documentation)
The sample documentation editor can be used to enter additional information with
the alphanumeric keyboard.
The following functions are available:
• Start F1
This function is used to start the method directly without going back to the
primary menu.
• Sample F4
The <Sample F4> key brings you back to the sample menu.
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6.5 Review
Starting from the main menu, press <Review F2> to reach the review menu. Run
data such as temperature and pressure values are stored automatically during
each process. Depending on the number of stored methods, the data of the last
4-8 hours of operation will be available under the review menu option.
Fig. 6 - 8 Review menu
The list is sorted by date / time and offers the following options:
• Enter F1
Press <Enter F1> to view the data of the run on the display. Depending on
the type of sensors used, you can select different displays.
• Send
Press <Send F2> to send the data of the selected run to an external PC
connected to Synthos 3000 via the serial interface.
• Print
Press <Print F3> to print the selected data on a connected printer.
Use the arrow keys <Ï F4>, <Ð F5> to select a stored run.
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6.5.1 Review - Displayed Diagrams
6.5.1.1 Review - Numeric
This screen provides an overview (text based) of all maximum values reached
during a run.
Max. applied power Max. pressure Max. inner temperature or

max. applied power
Sample/
Method
:
QQ

T$5DgF#ODU

ODU
%ODU&f
Max. IR temperatures assigned to

Program duration each vessel
Fig. 6 - 9 Review - Numeric
Explanation of the data:
• Power
The max. microwave power [W] which was applied during the run. The
applied power may deviate from the maximum power set point defined in the
method e.g. if the temperature or pressure limit was reached or the permitted
pressure rate was exceeded.
• Temp
Maximum inner temperature which was reached in the reference vessel.
• Pres
Maximum pressure which was reached during the reaction.
• IR
Maximum IR temperatures of reaction vessels and empty positions,
respectively.
• IR Lim
Temperature limit defined in the method for the IR temperature.
• T Lim
Temperature limit defined in the method for the internal temperature in the
reference vessel.
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• p Lim
Pressure limit defined in the method.
• p Rate
Limit of pressure increase rate defined in the method.
Hint:
Pressure and temperature values will only be available if the reaction was
carried out with activated and installed sensors.
6.5.1.2 Review - P-Graph
The review P-graph displays the power and pressure vs. the reaction time.
Programmed power
profile
Pressure curve
Actually applied microwave Time and reason of the first power reduction
power
Fig. 6 - 10 Review - P-graph
The diagram contains the following information:
• Programmed power profile

If a power program was used the programmed set point is displayed as a
dotted line.
• Actually applied microwave power

The black filled area shows the actually applied microwave power which may
deviate significantly from the programmed power profile if pressure,
temperature or pressure rate limits are reached.
• Pressure
This curve indicates the pressure course during the reaction.
• P-reduction time
For explanation of the herein stated "control parameters" refer to chapter
11.2.5, "Power Reduction by the Instrument".
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6.5.1.3 Review - T-Graph
The review T-graph displays the internal temperature and pressure vs. the
reaction time.
(Internal) Temperature Pressure
Fig. 6 - 11 Review - T-graph
• (Internal) temperature
Shows the temperature course in the reference vessel.
• Pressure
Shows the pressure course during the run.
6.5.1.4 Review - IR-Graph
The review IR-graph displays the individual IR temperatures and the reaction
pressure vs. the reaction time.
IR Temperatures
IR Temperature of the empty positions Pressure
Fig. 6 - 12 Review - IR-graph
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• IR temperature
Shows the IR temperature curves during a reaction. These data mainly
provide information about uniformity of heating.
Hint:
IR values may differ if varying mixtures are applied in the individual vessels.
• Pressure
Shows the pressure course during the run.
6.5.1.5 Review - Sample Documentation
This menu item allows the entry of additional sample information. Changes can
be entered as necessary. The printout includes date and time of changes, if the
changes were done after the run has been completed.
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6.6 Setting Up the Instrument
Starting from the main menu, press <Setup F3> to reach the setup menu.
The setup menu is used to change instrument settings. Use the arrow keys
<Ï F4> and <Ð F5> to select the desired options from the setup menu. Confirm
by pressing <Enter F1>.
Fig. 6 - 13 Setup - menu
The following options are available in the setup menu:
• Configuration
Use this option to set the language (v2.0 or higher), date, time and "device
name" and if necessary, make the appropriate layout settings for an external
keyboard.
• Printer Setup
This option is used to set the printer type, printer interface and character
settings.
• Serial Port Setup

This option is used to set the text compression and transfer delay for data
transmission.
• Safety Cooling
Set parameters for safety cooling like cooling intensity, cooling time or
temperature limits.
• Rotors
Activate / deactivate the appropriate rotor types.
• Sensors
Activate / deactivate the appropriate sensor types.
• Accessories
Activate / deactivate accessories.
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6.6.1 Configuration
Use the arrow keys <Ï F4> and <Ð F5> to select the configuration menu.
Confirm by pressing <Enter F1>.
Fig. 6 - 14 Setup - Configuration
Using the keys <+ F2> and <– F3> you may create or change any data or
parameters in the entry or option fields, i.e. you may select letters or change
between different options.
The arrow keys <Í F4> and <Î F5> are used to move to the next or return to
the previous entry field. Press <Exit F1> to store your entries / modifications and
revert to the setup menu.
Press <ESC> to exit without saving.
The setup configuration section consists of five entry / option fields:
• Language
Multilingual user interface (v2.0 or higher).
• Ext. Keyboard
Select between the German or English keyboard layout.
• Device Name
Enter an instrument name consisting of max. 12 characters. This name will
be stored in the run data and will be printed out.
• Date
Set the current date ("YYYY-MM-DD").
• Time
Set the internal clock.
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6.6.2 Printer Setup
Use the arrow keys <Ï F4> and <Ð F5> to select the printer setup menu. Confirm
by pressing <Enter F1>.
Fig. 6 - 15 Setup - Printer setup
The setup printer menu is used to select the connected printer. It consists of four
option fields.
• Printer Type
The system distinguishes between the following printer types:
- Plain Text
This setting is for printer models with an internal "character set", i.e. printers
that are capable of printing ASCII sequences. This setting can only be used
to print text - you will not be able to print any graphs using this setting.
- Epson 9 Pin
This setting is for Epson 9-pin printers or Epson-compatible printers. Used
printer protocol: ESC/P Standard; printing text and graphics.
- Epson 24 Pin
This setting is for Epson 24-pin printers or Epson-compatible printers. Used
printer protocol: ESC/P Standard; printing text and graphics.
- PostScript
This requires a PostScript printer (like special laser printers): e.g. HP
Laserjet 4 M-plus or a newer model, such as HP 4050n. Used printer
protocol: PostScript Language Level 3; printing text and graphics.
- HP DeskJet
This setting is for HP DeskJet printers or HP DeskJet-compatible printers.
Used printer protocol: PCL 5; printing text and graphics.
- HP LaserJet
This setting is for HP LaserJet printers or HP LaserJet-compatible printers.
Used printer protocol: PCL 5; printing text and graphics.
• Printer Port
Select Centronics if a printer is connected to the parallel port. Select Serial
for sending data via the serial port (RS232) to a connected PC.
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• Decimal Separator
Use this option to select between a period (1.123) or comma (4,567) as
decimal separator.
• Character Set
Use this option to select between the ASCII MS-DOS CP437 and ISO 8859-
1 Latin 1 character set, if some characters are not printed correctly.
The <+ F2> and <– F3> keys are used to select the different options. The arrow
keys <Í F4> and <Î F5> are used to move between the entry fields. Press
<Exit F1> to save your changes and revert to the Setup menu. Press <ESC> to
discard your entries.
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6.6.3 Serial Port Setup
The serial port setup menu is used to set the parameter for data transfer.
Use the arrow keys <Ï F4> and <Ð F5> to select the serial port setup menu.
Fig. 6 - 16 Setup - Serial port setup
The following parameters are available in the serial port setup menu:
• Text Compression
Text compression reduces the amount of data for faster transfer rates. Data
can be imported into a MS Excel irrespective of the used compression mode.
- None:
No compression, slowest data transfer. Best format for processing with a
text editor.
- Medium:
Character spaces are removed, transfer is accelerated.
- High:
Data duplications are removed, transfer needs only a quarter of the time
without compression.
• Transfer Delay
Depending on the CPU-type and operation system, data transfer without
delay might be too fast for the computer. Increase the transfer delay if you
experience problems with the data transfer.
- For data transfer to external PCs via a terminal program a delay is usually
not necessary.
- For data transfer with AP-Softprint we recommend a transfer delay of at
least 30 ms. (Possible transfer delays: None, 10, 20, 30, 50, 100, 250 and
500 ms;)
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6.6.4 Safety Cooling
The safety cooling menu can be used to adjust the intensity of cooling fan level,
cooling time, temperature limit and IR limit.
Use the arrow keys <Ï F4> and <Ð F5> to select the safety cooling menu.
Fig. 6 - 17 Setup - Safety cooling
The safety cooling system is activated:
• After terminating the experiment.

• An unexpected reset of the instrument, e.g. after a power failure.
• If no cooling step has been programmed in the method.
• Cooling Fan Level

Press the <+ F2> or <– F3> key to select between cooling fan level 2 and 3.
- Cooling Fan Level 3

Highest intensity (190 m3/h). Benefit: Short cooling time. The minimum
cooling time is 30 minutes.
- Cooling Fan Level 2
Medium intensity. Benefit: Lower noise level. The minimum cooling time is
60 minutes.
Hint:
After an overpressure release inside the cavity (e.g. safety disk or vessel
breakage), the safety cooling will always run on fan level 3.
• Temperature Limits
Depending on the used sensors, you can choose the temperature values,
which have to be reached during the cooling process. Default settings for
synthesis applications are 60 °C for internal temperature and 50 °C for IR
temperature, both limits can be reduced down to 40 °C.
Please note that reducing these values will result in increased cooling times.
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6.6.5 Rotors
Rotor types have to be activated before they can be used!

Use the arrow keys <Ï F4> and <Ð F5> to select the rotors menu. Confirm by
pressing <Enter F1>.
Fig. 6 - 18 Setup - Rotors step 1
Move the black cursor to the desired rotor type using the arrow keys <Ï F4> and
<Ð F5>.
Activate or deactivate the selected rotor type by pressing <+ F2> or <– F3>.
Press <Exit F1> to confirm the changes.
Press <ESC> to exit without saving the changes.
The current status is displayed by a symbol, which is shown to the left of the
selected rotor type:
- Empty rectangle : Rotor is deactivated.

- Filled rectangle : Rotor is activated.
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6.6.6 Sensors
Sensors have to be activated before they can be used!

Use the arrow keys <Ï F4> and <Ð F5> to select the sensors menu. Confirm by
Fig. 6 - 19 Setup - Sensors
Move the black cursor to the desired sensor using the arrow keys <Ï F4> and
<Ð F5>. Activate or deactivate the selected sensor by pressing <+ F2> or <– F3>.
selected sensor:
- Empty rectangle : Sensor is deactivated.

- Filled rectangle : Sensor is activated.
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6.6.7 Accessories
Accessories have to be activated before they can be used!

Use the arrow keys <Ï F4> and <Ð F5> to select the sensors menu. Confirm by
Fig. 6 - 20 Setup - Accessories
Move the black cursor to the desired accessory using the arrow keys <Ï F4> and
<Ð F5>. Activate or deactivate the selected accessory by pressing <+ F2> or
<– F3>.
selected accessory:
- Empty rectangle : Accessory is deactivated.

- Filled rectangle : Accessory is activated.
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6.7 Service
The service section of the software includes calibration and maintenance

programs. Use the arrow keys <Ï F4> and <Ð F5> to select the service menu.
Fig. 6 - 21 Service menu
The following options are available in the service menu:
• Software Update
For updating the software (requires an external PC)
• Power Calibration
For adjusting the microwave power output
• Power Check
For checking the microwave power output
• Temp. Sensor Calibration

For calibration of temperature sensor (p/T sensor or T-probe)
• Temp. Sensor Check

For checking the accuracy of temperature sensor (p/T sensor or T-probe)
• Temp. Sensor Settings

For entering the calibration factors of temperature sensor (p/T sensor or T-
probe)
• IR Sensor Calibration
For adjusting the IR sensor
• IR Sensor Check
For checking the IR sensor
• Solvent Sensor Settings

For entering the calibration factors of the solvent sensor
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• Exhaust Unit Installation

For changing the exhaust unit settings
• Library Maintenance Tool

For managing the methods of the method library.
• Advanced Service Routines

This program section includes special service programs. Access to this
option is password-protected and restricted to authorized service engineers.
6.7.1 Software Update
Hint:
We recommend to check regularly for new software versions (http://
www.anton-paar.com) and to install if appropriate.
The following equipment is required:
- External PC with a free serial interface, Windows 98 or higher with NET 2.0
(v2.00 or higher)
(Alternatively: External PC with USB port, serial-to-USB converter cable)
- Serial link (0-Modem) cable, this cable is also available from Anton Paar
GmbH or its sales representatives
- Flash update program for Synthos 3000 (available from Anton Paar GmbH
free of charge)
Synthos 3000 software installation file(s) (available from Anton Paar GmbH
free of charge)
Press <Enter F1> to enter the software update menu. Connect the host
computer´s serial port and run the program Flash Update to activate the
bootloader. Follow the instructions given therein to proceed with the update.
6.7.2 Power Calibration
The purpose of this calibration procedure is to adjust the microwave power

parameters to ensure accurate values for the applied power output.
The calibration is based on the knowledge of the specific heat capacity of water.
By heating up a certain amount of water with microwave energy, the apparent
power can be calculated from the water volume, the temperature of the water
before and after heating.
The power calibration consists of the following steps which are carried out
automatically by the software:
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- Determining the apparent power output of the microwave generators

- Calculating a power factor
Use the arrow keys <Ï F4> and <Ð F5> to select the power calibration menu.
6.7.2.1 To Perform a Power Calibration
To perform a power calibration, refer to chapter 5.5, "Microwave Power

Calibration".
6.7.3 Power Check
The power check function is used to verify the microwave power calibration. The
procedure is the same as described for the power calibration, but at a target
power of 1400 W.

Fig. 6 - 22 Service - Power check finished
Hint:
If the apparent microwave power deviates from the nominal value by more than
10% a microwave power calibration should be performed.
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6.7.4 Temperature Sensor Calibration with the Calibration

Accessory
For regular calibrations, an optional calibration accessory is required to calibrate

the p/T sensor (Rotor 16) and the T-probe (Rotor 8S). Calibration should be done
once a year, although it is recommended to calibrate the temperature sensor at
least twice a year.
Hint:
Description only valid for calibration accessory up to version 4.
If you are using a calibration unit, please follow the instructions in chapter
Use the arrow keys <Ï F4> and <Ð F5> to select the temperature sensor
calibration menu. Confirm by pressing <Enter F1>.
Version 4
Fig. 6 - 23 Calibration accessory
6.7.4.1 To Calibrate the p/T Sensor
1. Carefully insert the p/T sensor into the calibration accessory and close the
screw cap.
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Fig. 6 - 24 Inserting the p/T sensor into the calibration accessory
2. Place the calibration accessory with the temperature sensor into position 1 of
your rotor and place the rotor without lid into the microwave cavity.
Fig. 6 - 25 Inserting the calibration accessory
Important:
Do not close the instrument door as this will damage the cable of the
calibration accessory.
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Fig. 6 - 26 Temperature sensor calibration
3. Connect the cable of the calibration accessory to the CAL port on the right-
hand side of the instrument. Tighten the screws of the plug to ensure good
contact.
Fig. 6 - 27 Connecting the cable of the calibration accessory to the instrument
4. Press the <Calib F1> key to start the calibration. The serial number of the
temperature sensor is read out first. The calibration accessory starts to heat
and the temperature values are recorded automatically.
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5. At the end of the heating phase (approx. 15 - 20 minutes) the result of the
calibration is displayed. Press <Save F1> to store the calculated calibration
factors. You might press <Print F5> to print out the factors. By pressing
<Repeat F4> you can repeat the calibration. Press <ESC> to exit without
any changes.
Fig. 6 - 29 Service - Temperature sensor calibration - process finished
Warning:
The surface of the calibration accessory is hot. Do not touch the calibration
accessory for at least 20 min after finishing the calibration.
6. To avoid entering wrong calibration constants, remove the adhesive label

from the sensor arm, if new calibration factors have been stored in the
instrument.
6.7.4.2 To Calibrate the T-Probe
1. Put the calibration accessory into the protective casing. Make sure you lead
the cable of the calibration accessory to the left side of the protective casing
strap.
Fig. 6 - 30 Putting the calibration accessory in the protective casing
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2. The immersion tube with seal (XF/XQ) can now be put into the calibration
accessory. The venting screw has to point to the same direction like the
cable of the calibration accessory (left of the protective casing strap).
Fig. 6 - 31 Putting the immersion tube with seal into the calibration accessory
3. Put the protective cap onto the protective casing so that the cable and the
venting screw are led through the opening of the cap.
Fig. 6 - 32 Putting the protective cap on the calibration accessory
4. Place the complete vessel assembly together with 3 additional (empty)

vessels into Rotor 8S and close the rotor thumb wheels in order to fix the
vessels. The calibration accessory has to be placed at position 1.
Fig. 6 - 33 Inserting the vessel into position 1
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5. Use the glass rod to make sure that the vessel in position 1 is positioned
correctly. If there is any resistance when inserting the rod, adjust the vessel
and try again. Repeat the procedure until you feel no resistance when
inserting the rod.
Fig. 6 - 34 Using the glass rod
Important:
Never insert the T-probe unless the vessel is correctly positioned and the rotor
is correctly closed, otherwise the glass bulb and the capillary may break!
6. Insert the T-probe very carefully through the hole on the upper plate of the
rotor into the vessel at position 1. The torus-shaped part of the T-probe is
placed over the sensor module. Adjust the thumb wheels so that the T-probe
is attached completely on the rotor upper plate.
Fig. 6 - 35 Inserting the T-probe
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7. Place the rotor without protection lid into the microwave cavity.
Important:
Do not close the door of the instrument as this might damage the cable of the
hand side of the instrument. Tighten the screws of the cable plug to ensure
good contact.
Fig. 6 - 37 Connecting the cable of the calibration accessory
T-probe is read out first. The calibration accessory starts to heat and the
temperature values are recorded automatically.
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calibration is displayed on the display. Press <Save F1> to store the
calculated calibration factors. You might press <Print F5> to print out the
factors. By pressing <Repeat F4> you can repeat the calibration. Press
<ESC> to exit without any changes.
Warning:
instrument.
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6.7.5 Temperature Sensor Calibration with the Calibration

Unit
For regular calibrations, an optional calibration unit is required to calibrate the

p/T sensor (Rotor 48 and Rotor 16) and T-probe (Rotor 8S), respectively.
The calibration unit consists of a vessel jacket with an integrated heating block, a
Pt-100 temperature sensor for correct measurement of the temperature of the
heating block and a metal support.
During the calibration the heating block is heated up to two measuring points
(40 °C and 180 °C).
The difference between the measured temperature values of the heating block
and the p/T-sensor is used to calculate two calibration factors.
Important:
After carrying out any maintenance or repair work on the temperature sensor,
it has to be recalibrated.
Fig. 6 - 40 Calibration Unit
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Metal support
Lock II with two holes
Lock I
Calibration insert holder
Front side
Back side with

counter weight
Cable
Calibration insert
Fig. 6 - 41 Metal support for the calibration insert and calibration insert
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6.7.5.1 To Calibrate the p/T Sensor
1. Check all parts, which are needed for calibration.
Metal support
Calibration insert (T/IR) with

cable
p/T sensor Rotor 48
p/T sensor Rotor 16
Fig. 6 - 42 All parts, which are needed for calibration of the p/T sensor for
Rotor 48 or Rotor 16
2. Open the metal support (see Fig. 6 - 43 /1).

Lift lock I towards the back side of the metal support (see Fig. 6 - 43 /2) to
open the interlock. Afterwards raise the pendant (see Fig. 6 - 43 /3) toward
the front side until the stop position is reached (see Fig. 6 - 43 /4). The
device is automatically fixed in this position.
Back side
Lock I
Front side
1 2
3 4
Fig. 6 - 43 Opening the metal support
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3. Attach the calibration insert to the ring on the front side of the metal support
(see Fig. 6 - 44 /1). Be aware that the two screws have to be at the side of
the lock II (see Fig. 6 - 44 /2). Lift the lock II, hold it and push the calibration
insert back to the fixed pendant (see Fig. 6 - 44 /3). Release the lock II, the
two screws have to fit into the two holes and then the calibration insert itself
is fixed (see Fig. 6 - 44 /4).
Screws
Lock II
with
two
holes
1 2
3 4
Fig. 6 - 44 Attaching the calibration insert to the metal support
4. Put the corresponding p/T sensor into the calibration insert. Be aware that
the arm of the p/T sensor rests between the two screws on the upper side of
the metal support.
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Fig. 6 - 45 Placing the p/T sensor into the calibration insert
5. Place the assembled calibration unit carefully (hold the sensor arm with one
hand) into the microwave cavity to avoid scratches to the coating. Take care
that the metal support fits as accurate as possible on the turntable. Then
connect the cable of the calibration unit to the CAL-port on the right-hand
side of the instrument. Tighten the screws of the cable plug to ensure good
contact.
Important:
Do not close the instrument door as this might damage the cable of the
calibration insert.
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Fig. 6 - 46 Inserting the assembled calibration unit
6. Select the service menu in the main menu by pressing <Service F4>.
7. Use the arrow keys <Ï F4> and <Ð F5> to select the temperature sensor
Fig. 6 - 47 Temperature sensor calibration - step 1
temperature sensor is read out first. The calibration insert starts to heat and
the temperature values are recorded automatically.
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calibration is shown on the display. Press <Save F1> to store the calculated
calibration factors. You might press <Print F5> to print out the factors. By
pressing <Repeat F4> you can repeat the calibration. Press <ESC> to exit
without any changes.
Warning:
Hot surface!
The surface of the calibration insert is hot.
Do not touch the calibration insert for at least 20 min after finishing the
calibration.
instrument.
11. After complete cooling, clean the calibration insert with a damp cloth, if
necessary. Let the calibration insert dry completely before next use.
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6.7.5.2 To Calibrate the T-Probe
1. Check all parts, which are needed for calibration.
Rotor 8
(without
protection lid)
Centering
jacket
Protective
cap
Spacer
T-probe Glass rod Calibration insert (T/IR) with cable

Immersion tube with seal
Fig. 6 - 50 All parts, which are needed for calibration
Protective cap
Immersion tube with seal
Spacer
Cable of the calibration

insert
Calibration insert
Centering jacket
Fig. 6 - 51 Assembled accessory for calibration of the T-probe
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2. Put the calibration insert into the centering jacket. Make sure to lead the
cable of the calibration insert through the slot of the casing.
Fig. 6 - 52 Putting the calibration insert into the centering jacket
3. Add the spacer directly on the top of the calibration insert with the two pits on
the bottom side. The two screws of the calibration unit have to fit into the two
pits.
Fig. 6 - 53 Adding the spacer
4. The immersion tube with seal (XF / XQ) can now be put into the calibration
insert. The venting screw has to point to the same direction as the cable of
the calibration insert.
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Fig. 6 - 54 Putting the immersion tube with seal into the calibration insert
5. Put the protective cap onto the centering jacket.
Fig. 6 - 55 Putting the protective cap on the centering jacket
6. Place the complete vessel assembly together with 3 additional (empty)

vessels into Rotor 8S and close the rotor thumb wheels in order to fix the
vessels. The calibration insert has to be placed at position 1.
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Fig. 6 - 56 Inserting the assembled calibration vessel into position 1
7. Use the glass rod to make sure that the vessel (in position 1) is positioned
correctly. If there is any resistance when inserting the rod, adjust the vessel
and try again. Repeat the procedure until you feel no resistance when
inserting the rod
Fig. 6 - 57 Proper positioning by using the glass rod
8. Afterwards close the rotor thumb wheels completely (no movement of the
vessels).
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Fig. 6 - 58 Closing the rotor thumb wheels with inserted glass rod
Important:
Never insert the T-probe unless the vessel is correctly positioned and the rotor
is correctly closed. Otherwise the glass bulb and the capillary may break!
9. Remove the glass rod and insert the T-probe very carefully through the hole
on the upper plate of the rotor into the vessel at position 1. The torus-shaped
part of the T-probe is placed over the sensor module. Adjust the thumb
wheels so that the T-probe is attached completely on the rotor upper plate.
10. Place the rotor without protection lid into the microwave cavity. Then connect
the cable of the calibration insert to the CAL-port on the right-hand side of
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the instrument. Tighten the screws of the cable plug to ensure good contact.
Important:
Do not close the instrument door as this might damage the cable of the
calibration insert.
Fig. 6 - 60 Placing the rotor into the cavity and connecting the cable of the unit
11. Select the service menu in the main menu by pressing <Service F4>.
12. Use the arrow keys <Ï F4> and <Ð F5> to select the temperature sensor
Fig. 6 - 61 Service - Temperature sensor calibration
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13. Press the <Calib F1> key to start the calibration. The serial number of the T-
probe is read out first. The calibration insert starts to heat and the
temperature values are recorded automatically.
calibration is shown on the display. Press <Save F1> to store the calculated
calibration factors. You might press <Print F5> to print out the factors. By
pressing <Repeat F4> you can repeat the calibration. Press <ESC> to exit
without any changes.
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Warning:
The surface of the calibration insert is hot. Do not touch the calibration insert
for at least 20 min after finishing the calibration.
instrument.
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6.7.6 Temperature Sensor Check with the Calibration

Accessory
You can use the temperature sensor check menu to test the accuracy of the
temperature sensor between 40 °C and 220 °C, by use of the calibration
accessory unit.
This procedure cannot be used for calibration purposes.
Preparing the calibration accessory is the same as described for temperature
sensor calibration, refer to chapter 6.7.4, "Temperature Sensor Calibration with
the Calibration Accessory".
6.7.6.1 To Check the Temperature Sensor
1. Insert the rotor and the calibration accessory into the oven cavity as
described in chapter 6.7.4.1, "To Calibrate the p/T Sensor" and chapter
6.7.4.2, "To Calibrate the T-Probe". Connect the calibration accessory and
press <Check F1> to continue.
2. Enter the desired temperature value via the external keyboard or use the
<+ F2> or <– F3> keys. The test temperature can be between 40 °C and
220 °C. Recommended values are:
Vessel type Temperature [°C]
MF100 190
HF100 / XF100 /XQ80 220
Press <Check F1> to continue.
3. The calibration accessory is heated to the defined temperature value. The

temperature measured by the p/T-sensor or T-probe is compared to the
temperature of the heating block sensor.
4. At the end of the heating phase the results are shown on the display. Using
the <Print F5> key you can print out the results or press <Repeat F4> to
repeat the check. (If the difference between the set value and the actual
value is more than 2 - 3, we recommend to repeat the check.)
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Fig. 6 - 65 Service - Temperature sensor check - process finished
Warning:
6.7.7 Temperature Sensor Check with the Calibration Unit
You can perform a temperature sensor check to test the accuracy of the
temperature sensor between 40 °C and 220 °C, by use of the calibration
accessory unit.´
This procedure cannot be used for calibration purposes.
Preparing the calibration unit is the same as described for temperature sensor
calibration, refer to chapter 6.7.5, "Temperature Sensor Calibration with the
Calibration Unit".
Important:
Instead of the rotor (when using the calibration accessory) you have always to
use the assembled calibration unit.
6.7.7.1 To Check the Temperature Sensor
1. Insert the calibration unit into the oven cavity as described in chapter 6.7.5.1,
"To Calibrate the p/T Sensor". Connect the cable of the calibration unit and
press <Check F1> to continue.
2. Enter the desired temperature value via the external keyboard or use the
<+ F2> or <– F3> keys. The test temperature can be between 40 °C and
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220 °C. Recommended values are:
MF50 200
MF100 190
HF100 220
Press <Check F1> to continue.
3. The calibration insert is heated to the defined temperature value. The

temperature measured by the p/T sensor is compared to the temperature of
the heating block sensor.
4. At the end of the heating phase the results are shown on the display. Using
the <Print F5> key you can print out the results or press <Repeat F4> to
repeat the check.

Fig. 6 - 66 Service - Temperature sensor check - process finished
Important:
If the difference between the set value and the actual value is too big (more
than 1%), perform a calibration!
Warning:
The surface of the calibration unit is hot. Do not touch the calibration unit for at
least 20 min after finishing the calibration.
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6.7.8 Temperature Sensor Settings
Temperature sensors are calibrated at the factory before shipping. The correct
factors are stated on an adhesive label attached to the temperature sensor and
on the supplied calibration certificate. The factors are assigned according to the
serial number of the sensor.
The software is able to store the calibration factors of several temperature

sensors.
Before using a new sensor for the first time, the calibration factors have to be
entered into the Synthos 3000 software. You can enter the factors using the
function keys. It is recommended to connect an external keyboard for easy entry
of numbers and letters.
Use the arrow keys <Ï F4> and <Ð F5> to select the temperature sensor settings
menu. Confirm by pressing <Enter F1>.
Fig. 6 - 67 Service - Temperature sensor menu
- If you want to enter factors for a new sensor, use <Ï F4> or <Ð F5> to
select "New Sensor“.
- For editing factors of an installed sensor, use <Ï F4> or <Ð F5> to select
an installed sensor.
- Press <Exit F1> to exit without any changes.
- For printing press <Print F3>.
Important:
Entering wrong values will result in incorrect measurement!
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1. Press <Edit F2> to access the edit mode.
Fig. 6 - 68 Service - Temperature sensor edit mode
2. Use the arrow keys <Í F4> and <Î F5> to move the cursor.
3. Enter or edit the values for the sensor via the function keys <+ F2> or <– F3>
or use an external keyboard:
- Serial number of the sensor (Sensor ID)
- Calib. Factor A
- Calib. Factor B
4. Press <Save F1> to store the entries. You might press <Discard F3> to
cancel the entries / modifications. By pressing <Delete F4> you can remove
an entry completely from the list. Press <ESC> to exit without any changes.
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6.7.9 IR Sensor Calibration with the Calibration Accessory
Hint:
For checking the accuracy of the IR sensor you have to perform an IR check
instead of a calibration (refer to chapter 6.7.11, "IR Sensor Check with the
Calibration Accessory"). Possible deviations of the IR measurement are not
shown during the calibration procedure.
To comply with the demands of GLP, an annual recalibration of the sensor is

recommended, to ensure the specified measuring accuracy.
Important:
For calibration of the IR sensor with the calibration accessory a calibration
accessory version 4 is required.
Indicates version 4
44
Fig. 6 - 69 Calibration accessory version 4
When calibrating a calibration accessory version 3 or older, the measured IR

temperatures might be wrong.
Use the arrow keys <Ï F4> and <Ð F5> to select the IR sensor calibration menu.
Important:
• Make sure you have entered the calibrator constant correctly.
- The calibrator constant is important for correct calibration.
Calibration without entering this constant or with an incorrect constant
leads to incorrect IR values and may leads to vessel overheating.
• Make sure that the vessel holder is correctly aligned.
- The correct alignment of the vessel holder is important for correct
calibration. Incorrectly aligned vessel holder leads to vessel
overheating.
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6.7.9.1 To Calibrate the IR-Sensor
This procedure works with both, Rotor 16 as well as Rotor 8S. For proper setup
with Rotor 8S refer to chapter 6.7.4.2, "To Calibrate the T-Probe".
1. Place the rotor in the oven cavity so that the calibration accessory is posi-
tioned exactly above the IR sensor. You can use the sensor for the rotor lid
detection as an orientation guide.
Protection lid detection
Fig. 6 - 70 Correct position of the calibration accessory
Important:
Do not close the door of the instrument as this will damage the cable of the
hand side of the instrument. Tighten the fastening screws of the plug to
ensure good contact.
Fig. 6 - 71 Connecting the cable of the calibration accessory
3. Enter the calibrator constant to ensure a correct IR sensor calibration. Use

the <+ F2> or <– F3> keys or an external keyboard.
Before calibrating the IR sensor, the calibrator constant has to be entered,
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which takes the emission value of the surface of the calibration accessory
into consideration. This calibrator constant is given on the supplied
calibration certificate.
Fig. 6 - 72 Service - IR Sensor Calibration - Entering the calibrator constant
4. Press <Next F4>.
5. Set the calibration temperature (range: 100 - 220 °C) depending on your
main operation range. Recommended values are:
MF100 160
HF100 210
XF100 /XQ80 220
Fig. 6 - 73 Service - IR Sensor Calibration - Entering the calibration

temperature
6. Press <Next F4>.
7. Check for proper alignment of the calibration accessory and press

<Calib F1> (see Fig. 6 - 70).
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Fig. 6 - 74 Service - IR Sensor Calibration - Starting the calibration
8. When pressing <Calib F1> the calibrator is heated. After a short period for
equilibration the turntable starts to rotate, indicating the beginning of the
calibration.
9. After completing the calibration you can either save the new transmission via
<Save F1>, print the calibration data via <Print F5> and/or repeat the
calibration via <Repeat F4>. Press <ESC> to exit without any changes.
%
Fig. 6 - 75 Service - IR sensor calibration - End of the calibration
Warning:
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6.7.10 IR Sensor Calibration with the Calibration Unit
Hint:
For checking the accuracy of the IR sensor you have to perform an IR check
instead of a calibration (refer to chapter 6.7.12, "IR Sensor Check with the
Calibration Unit"). Possible deviations of the IR measurement are not shown
during the calibration procedure.
To comply with the demands of GLP, an annual recalibration of the sensor is

recommended, to ensure the specified measuring accuracy.
Before calibrating the IR sensor, the calibrator constant has to be entered, which
takes the emission value of the surface of the calibration unit into consideration.
This calibrator constant is given on the supplied calibration certificate.
Use the arrow keys <Ï F4> and <Ð F5> to select the IR sensor calibration menu.
6.7.10.1 To Calibrate the IR Sensor
1. For proper assembling of the calibration device (without p/T sensor or T-

probe) refer to chapter 6.7.5, "Temperature Sensor Calibration with the Cali-
bration Unit".
2. Place the assembled unit carefully into the microwave cavity to avoid
scratches in the oven. Make sure that the calibration insert is opposite to the
sensor for the protection lid detection (on the right hand side of the oven
cavity).
Take care that the metal support fits as accurately on the turntable. Then
connect the cable of the calibration insert to the CAL-port on the right-hand
side of the instrument. Tighten the screws of the cable plug to ensure good
contact.
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Sensor protection lid
Fig. 6 - 76 Assembled unit in the oven
Important:
Do not close the door of the instrument as this will damage the cable of the
calibration unit.
3. Enter the calibrator constant to ensure a correct IR sensor calibration. Use

the <+ F2> or <– F3> keys or an external keyboard.
This calibrator constant is given on the supplied calibration certificate.
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Fig. 6 - 77 Service - IR Sensor Calibration - Entering the calibrator constant
Important:
• Make sure you have entered the calibrator constant correctly.
- The calibrator constant is important for correct calibration.
Calibration without entering this constant or with an incorrect constant
leads to incorrect IR values and may leads to vessel overheating.
• Make sure that the vessel holder is correctly aligned.
- The correct alignment of the vessel holder is important for correct
calibration. Incorrectly aligned vessel holder leads to vessel
overheating.
4. Press <Next F4>.
5. Set the calibration temperature (range: 100 - 220 °C) depending on your
main operation range.
Recommended values are:
MF50 140
MF100 160
HF100 210
XF100/XQ80 220
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Fig. 6 - 78 Service - IR Sensor Calibration - Entering the calibration

temperature
6. Press <Next F4> and start the calibration while pressing <Calib F1>.
Fig. 6 - 79 Service - IR Sensor Calibration - Starting the calibration
7. When pressing <Calib F1> the calibrator is heated. After a short period for
equilibration the turntable starts to rotate, indicating the beginning of the
calibration.
8. After completing the calibration you can either save the new transmission via
<Save F1>, print the calibration data via <Print F5> and/or repeat the
calibration via <Repeat F4>. Press <ESC> to exit without any changes.
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%
Fig. 6 - 80 Service - IR sensor calibration - End of the calibration
Warning:
6.7.11 IR Sensor Check with the Calibration Accessory
By performing the IR sensor check you can observe a possible deviation of the IR
Sensor. This procedure cannot be used for calibration purposes.
For checking the IR sensor the calibration accessory version 4 is required.
Indicates version 4
Fig. 6 - 81 Calibration accessory
Use the arrow keys <Ï F4> and <Ð F5> to select the IR sensor check menu.
Perform the handling procedures as described in chapter 6.7.9, "IR Sensor

Calibration with the Calibration Accessory".
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Fig. 6 - 82 Service - IR Sensor Check - During the check
Fig. 6 - 83 Service - IR Sensor Check - End of the check
Warning:
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6.7.12 IR Sensor Check with the Calibration Unit
The accuracy of the IR sensor can be tested by using the IR sensor check.
By performing the IR sensor check you can observe a possible deviation of the IR
Sensor. This procedure cannot be used for calibration purposes.
Fig. 6 - 84 Calibration Unit
Use the arrow keys <Ï F4> and <Ð F5> to select the IR sensor check menu.
Perform the handling procedures as described in chapter 6.7.10, "IR Sensor

Calibration with the Calibration Unit".
Fig. 6 - 85 Service - IR Sensor Check - During the check
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Fig. 6 - 86 Service - IR Sensor Check - End of the check
Warning:
6.7.13 Solvent Sensor Settings
The solvent sensor is calibrated at the factory before shipping. The correct
calibration constant is stated on an adhesive label attached to the solvent sensor
and on the supplied calibration certificate.
Before using a new sensor for the first time, the calibration factors have to be
entered into the Synthos 3000 software.
The settings of the solvent sensor can be checked by using the solvent sensor
settings.
Use the arrow keys <Ï F4> and <Ð F5> to select the solvent sensor settings
Fig. 6 - 87 Solvent sensor settings
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6.7.13.1 To Enter the Calibration Constant
1. Press <Edit F2> to access the Edit mode.
Fig. 6 - 88 Service - Solvent sensor settings - step 2
2. Enter the calibration value noted on the calibration certificate of your sensor.
3. After entering the calibration constant press <Exit F1>.
Fig. 6 - 89 Service - Solvent sensor settings - step 3
4. Press <New F2> to add a new setup. You might press <Discard F3> to
cancel the entry. Press <ESC> to exit without any changes.
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6.7.14 Exhaust Unit Installation
Hint:
This function is only needed if the whole exhaust unit has been replaced.
Use the arrow keys <Ï F4> and <Ð F5> to select the exhaust unit installation
To install an exhaust unit press <Edit> and select the type. Confirm by pressing
<Install>.
Detailed description will be provided with every replacement exhaust unit.
6.7.15 Library Maintenance Tool
The library maintenance tool is a software function for the maintenance and
management of the method library. After opening the "Library Maintenance Tool“
menu, a list of all stored methods will be displayed.
Hint:
To simplify matters you can jump to an appropriate method by pressing the
initial letter.
Use the arrow keys <Ï F4> and <Ð F5> to select the library maintenance tool
%
%
Fig. 6 - 90 Service - Library maintenance tool
1. Use the external keyboard (with page up and page down) to select the
sample. The active entry is highlighted.
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2. Choose between the following options:
- View:
Allows you to view the methods on the display. In the "view" mode you may
add notes but you cannot modify the method.
- Lock:
Use this feature if you want to prevent a method from being modified.
Locked methods can be unlocked by repeating this command. A locked
method is marked by an "L" on the left side of the method name. When
editing a locked method in the library menu, it will be stored as a new
method.
- Hide:
Allows you to "hide" a method. The method is not visible in the library menu
but not deleted. Hidden methods are marked with "H“.
- Delete:
Allows you to delete a method. You must confirm this step by answering the
prompt with <Yes F1> or you can abort it by pressing <No F5>.
- Send:
Allows you to send all methods within an encrypted txt-file to an external
PC.
3. Press <ESC> to exit without any changes.
6.7.15.1 Method Transfer to the PC
You can transfer the encrypted method file from Synthos 3000 to your PC for
backup purposes. It is not possible to edit the methods within this file.
To Transfer the Methods to a PC:
Interconnect the external PC with COM1 of Synthos 3000 using a serial link cable
(0-Modem) and switch on Synthos 3000.
• First Step - On the PC:
1. Start the hyper terminal program by doubleclicking

"MW3000_Method_Update.ht"-file.
2. Choose from the menu bar "Transfer" and "Capture text file".
3. A new window appears which asks you where to store the text file.
4. Choose a file where you want to store the methods.
• Second Step - On Synthos 3000:
1. Press <Service F4> and open <Library Maintenance Tool>.

2. Press <Send F5> to transfer the methods to the PC.
3. During the transfer process a message box "Remote Access..." appears on
the display of Synthos 3000.
C49IB08A 128
6 Software
4. The transfer is finished as soon as the message box on the display

disappears.
5. Do not switch off the instrument during transferring the method file to the PC.
• Third Step - On the PC:
1. To store the file select "Capture Text- Stop" from the "Transfer" menu.
Hint:
For security reasons, the transferred method file is encrypted, thus it cannot
be edited on the PC.
• Fourth Step - Saving back the file:
1. Choose in the menu bar the item "Transfer".

2. Within this menu select "Send Textfile".
3. After selecting this "Send Text File" enter the file (use the
"C49IA08B_Aktuell_Application_Library.txt").
4. After selecting the file the transfer will start automatically and a pop up
message on the Synthos 3000 screen appears.
Please note, depending on the computer, the transfer can take between
5 min and 20 min.
5. After the pop-up message disappears, the upload is done.
6.7.16 Advanced Service Routines
The menu "Advanced Service Routines" is for authorized service engineers only.
For this reason it is secured with a password.
C49IB08A 129
6 Software
6.8 Info
Pressing <Info F5> on the main menu provides the Info screen giving the
following information about the instrument and Anton Paar GmbH.
6j\dS]c
Fig. 6 - 91 Info - Manufacturer information
• Instrument:
- Version number of the installed software.

- Serial number of the instrument
• Anton Paar GmbH:
- Postal address
- Telephone and fax number
- Email and URL address
When pressing <Next F1>, the usage history is shown (v2.0 or higher).
C49IB08A 130
6 Software
6.9 AP Softprint
AP Softprint is used to transfer run data from Synthos 3000 directly into a
Microsoft Excel sheet. This Excel Add-In supports the following functions:
• Receiving run-data during and after a run

• Auto-draw function to generate graphs from the received run-data
(including RTP - Online graph - for viewing the run-status during operation)
The program is available free of charge for users of Anton Paar's Synthos 3000
at our homepage (www.anton-paar.com) and already included on the Manual CD.
Hint:
For detailed information refer to the instruction manual for AP Softprint on the
Manual CD (Doc. No. B83IB39) or download this document from our
homepage.
RTP
Fig. 6 - 92 Data transfer using AP Softprint
C49IB08A 131
7 Troubleshooting
7 Troubleshooting
This section includes the most important error messages that might be given
during the operation of Synthos 3000. The tables below give an explanation of
error causes and indicate possible remedies.
If you have any problems which are not described below, do not hesitate to
contact our local customer service.
7.1 Software
The most important error messages appear as pop-up error messages. This is a
highlighted text on the instrument display which gives a description of the error
situation and recommends ways to remedy these errors.
7.1.1 Error Message Menu - List of Error Codes
More detailed error information is frequently offered by Synthos 3000 in the form
of error codes. In contrast to "pop-up error messages" these error codes have to
be accessed and viewed manually in an error message menu. The error menu
(list) includes a print option, i.e. you can print the listed error codes and messages
on a connected printer or send them to an external computer.
The "error code table" can be accessed in two different ways:
• By pressing <CTRL> + <SHIFT> + <E> on the external keyboard anywhere

in the software menu).
• Via several selected "pop-up error messages". In such cases the <F5>
function key is re-assigned for details, i.e. will give you access to the error
menu by pressing <Details F5>.
Error codes can be interpreted quickly by skilled service engineers.

Therefore note down the error codes before consulting our local customer
service.
C49IB08A 132
7 Troubleshooting
>?-DUPoDUF._]g]D[]qDg]`_+
>
?.5$6F_fÙ._]g+D][FP
>
?.5$6F_fÙ5FNFTg]`_7]^F
>
?.5$6F_fÙ5FNFTg]`_7]^F
>
?4òFU(`DUP8_W_ò_5FfT`
Fig. 7 - 1 Example for an Error Code List
C49IB08A 133
7 Troubleshooting
7.1.2 Pop-up Error Messages in the Case of an "Alarm"
Error message
Explanation/possible cause • Remedy 1

• Remedy 2 ...
Explosion!
Rotor may be polluted with reagents / sample! In case of vessel breakage, do
not continue with your work! Danger of microwave leakage! (see F4 Info)
Safety cooling will not stop automatically!
Power off in: xx:xx min.
• Rupture of a safety disk or • At the end of the countdown

reaction vessel due to a switch off the instrument.
spontaneous reaction. After rupture of a safety disk,
• Door opened without using the clean and inspect the oven
door opener. cavity carefully before further
operation.
In case of vessel explosion, the oven

and the rotor have to be inspected by
a service engineer to guarantee
microwave safety.
Fire or Overtemperature!
Danger of hot vessels and reagents! Let cool down for at least 6 hours before
opening! (see Info F4)
• Fire or overtemperature in the • Refer to chapter chapter 3.3,

microwave cavity. "Unexpected Operation
• Malfunction of "Fire" sensor. Behavior".
After a fire or overtemperature, the

oven and the rotor have to be
inspected by a service engineer to
guarantee microwave safety.
If no fire occurred and the problem
still persists, contact our local
customer service.
C49IB08A 134
7 Troubleshooting
Error message

• Remedy 2 ...
Overtemperature Alarm!
The magnetron´s temperature limit was exceeded!
• The microwave cavity was • Observe the minimum filling

operated with insufficient load. volume per vessel.
• You have used badly coupling • Change the reagent mixture.
reagents such as non-polar • Change the position of the
organic solvents. instrument.
• The magnetron cooling system • If the problem still persists,
failed. (e.g. The instrument is contact our local customer
positioned too close to a wall, service.
sound insulating hood too
close to a wall.)
Power Unit Failure!

An unexpected reset occurred.
• Internal failure of the power • If the reaction program was

unit. aborted, wait until the safety
cooling time has elapsed.
Switch the instrument off and
on again. If the problem still
persists, contact our local
customer service.
Power Unit Failure!

Internal stack error.
• Internal failure of the power • If the reaction program was

unit. aborted, wait until the safety
cooling time has elapsed.
Switch the instrument off and
on again. If the problem still
customer service.
C49IB08A 135
7 Troubleshooting
Error message

• Remedy 2 ...
Safety Module SOLV failure!

Danger of hot vessel resp. high concentration of solvents or acid inside the
oven. Do not open the door! Power off in xx:xx min.
• The exhaust unit was switched • Make sure that the cooling air
off by the thermal protector. inlet and outlet of the exhaust
• The exhaust unit is defective / unit are not blocked.
blocked. • Check proper function of the
• The exhaust unit is activated exhaust unit.
but the safety module SOLV • Reconnect any loose sensor
causes an error. hoses.
• The sensor hoses are loose. • If further maintenance is
required, contact our local
customer service.
Solvent Sensor Alarm!

Dangerous concentration of flammable solvents inside the cavity. Press STOP
and let the rotor cool down for 30 min! Do not open the door. Power off in xx:xx
min.
• The solvent concentration • Press STOP to let the

inside the cavity is higher than instrument cool down and
the calibrated limit. check the vessels, sealings
• The stored sensor values are and safety disks for visible
incorrect. damage.
• The sensor is defective. • Check the function of the
sensor.
• Replace the sensor.
Solvent Sensor failure!

Bad contact or sensor breakage! Check proper installation or replace the
sensor!
• The solvent sensor has a bad • Plug in the solvent sensor or

contact. check the connection.
• The sensor is defective. • If the problem still persists,
contact our local customer
service.
• Replace the sensor.
C49IB08A 136
7 Troubleshooting
Error message

• Remedy 2 ...
Stirrer blocked!
The power supply of the power unit failed.
• Magnetic stirrer drive is • Switch the instrument off and

blocked. on again.
• If the problem still persists,
service.
Warning!
Pressure increase exceeded 3.0 bar/s after xx:xx min. Process continues
automatically. Change profile or sample weight to optimize the method!
• The pressure increase • Use more diluted mixtures.

exceeded 3.0 bar/s in the • Reduce microwave power or
reaction vessels and caused increase the temperature/
the microwave to be switched power ramp time.
off temporarily. The cooling
intensity was increased to level
3. The microwave power will
slowly be increased again to
the default intensity.
C49IB08A 137
7 Troubleshooting
7.1.3 Pop-up Messages During System Check
Error message

• Remedy 2 ...
The solvent sensor is not calibrated.

Please refer to menu service for calibration. Do you want to continue without it?
• The calibration factor has not • Enter the calibration factors.

been entered.
STOP!
The IR sensor is not activated! For safe operation you must use a slightly
increasing power profile. Do you want to continue?
• The IR sensor is not activated. • Activate the sensor and/or use

a very slightly increasing power
profile.
• For method development,
contact the application
specialists at Anton Paar
GmbH.
Start temperature lower than 10 °C! Please check the temperature sensor.
• The temperature sensor is • Perform a temperature

invalid calibrated. calibration.
• Capillary is broken. • If the calibration does not work,
• The temperature sensor is send the sensor to our local
defective. customer service for
calibration.
• Send the temperature sensor
to our local customer service
for repair.
The starting pressure is not within the range of 2 to 25 bar! Please close the
rotor in the proper way and restart the process.
• Rotor 8S is closed too much. • Release the gas pressure.

• Rotor 8S is closed too less. Open the upper plate of
• The charging with gas was too Rotor 8S once again and close
much. it using less force.
• Release the gas pressure.
Open the upper plate of
Rotor 8S once again and close
it using more force.
• Fill once again with gas.
• Check the correct positioning
of all vessels.
C49IB08A 138
7 Troubleshooting
7.1.4 Pop-up Error Messages During System Check
Error message

• Remedy 2 ...
Invalid rotor type or vessel position marks could not be recognized.
• You are using the wrong rotor • Use the correct rotor type.
type for the selected method. • Clean the position recognition
• The optical sensor for position sensors with a damp cloth (or
recognition is contaminated or with a cotton bud).
defective. • Check and clean the reflective
• The rotor does not turn. stripes (vessel position marks)
• The reflective stripes on the on the rotor bottom.
rotor are missing or dirty. • If the problem still persists,
service.
Invalid rotor type. Please change method according to the used rotor.
• You are using the wrong rotor • Use the correct rotor type or
type for the selected method. change the method.
Please install p/T sensor to run temperature controlled reaction or change your
method according to the used sensors!
• You have started a method that • Insert the p/T sensor or change
requires the optional p/T the method.
sensor but the sensor was not • If the p/T sensor is installed,
detected. check the correct alignment of
the sensor. If it is aligned
properly but the failure still
customer service.
Please install T-Probe to run temperature controlled reaction or change your

method according to the used sensors!
• You have started a method that • Insert the T-probe or change

requires the optional T-probe the method.
but the sensor was not • is installed, check the correct
detected. alignment of the sensor. If it is
aligned properly but the failure
still persists, contact our local
customer service.
C49IB08A 139
7 Troubleshooting
Error message

• Remedy 2 ...
Starting of the reaction process failed.
• The starting procedure has • For more detailed information,

been interrupted. press <Shift+Ctrl+E>.
• Internal program error. • Switch the instrument off and
on again.
service.
The Exhaust Module does not work!

Check if it is connected.
• The power plug of the exhaust • Insert the plug of the exhaust
unit is not connected or is not unit into the appropriate socket
connected properly. at the rear side of the
• The exhaust unit is defective. instrument.
• Check if it is connected
properly.
• If it is connected properly but
the problem still persists,
service.
The Microwave Unit could not be activated.
• Internal failure of the • Switch the instrument off and

instrument. on again.
service.
The power unit reports an alarm and is not ready for operation!
Please power up the device again.
• After switching on the device, • For more detailed information,

the software detects an alarm press <Shift+Ctrl+E>.
status in the electronics which • Switch the instrument off and
has not been reset on again.
automatically. • If the problem still persists,
service.
C49IB08A 140
7 Troubleshooting
Error message

• Remedy 2 ...
The Protection Lid was not detected.
• The rotor lid is missing. • Install the rotor lid.

• The optical sensor for rotor lid • Clean the rotor lid sensor with a
detection is contaminated or damp cloth (or with a cotton
defective. bud).
• The white marker on the rotor • Clean the marker on the rotor
lid is missing or dirty. lid.
service.
The rotor could not be turned on.
• Internal failure of the • Switch the instrument off and

instrument. on again.
service.
The sample contains one or more invalid parameters.
• Invalid parameters have been • Check the method.

found in the method after a • Correct the invalid parameters
plausibility check. and restart the reaction run.
The system check failed.
• Internal failure of the • For more detailed information,

instrument. press <Shift+Ctrl+E>.
• Switch the instrument off and
on again.
contact our customer service.
The Temperature Sensor was not calibrated! Please refer to menu service for
calibration.
• Calibration factors have not • Enter the calibration factors

been entered. (Setup-Temperature Sensor
Settings) or run a sensor
calibration.
C49IB08A 141
7 Troubleshooting
Error message

• Remedy 2 ...
Safety Module SOLV initialisation failed.

Check all sensor hoses, the exhaust channel as well as the exhaust unit for
proper installation.
• Sensor hoses are • Check all sensor hoses and

disconnected or blocked. external exhaust system for
• The exhaust channel is proper installation.
blocked. • Clean the exhaust channel.
• The external exhaust duct work • Push the silencer foam deeper
has incorrect specifications. into the exhaust hose.
• The silencer foam in the • Check the bending of the
exhaust hose is too close to the exhaust hose.
exhaust unit. • Contact our local customer
• The exhaust hose is bent too service.
much.
Pressure sensor not detected!

Please equip the rotor with the sensor or deactivate the sensor in the setup
menu if the method was designed to be done without sensor.
• Rotor 16 is not equipped with a • Insert the p/T Sensor.

p/T Sensor. • Deactivate the p/T Sensor if it
• The p/T Sensor is defective. is not used for your method.
• Rotor 8S is defective. For method development
without sensor contact our
local customer service.
• If the sensor is defective
service.
Temperature sensor not detected!

Please equip the rotor with the sensor or deactivate the sensor in the setup
menu if the method was designed to be done without sensor.
• Rotor 16 is not equipped with a • Insert the p/T Sensor or T-

p/T Sensor. Probe.
• The p/T Sensor is defective. • Deactivate the p/T Sensor or T-
• Rotor 8S is not equipped with a Probe if it is not used for your
T-Probe. method. For method
• The T-Probe is defective. development without sensor
service.
• If the sensor is defective
service.
C49IB08A 142
7 Troubleshooting
7.1.5 Pop-up Error Messages Under Various Conditions
Error message

• Remedy 2 ...
An error occurred. Data transfer aborted.
• A data transfer error has • Try to send the data again.

occurred while sending from • If the problem still persists,
menu "Review". contact our local customer
service.
Significant IR-Temperature Limit Overrange!

The process has to be aborted.
• The IR temperature limit has • Change your method. For

been exceeded significantly application support contact the
during a run. This may lead to application specialists at Anton
damage of the vessels. Paar GmbH.
Significant Pressure Limit Overrange!

• The reaction pressure limit has • Change your method. For

been exceeded significantly application support contact the
during a run. This may lead to application specialists at Anton
damage of the vessels. Paar GmbH.
Significant Temperature Limit Overrange!

• The reaction temperature limit • Change your method. For

has been exceeded application support contact the
significantly during a run. This application specialists at Anton
may lead to damage of the Paar GmbH.
reaction vessels.
The door did not close properly!

• The door opened during the • Let the instrument cool down
run due to thermal influences. and contact our local customer
• Failure of power supply. service.
The IR-Sensor failed!
• The IR sensor has failed during • Run a short program using

a run. 6 mL water with 1 mL of nitric
• The IR sensor is defective. acid and check the measured
IR temperatures.
service.
C49IB08A 143
7 Troubleshooting
Error message

• Remedy 2 ...
The Pressure Sensor failed!
• The pressure sensor has failed • Run a short program using

during a run. 6 mL water with 1 mL of nitric
• The pressure sensor is acid and check the measured
defective. pressure.
• If the error still persists, contact
our local customer service.
The Pressure Sensor grew hot inadmissibly!

• The temperature of the sensor • Increase the number of vessels

has exceeded the permissible or the applied volumes.
limit during the run. • Change the reaction mixture,
• The rotor was operated with or use passive heating
insufficient load. elements.
• You have used weak coupling • Refer to chapter 11,
reagents or unpolar solvents. "Applications" or contact our
local application specialists.
• Check the sensor for oil
leakage or deformation.
The Temperature Sensor failed!
• The temperature sensor has • Run a short program using

failed during a run. 6 mL water with 1 mL of nitric
• The temperature sensor is acid and check the measured
defective. temperature.
• If the error still persists, contact
C49IB08A 144
7 Troubleshooting
Error message

• Remedy 2 ...
The Temperature Sensor grew hot inadmissibly!

• The temperature of the sensor • Increase the number of vessels

has exceeded the permissible or the applied volumes.
limit during the run. • Change the reaction mixture,
• The rotor was operated with or use passive heating
insufficient load. elements.
• You have used weak coupling • Refer to chapter 11,
reagents or unpolar solvents. "Applications" or contact our
application specialists.
• Check the sensor for oil
leakage or deformation.
Turntable Error!
The turntable is not rotating.
• The rotor has stopped during a • Check the turntable and the
run or the rotor does not rotate reflective stickers.
at the defined speed. • If the error still persists, contact
Inside temperature dropped below the IR temperature!

The process has to be aborted. Please check the temperature sensor.
• The temperature sensor is • Calibrate the temperature

leaking or defective. sensor.
• IR-temperatures are wrong. • Calibrate the IR-sensor.
• You are using weak coupling • If the problem still persists,
reagents and/or unpolar contact our local customer
solvents. service.
Temperature did not increase during the last 5 minutes!

The process has to be aborted. Please check temperature sensor or adapt
programmed method.
• The sensor is defective. • Run a sensor calibration.

• The ramp is too long. • Reduce the ramp.
• Solvent and reagents are • If the problem still contact our
completely inert to microwave local customer service or our
irradiation. application specialists.
• Change the solvent, if
applicable.
C49IB08A 145
7 Troubleshooting
Error message

• Remedy 2 ...
Pressure loss of the hydraulic system!

Leakage might be caused by fire or melting of the top plate. Danger of hot
vessels and reagents!
Let cool down for at least 6 hours before opening. Please prepare an
extinguisher before opening the instrument.
• Pressure of the hydraulic • Refer to chapter 3.3,

system dropped below the "Unexpected Operation
limit. Behavior".
• Contact our local customer
service.
C49IB08A 146
7 Troubleshooting
7.1.6 Pop-up Error Messages During "Power Calibration"
Error message

• Remedy 2 ...
An error occurred. The power calibration process has to be aborted.
• An internal error has occurred. • For more detailed information,

press <Shift+Ctrl+E>.
on again.
service.
The door was opened! The process has to be aborted.
• The instrument door was • Repeat the power calibration.

opened during the power Keep the instrument door
calibration. closed.
The power ratio exceeds the range 0.7 and 1.3 and cannot be saved. Please
refer to the user manual!
• The start and/or end • Repeat the power calibration

temperature of the water has and make sure that the
been measured or entered temperature values are
incorrectly. recorded correctly.
• If the failure persists, enter a
• The calculated factor is out of limit value that is close to the
range due to aging or calculated factor (e.g. 1.3, if the
magnetron malfunction. calculated value is higher than
1.3, or 0.7, if the calculated
value is less than 0.7). Now
repeat the power calibration.
The "Power Factor" calculated
in this second step should
range between 0.7 and 1.3.
service.
C49IB08A 147
7 Troubleshooting
Error message

• Remedy 2 ...
The required microwave power cannot be achieved due to the power supply
limitations. The process has to be aborted.
• A power consumption of • Perform a power calibration at

> 16 A has been detected. a lower rating between 500 W
and 800 W.
• Call an electrician to check if
the line voltage is within the
specified range.
service.
C49IB08A 148
7 Troubleshooting
7.1.7 Pop-up Error Messages During "Temp. Sensor

Calibration" and "Temp. Sensor Check"
Error message

• Remedy 2 ...
An error occurred. The temperature calibration process has to be aborted.
• An internal error has occurred. • For more detailed information,

press <Shift+Ctrl+E>.
on again.
service.
The calibration factors exceed the range and cannot be saved.

Please refer to the user manual!
• The thermometer capillary is • Tighten the fixing screw of the

not fixed tightly enough. thermometer capillary.
• The seal of the thermometer • Loosen the thermometer
capillary is defective. capillary connections and
• The thermometer capillary is check the sealing surfaces.
broken. • Replace the capillary.
service.
The calibration temperature could not be reached!
• The calibration accessory/unit • Contact our local customer

or control unit is defective. service.
The calibrator unit is defective!
• The calibration accessory/unit • Connect the calibration

has not been recognized (bad accessory/unit to the
contact). appropriate CAL port on the
• The calibration accessory/unit right-hand side of the
is defective. instrument.
• Connection lost. • Tighten the fixing screw of the
plug using the screwdriver.
service.
C49IB08A 149
7 Troubleshooting
Error message

• Remedy 2 ...
The calibrator unit was disconnected!
• The calibrator unit was • Connect the calibrator unit to

disconnected during the appropriate CAL port on the
temperature sensor calibration. right-hand side of the
• The calibrator unit has not instrument.
been recognized (bad contact). • Tighten the fixing screws of the
plug using a screwdriver.
The maximum number of sensor setups was reached.

Please refer to menu service - temp. sensor settings to delete an unused
setup.
• Max. 30 sensor entries can be • Delete sensor settings which

stored in the menu service - are no longer needed.
temp. sensor settings.
The serial number is invalid. Please refer to the user manual!
• An invalid serial number has • Enter the serial number of the

been entered. sensor as stated on the
adhesive label of the sensor.
The Temperature Sensor has not initialized!
• The p/T sensor or T-probe has • Install the p/T sensor or T-

not been installed. probe.
• The rotor has not been placed • Check the position of the rotor
correctly (centrically) on the in the microwave cavity. Make
rotor drive. sure that the rotor has properly
• The p/T sensor or T-probe is engaged in the rotor drive.
defective. • If the problem still persists,
service.
C49IB08A 150
7 Troubleshooting
7.2 Rotor 16 and Rotor 8S
Malfunction
Possible cause • Remedy 1

• Remedy 2 ...
Traces of solvent at the venting screw or syringe adapter.
• Worn O-ring • Observe the maintenance

• The venting screw was not intervals and exchange the O-
closed properly. rings regularly.
• The venting screw was opened • Close the venting screw hand-
too much. tight until it reaches the stop
position.
• Do not open the venting screw
too much (max. 1 turn).
• Always store the screw cap /
seal holder assembly with the
venting screw opened to
increase the working life of the
material.
Vessels cannot be vented in the rotor after a reaction run.
• The rotor lid is not positioned • Turn the lid to the correct
correctly. position
• The venting screw is broken. • Rotor 16:
• The venting system of the seal Allow the vessel to cool down
has been clogged. completely and remove it from
the rotor. Carefully and slowly
open the screw cap. Venting
will occur via the safety
grooves in the liner.
• Rotor 8S:
Allow the vessels to cool down
completely. Slowly open the
thumb wheels of Rotor 8S
under a fume hood. Venting will
occur via the safety grooves in
the liner.
• Purge the seal (refer to chapter
9.4, "Cleaning and
Maintenance" for Rotor 16 and
chapter 10.4, "Cleaning and
Maintenance" for Rotor 8S).
C49IB08A 151
7 Troubleshooting
Malfunction

• Remedy 2 ...
Small amounts of solvent are lost.
• The seal was not expanded • Expand the seal for at least
properly. 3 seconds or use the seal
• The sealing lip is damaged. forming device. Expand a new
seal for 10 seconds.
• Replace the seal and/or liner.
7.3 Sensors
Malfunction

• Remedy 2 ...
Extreme differences in the IR temperature distribution of identical samples
• Leaking vessels. • Check the seal and venting

• The vessel holder is out of screw.
position. • Center the vessel holder above
• The vessel holder seal is out of the IR measuring eyelet.
position or missing. • Clean the vessel jackets.
• The ceramic / PEEK vessel • Install the Positioning Ring
jackets are contaminated. which fixes the vessel holders.
Traces of oil on the p/T sensor of Rotor 16 resp. pressure sensor of Rotor 8S
• Defective hydraulic system. • Do not use this sensor/rotor

• Send the sensor/rotor for
service/repair to our local
customer service.
C49IB08A 152
8 Rotor 48MF50
8 Rotor 48MF50
The following chapters contain a description of Rotor 48MF50 and provide
information on handling, cleaning and maintenance.
Fig. 8 - 1 Rotor 48 MF50
Rotor 48 has been designed specially for high sample throughput and is used for
a wide range of standard applications with Synthos 3000, which require pressures
and temperatures of up to 20 bar and 200 °C, such as library generation and
functionalization. It can be operated with up to 48 pressure vessels of the type
MF50.
8.1 Technical Description of Rotor 48
Rotor 48 consists of a rugged and microwave-transparent polymer construction.

Vessel holders, which are inserted into the rotor body, hold the reaction vessels
and provides effective guiding of the cooling air.
The rotor lid with a bayonet locking closes the rotor and ensures protection in
case of a sudden overpressure release (e.g. breakage of a safety disk).
Principle of rotation allows homogeneous heating characteristics as long as the

recommended loading patterns (refer to chapter 8.4.3.1, "To Load the Vessels
into the Rotor") are adhered to.
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Reactions are controlled via IR temperature measurement at every position in the

center circle (up to 16 vessels) and/or via the Pressure / Temperature Sensor M50
located in one reference vessel.
Important:
Never attempt to change the rotor geometry or to bring metal parts into the
microwave field. This will cause serious damage.
Rotor 48 Lid
Interlock Bolt 48
Pressure Vessel MF50
Rotor 48 Tray
Rotor Inner Base Ring 48
Rotor 48 Body
Rotor Base Ring
Fig. 8 - 2 Rotor 48MF50
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8.1.1 Vessels for Rotor 48
The combination of well-proven elements, such as fluoropolymers for the reaction

vessel, PTFE-TFM for the conical seal and the air cooling system, has led to the
design of high-performance, easy-to-handle pressure vessels with the following
technical data:
MF50
Liner Material PFA
Vessel Jacket Fiber-reinforced PEEK
Max. Operating Pressure 20 bar (290 psi)
Opening Pressure 30 bar (435 psi)
a 200 °C, for 30 min
Max. TINTERNAL
b 140 °C
Max. TIR
Nominal Volume 50 mL
Min. Filling Volume 6 mL
cMax. Filling Volume 25 mL
Typical Applications Library generation, functionalization/
derivatisation, small scale method
optimisation, solid-phase synthesis;
a. Temperature inside the reference vessel, measured via the p/T
sensor
b. Surface temperature at the base of the vessel, measured via the IR
sensor
c. The max. filling volume may exceed 25 mL for special methods
after consultation of Anton Paar application specialists
Important:
Do not fill in less than the minimum volume of 6 mL.
When using a volume of less than 6 mL, the amount of liquid phase in the
reaction vessel will be too low. As a result, microwave energy will couple
directly to parts of the vessel, the rotor or the sample. This may cause
damage to rotor components and pressure vessels.
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Screw Cap M50

Vent Pipe M50
Seal for Pressure

Vessel MF50
Safety Disk M50
Liner F50 PFA

O-Ring 22x2
Vessel Jacket M50

PEEK
Fig. 8 - 3 Pressure Vessel MF50
8.2 Limitations of Operation
8.2.1 Number of Vessels
For uniform heating, the vessels have to be loaded symmetrically into the rotor. If
the number of used vessels does not allow symmetrical loading it is possible to
substitute the missing vessel positions with blanks. (Refer to Chapter 8.4.3,
"Loading Rotor 48")
• Never use less than 4 vessels!
• When programming a power profile, always take care to adapt the

programmed power to the number of used vessels. The lower the number of
vessels used, the lower the power (see table below).
• When programming a temperature profile, the programmed temperature is

independent of the number of used vessels but the power limit should be
adapted accordingly (see table below!).
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Number of vessels Power max.

4 600 W
8 800 W
16 1100 W
24 1400 W
32 1400 W
48 1400 W
8.2.2 Temperature profiles
At max. temperature of 200 °C the hold time of 30 min. must not be exceeded!
At temperatures lower than 180 °C hold times of 60 minutes and longer may be
applied without compromising the vessel stability. Heat-up times (ramp times) are
not critical concerning material stability. However, a warning message will be
displayed when entering programs longer than 60 minutes.
8.2.3 Power Profiles
It is also possible to run power controlled experiments but power profiles must be
carefully chosen in order to avoid material stress to the vessel. The stored library
contains only tested temperature controlled methods as we highly recommend to
use the temperature/pressure sensor in any experiment.
Registered users can download the latest version of the method library from the
Anton Paar website (www.anton-paar.com).
8.2.4 Fan Settings
In order to avoid thermal overload, the fan must be set to level 2 (medium
intensity) after 30 minutes if a combination of following conditions applies:
- Ambient temperature higher than 25°C and

- Rotor loaded with more than 32 vessels and
- Reaction temperature higher than 150°C and
- Program run time longer than 30 minutes
The cooling time at fan level 3 must be set to 30 minutes. Even longer cooling
times may be required for fully loaded rotors at high ambient temperature.
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8.3 Prior to the First Reaction
Before you start your first experiment, it is recommended to get familiar with the
Synthos 3000 Microwave Reaction System. The best way is to start with either a
cleaning or a performance run from the method library.
If you are more familiar with microwave reactions, you should also perform a
blank run to clean the liner and seal (refer to chapter 8.5.1.1, "To Perform a
Cleaning Run").
Both ways enable you to operate the instrument without the risk of spontaneous
reactions and to learn about:
• Handling of instrument, rotor and pressure vessels

• Software functions
• Tightness of the pressure vessels
8.3.0.1 To Prepare the First Run
1. Check if rotors, sensors and accessories of Synthos 3000 are activated in

the software (refer to Chapter 6.6, "Setting Up the Instrument").
2. Prepare 10 mL of acidified water (1% of conc. nitric acid) per vessel. Using
this mixture will allow you also to check the functioning of the pressure and
temperature sensors.
Important:
Do not use deonised water due to the possible super-boiling effect. Using
pure water may result in a vessel explosion.
3. Select either a cleaning or a performance method ("PQ MF50") from the

method library.
4. When doing a blank run use either 6 mL of aceton, isopropanol, or the same
reagent mixture which will be used for synthesis.
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8.4 Performing a Reaction
This chapter provides the required information on how to perform a Microwave

Synthesis Reaction correctly. Follow these instructions to ensure safe and proper
operation.
Warning:
when handling solvents. Follow any special national safety regulations.
Important:
Before the first experiment read chapter 11, "Applications" very
carefully.
Performing a microwave sythesis consists mainly of the following steps:
• Selecting an appropriate method

• Adding reagents and solvents
• Assembling of the vessels
• Loading the rotor
• Starting the run
• Unloading the rotor after the reaction and venting the pressure vessels
• Cleaning the rotor, vessels and instrument
• Checking all parts for damages
8.4.1 Adding Reagents and Solvents
Guidelines for frequently used standard procedures are given in the method
library of Synthos 3000. Depending on a possibly different reaction behavior of
your reagents, the suggested mixture may have to be modified. The user is
responsible for this decision.
Important:
The use of the p/T sensor is highly recommended to thoroughly observe the
reaction progress.
8.4.1.1 To Add Reagents and Solvents
1. Weigh in the compounds into the liner.

Take care that no residues are sticking on the sealing area of the liner.
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Take care that no

residues are sticking
on the sealing area!
Fig. 8 - 4 Charging the vessels
2. Add solvent.
Rinse the liner by adding the solvent to remove material sticking on the top of
the liner wall. Make sure that no deposits remain on the wall of the vessel.
8.4.2 Closing the Vessels
The vessel is closed with a screw cap containing a conical seal made of PTFE-
TFM. Contrary to a lip-type seal, there is no need to expand this conical seal. This
facilitates vessel handling and saves time.
Sealing area
Fig. 8 - 5 Screw cap with conical seal
Important:
To avoid damage of the seal, do not close the screw cap without a liner
inserted into the vessel jacket.
Replace damaged seals immediately, as tightness of the vessel is not
ensured any longer.
Be aware that the O-Ring, which is positioned on the liner, fits properly to the
corresponding groove on the top of the liner. If the O-Ring is worn out, replace it
(refer to chapter 8.5.4.2, "To Replace the O-Ring").
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O-ring
Fig. 8 - 6 PFA liner with O-ring
8.4.2.1 To Close the Pressure Vessel
1. Remove any solvents or water droplets from the vessel jacket and the outer
surface of the liner. Liquid residues between liner and vessel jacket may
cause overheating and damage to the reaction vessel!
2. Place the liner into the vessel jacket.
3. Close the screw cap hand-tight in clockwise direction.
Important:
Do not use any tools for closing the screw cap.
Fig. 8 - 7 Closing the pressure vessel
8.4.2.2 To Apply the p/T Sensor
For appropriate reaction control the use of the optional p/T sensor M50 is
recommended.
Important:
The p/T sensor is equipped with a lip type seal instead of a conical seal. For
that reason it is important to expand the seal before use to ensure
tightness.
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1. Remove any solvents or water droplets from the vessel jacket and the outer
3. Press the screw cap completely onto the seal forming tool for at least 3
seconds to expand the sealing lip. (New seals have to be expanded for at
least 10 seconds.)
Seal Forming Tool p/T M50
Fig. 8 - 8 Expanding the lip-type seal of the p/T sensor
Important:
Make sure not to damage the immersion tube of the p/T sensor when
handling the seal forming tool.
4. Carefully apply the p/T sensor to the vessel.

Make sure that the seal of the sensor is inserted exactly into the liner. Take
care that there are no residues between the lip and sealing area.
Important:
Be careful when inserting the immersion tube of the p/T sensor, especially if
higher amounts of bulky samples or a magnetic stir bar is used. The
immersion tube may break!
5. Close the vessel hand-tight in clockwise direction.
6. The seal of the p/T sensor is connected to the hydraulic system and thus
slightly movable. For correct pressure measurement in the reference vessel,
the screw cap of the reference vessel has to be reopened from the stop
position for approx. 60° - 90°. If the reference vessel with the p/T sensor is
not reopened properly, pressure will be applied already by the vessel jacket.
As a consequence, the pressure readout will not show the correct reaction
pressure inside the reference vessel.
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90°
90°
Fig. 8 - 9 Reopening the sensor (90°)
8.4.3 Loading Rotor 48
The following procedures describe how to load the reaction vessels into the rotor
and how to close and insert the rotor into Synthos 3000.
8.4.3.1 To Load the Vessels into the Rotor
1. Place the vessels into the rotor following the recommended loading patterns.
To ensure uniform temperature distribution during the reaction process, the
rotor has to be loaded symmetrically. The recommended load patterns are
shown in Fig. 8 - 11.
2. If applicable: Insert the reference vessel with p/T sensor into position 1.
Fig. 8 - 10 Reference vessel with p/T sensor in position 1
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Fig. 8 - 11 Load patterns of Rotor 48MF50
Important:
Never use less than 4 vessels to avoid overheating of rotor or vessel parts!
3. Reduce the max. power in the method when using less than 48 vessels. As a
guideline, limit the max. power output to 800 W (8 vessels) or 400-600 W
(4 vessels), respectively.
4. If you have other numbers than the recommended ones to be processed, fill
the vacant positions with pure solvent to obtain a symmetrical load pattern.
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8.4.3.2 To Close the Rotor
1. Put the protection lid on the rotor body.
2. Close the rotor with the rotor lid by turning it clockwise.
Rotor 48 Closed position
Fig. 8 - 12 Closing Rotor 48
8.4.4 Performing a Synthesis Run
After the rotor and vessels have been prepared, the loaded rotor is put into the
microwave cavity. The experiment is started from the software menu.
Synthos 3000 controls all parameters automatically and usually does not require
user intervention.
At the end of a run, the cooling starts automatically. The safety cooling is also
activated automatically if an experiment run is aborted. The cooling is stopped as
soon as all vessels have cooled down to an internal temperature below 60 °C and
an IR temperature below 50 °C, depending on the installed sensors.
Warning:
Do not attempt to remove the rotor and vessels from the instrument before the
safety cooling has finished! Danger of hot and pressurized vessels!
Refer to chapter 3, "Safety Instructions".
8.4.4.1 To Start a Synthesis Run
1. Switch on Synthos 3000. The software starts automatically.
2. To put the loaded rotor into the microwave cavity, hold it with both hands at
the rotor bottom plate. Place it on the turntable inside the oven cavity until it
engages onto the rotor drive.
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Fig. 8 - 13 Placing rotor 48 into the microwave cavity
3. Close the door of Synthos 3000.
4. Select and start the method of your choice.

Synthos 3000 initiates a system check.
5. Start the experiment by pressing the green <Start> button after the system
check was successful. During the run the display informs you about the
reaction progress.
8.4.4.2 To Abort a Run
1. To interrupt (pause) the program, press the <Stop> button once to shut
down the microwave energy.
The program can be aborted at any time, pressure and temperature data
acquisition will be continued. To continue with the run, press the <Start> but-
ton.
2. To abort the program, press the <Stop> button twice.

The current run will be terminated and the safety cooling will be activated.
8.4.4.3 To Finish a Run
1. After the run has been finished, select from the menu on the display one of
the following options:
• Print: Print out a summary of the last run, including pressure and
temperature graphs, on a connected printer.
• Send: Transfer all relevant data of the last run to an external
computer via the serial interface.
• Review: View all relevant data of the last experiments on the graphic
display and allows to print them on a connected printer or send them
to an external computer.
• Next Run: Return to the sample menu to modify and/or restart the
current method.
2. Take the rotor out of the cavity and unload it as soon as practicable.
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8.4.5 Unloading Rotor 48
After the cooling has finished vent the pressure vessels under a fume hood prior
to opening. Follow these instructions to ensure safe and proper handling of the
vessels.
Warning:
Take safety precautions: Use goggles, protective gloves and lab coat.
Depending on the application, noxious gases may be released during the
venting procedure.
8.4.5.1 To Remove the p/T Sensor
1. Remove the rotor from the oven cavity and place it into a fume hood.
2. Turn the bayonet lid of the rotor counterclockwise to the stop position.
3. Carefully lift off the lid and place it with the top facing upwards on a clean
surface.
4. Remove the reference vessel with the p/T sensor from the rotor.
5. Unscrew the p/T sensor carefully in front of the supplied protection shield,
which is placed into a beaker. The beaker has to be filled with water to
absorb potential solvent drops.
The reaction gases are vented via venting grooves in the liner through the
vent pipe.
Warning:
Make sure that the vent pipe points away from your face!
Vent pipe
Fig. 8 - 14 Venting of the reference vessel
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6. Remove the vessel jacket and store it in a safe place.
7. Carefully loosen the liner.
Important:
Take care not to damage the immersion tube.
8. Place the sensor with the liner in a rack. If applicable, rinse the immersion
tube while removing it from the liner.
Fig. 8 - 15 Rinsing the immersion tube
8.4.5.2 To Vent and Open the Pressure Vessel
1. Vent each pressure vessel by opening the screw cap in front of the supplied
protection shield, which should be placed into a beaker.
Warning:
Make sure that the vessel points away from your face!
Vent pipe
correct incorrect
Fig. 8 - 16 Opening of the pressure vessel
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Warning:
Do not use any tool for opening the pressure vessel, even if the vessel cannot
be opened by hand due to a high residual pressure.
If so, let the vessel stand overnight and try to open it at the next day.
Do not force cooling of the vessel.
Reduce the sample amount during subsequent runs.
Hint:
If the reaction gases were not released via the venting system, the gases can
also escape safely via the venting grooves in the liner.
Venting grooves
Fig. 8 - 17 Venting grooves in the liner
2. Remove the vessel jacket and store it in a safe place or leave them in the
Rotor tray.
Warning:
Always open the vessel in a fume hood as noxious gases may be released.
Leakage may lead to chemical deposits on vessel or rotor parts.
3. Pop off the cap by pressing down on one side with your thumb to remove it
from the liner.
Fig. 8 - 18 Removing the cap from the liner
4. Put the liners into an appropriate rack (like Rack 24).
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8.5 Cleaning and Maintenance
For troublefree operation, thorough cleaning and maintenance procedures are

required. Even minor residues of corrosive reagents will lead to severe damages
during subsequent runs and therefore need to be removed.
In this chapter you will find information on how to clean and inspect the instrument
and the vessels after every reaction run, but also how to proceed after breakage
of a safety disk or vessel.
At the end of this chapter, you will find appropriate maintenance procedures for
the p/T sensor.
Important:
Proper cleaning and maintenance of all instrument parts, especially reaction
vessels and rotors, is vital to extend the service life and to ensure proper
functioning of the instrument.
Disregarding the instructions given in this chapter will lead to premature
failure and cost-intensive repairs.
8.5.1 Cleaning of the Reaction Vessels
The most effective cleaning procedure for reaction vessels is to perform a blank
reaction in Synthos 3000.
8.5.1.1 To Perform a Cleaning Run
1. Fill each vessel with at least 6 mL HNO3 (10%) or any cleaning solvent (ace-
tone, isopropanol etc.).
2. Select a cleaning program from the method library stored in Synthos 3000.
Instructions for handling and preparing the vessels and rotor are given in
chapter 8.4.4, "Performing a Synthesis Run".
3. Use the solvents for one cleaning cycle only.
4. If there are vacant positions during a reaction, these positions can be filled
up with “solvent blanks” for cleaning the vessels and seals.
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8.5.2 Cleaning After Every Run
Carefully clean the reaction vessels after every run to protect subsequent
samples against contamination, but also to avoid corrosion and overheating of the
vessel parts and rotor due to contamination with residues of reagents. This will
help to increase the service life of these parts.
Important:
Always let the parts dry completely before the next use. Do not use wet parts.
The evaporating water may lead to deformation of parts or may initiate local
overheating.
If you use a drying oven, do not exceed 80 °C.
Warning:
while cleaning the rotor, vessels and instrument.
8.5.2.1 To Clean the Vessel After Every Run
1. Rinse the liner thoroughly with deionized water and/or acetone.
2. Rinse the inner side of the seal thoroughly with deionized water and/or
acetone.
Fig. 8 - 19 Rinsing the seal
3. Remove any residues of reagents from the screw cap and the vessel jacket
with deionized water.
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4. When using different types of samples:

Perform a cleaning run (refer to chapter 8.5.1.1, "To Perform a Cleaning
Run") to avoid memory effects.
Hint:
You can alternatively clean the liners in a dishwasher.
5. Let all parts dry completely before the next use.
8.5.2.2 To Clean the p/T Sensor After Every Run
Important:
Do not wet the electronic module of the p/T sensor when cleaning the sensor.
1. Rinse the inner side of the seal thoroughly with deionized water and/or ace-
tone with the immersion tube facing downwards.
Fig. 8 - 20 Rinsing the seal of the p/T sensor
2. Carefully rinse the immersion tube with deionized water and/or acteone.
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3. If necessary, carefully remove solid residues from the immersion tube with a
acteone-damp cloth. Do not use sharp tools! Stubborn residues are removed
best during a run.
4. Remove any residues of reagents from the p/T sensor.
8.5.2.3 To Clean the Rotor After Every Run
1. Remove visible contaminations (e.g reagent spills) using a damp cloth.
8.5.2.4 To Clean the Instrument After Every Run
1. Wipe the interior of the microwave cavity and the safety door with a damp
cloth.
2. Clean the outer surfaces of Synthos 3000 with a damp cloth. Do not use
organic solvents!
Important:
If you detect any reagent residues at the bottom of the cavity, proceed with a
thorough inspection of your reaction vessels for signs of leakage.
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8.5.3 Checking After Every Run
Perform a visual check of the reaction vessels, rotor and instrument after every
experiment.
Important:
Replace damaged parts immediately! If not detected, even slight damages
may develop into cost-intensive repairs.
8.5.3.1 To Check the Vessels After Every Run
1. Check the liner for deformations and scratches in the sealing area.
Replace liners with a scratched sealing area (approx. 1 cm from the top), as
tightness during subsequent experiments is not ensured anymore.
2. Check the O-ring of the liner for damage. Replace corroded or worn O-rings.
3. Check the PEEK vessel jacket for any sign of cracks and corrosion.
4. Check the conical seal for any sign of damage, like deformation or cuts.
8.5.3.2 To Check the p/T Sensor After Every Run
1. Check the immersion tube for cracks or scratches.
2. Check the sealing lip of the lip-type seal for any sign of damage, e.g.
deformation or cuts.
3. Check the p/T sensor for oil leakage of the hydraulic system.
An oil leakage requires repair at Anton Paar, contact our local distributor.
Possible oil leaking elements
Fig. 8 - 22 Potential oil leakage from the hydraulic system on the p/T sensor
4. Check the seal husk for correct positioning.
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5. Proceed with Chapter 8.6, "Maintenance of the Pressure / Temperature

Sensor M50" if the p/T sensor shows any damages.
8.5.3.3 To Check the Rotor After Every Run
1. Check both the rotor body and the rotor tray for any obvious signs of dam-
age, e.g. melting of the rotor tray.
2. Check the alignment of the vessel holders.

If the reaction vessels are improperly aligned, IR measurement may provide
erroneous data.
Fig. 8 - 23 Proper alignment of the vessel holder
8.5.4 Standard Cleaning and Maintenance Procedures
Perform these combined cleaning and maintenance procedures after one or two
working weeks, depending on the operation frequency of Synthos 3000. If you
have to handle unknown sample material, perform these procedures daily.
Following these procedures will help to increase the service life of rotor and
vessel components, but will also reduce the risk of downtimes due to equipment
failure.
Important:
overheating.
Warning:
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8.5.4.1 To Clean and Check the Liner
1. Remove stubborn residues mechanically using water, a mild detergent and a

soft brush.
Be careful not to scratch the sealing surface of the liner (approx. 1 cm from
the top) in order to avoid leakage during subsequent runs. Do not use sharp
objects!
Alternatively: Clean the liners in an ultrasonic bath.
Fill the liner with reagent mixture to approx. 1 cm above the usual filling level
and place it in an ultrasonic bath for 10-15 minutes.
2. Rinse the liner thoroughly with deionized water and/or acteone.

Alternatively: Use a dishwasher to clean the liner.
3. Check the liner for any sign of damage, like deformations, cracks or
scratches of the sealing area.
Replace damaged liners immediately, as tightness during subsequent
experiments is not ensured anymore.
4. Perform a cleaning run to remove any detergent residues from the liner and
seal (refer to chapter 8.5.1.1, "To Perform a Cleaning Run").
Alternatively: Steam the liner with nitric acid vapors overnight using a
steaming apparatus. When doing so, remove the black O-ring from the
liner prior to steaming.
5. Store the liner in a dry and clean place.
Important:
Do not store the liner in the vessel jacket.
8.5.4.2 To Replace the O-Ring
1. Squeeze the top of the liner and push the O-ring slightly forwards.
Fig. 8 - 24 Pushing the O-ring forwards
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2. Scroll the O-ring with your finger and remove it.
Fig. 8 - 25 Remove the O-ring from the liner
3. Slip the new O-ring over the top of the liner until it fits into the groove of the
liner.
8.5.4.3 To Clean and Check the PEEK Vessel Jacket
1. Clean the vessel jacket with water, a mild detergent and a soft brush.
2. Thoroughly rinse with deionized water.
3. Let the vessel jacket dry completely before the next use.
4. Check the vessel jacket for any sign of damage, like cracks or chemical
attack (corrosion).
Replace PEEK vessel jackets immediately if you detect cracks or severe
material degradation.
8.5.4.4 To Clean and Check the p/T Sensor

Important:
1. Follow the instruction given in Chapter 8.5.2.2, "To Clean the p/T Sensor
After Every Run" and Chapter 8.5.3.2, "To Check the p/T Sensor After Every
Run".

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8.5.4.5 To Clean and Check the Rotor
• Follow the instructions given in Chapter 8.5.2.3 and Chapter 8.5.3.3.
8.5.4.6 To Clean and Check the Microwave Cavity
cloth.
organic solvents!
3. Clean the Fresnel lens of the IR sensor with a damp cotton bud.
Sensor for the protection lid detection Sensor for the position recognition
Fresnel lens of the IR sensor
Fig. 8 - 26 Cleaning the microwave cavity
4. Clean the sensors for the position recognition (at the bottom of the cavity)
and for the protection lid detection (at the right hand side of the cavity) with a
damp cotton bud.
5. Check the microwave cavity and safety door for any sign of damage or
deformation.
Warning:
Do not use the instrument if you detect any deformation on the microwave
cavity or the door. Danger of microwave leakage!
Contact an authorized service engineer.
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8.5.5 Procedures After the Rupture of a Safety Disk
If a safety disk breaks during the experiment (e.g. due to spontaneous reactions),
reagents usually escape from the reaction vessels. This leads to contamination of
the rotor, the outer surfaces of the vessels and the microwave cavity.
For this reason, extensive cleaning and checking is required.
Warning:
Let the safety cooling run for at least 60 minutes before removing the rotor
from the instrument. Refer to Chapter 3, "Safety Instructions".
while removing the rotor and cleaning the instrument.
8.5.5.1 Immediately After the Rupture of a Safety Disk
1. Let the safety cooling run for at least 60 minutes.

The safety cooling does not switch off automatically.
3. Carefully remove the rotor, place it under a fume hood, remove the rotor lid
and vent the vessels (refer to chapter 8.4.5.2, "To Vent and Open the
Pressure Vessel").
4. Take care for splinters and reagent residues.
5. Take out and open the reaction vessels (refer to chapter 8.4.5.2, "To Vent
and Open the Pressure Vessel"). It is most probable that the reaction was
incomplete, so you may discard the solutions.
Important:
After the breakage of a safety disk, both safety disk and conical seal have to
be replaced.
8.5.5.2 To Clean the Reaction Vessel
1. Clean all vessel parts thoroughly under running water. Use a mild detergent
and a soft brush if necessary.
2. Proceed with the standard cleaning and maintenance procedure (refer to

chapter 8.5.4.1, "To Clean and Check the Liner" and chapter 8.5.4.3, "To
Clean and Check the PEEK Vessel Jacket").
Pay special attention to a thorough check of all vessel parts. Immediately
replace damaged parts!
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8.5.5.3 To Disassemble the Screw Cap Assembly
For replacement of seal you have to disassemble the screw cap. Therefore you
will need the unlock disk and the seal forming device.
1. Thoroughly rinse the complete screw cap assembly under running water to
remove any reagent residues.
2. Place the unlock disk on the pressure vessel jacket (without liner).
Unlock Disk for seal
Fig. 8 - 27 Unlock Disk on the Pressure Vessel MF50
3. Compress the conical seal by closing the pressure vessel with the unlock
disk in place. Close it a half turn further than hand-tight.
4. Open the screw cap again and put in on a clean working bench.
5. Use the seal forming tool to push the seal out of the screw cap with the two
pins.
Seal Forming Tool M50
Fig. 8 - 28 Putting out the seal
6. Replace the defective parts (safety disk, seal and vent pipe).
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Fig. 8 - 29 Replacing the safety disk, seal and vent pipe
7. Clean the screw cap with water, a mild detergent and a soft brush. Remove
any deposits, especially from the inner side of the screw cap.
8.5.5.4 To Check the Screw Cap
1. Check the screw cap for any sign of corrosion.

A slightly yellowish discoloration inside the cap is normal due to acid vapors
and does not affect proper and safe functioning. Replace the screw cap if the
thread shows severe material degradation.
2. Check the screw cap for cracks.

Immediately replace the screw cap if you detect cracks in the thread of the
screw cap or around the seal.
3. Check the vent pipe for deformations.

Replace the vent pipe if it is deformed or damaged.
8.5.5.5 To Reassemble the Screw Cap Assembly
1. Insert the safety disk in the center of the screw cap. Take care that the safety
disk is positioned correctly.
Safety Disk M50

Screw Cap
Safety Disk
Fig. 8 - 30 Positioning of the safety disk
2. Put the vent pipe into the seal.
3. Put the assembled seal with the vent pipe on a liner with an O-ring.
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Seal M50 with the vent pipe
Liner with O-ring
Fig. 8 - 31 Liner with assembled Seal for Pressure Vessel MF50
4. Turn the liner upside down and push the seal into the screw cap until you
reach the locking position. Take care to immerse the vent pipe into the
appropriate borehole of the screw cap.
Fig. 8 - 32 Putting the seal into the screw cap
5. Use a pressure jacket to fix the seal by tightening the screw cap.
Fig. 8 - 33 Fixing the seal
6. Unscrew the vessel and check the correct (centered) position of the safety
disk.
7. Perform a blank run to clean the new seal.
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Important:
1. Follow the instruction given in Chapter 8.5.2.2 and Chapter 8.5.3.2.

1. Remove visible contaminations (e.g. reagent spills) with deionized water or

using a damp cloth.
2. If the rotor is strongly contaminated, a more thorough cleaning procedure,

including disassembly of the rotor, will be required. In such a case follow the
procedures described in Chapter 8.5.6.6, Chapter 8.5.6.7 and Chapter
8.5.6.8.
3. Let all parts dry completely before next use.
1. Remove the turntable, the drive star and the drive base from the microwave
cavity.
Turntable Drive Star Drive Base
Fig. 8 - 34 Disassembling the turntable, drive star and drive base
2. Clean these parts under running water, use a mild detergent and a soft brush
if necessary.
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3. Use a damp cloth to thoroughly clean the microwave cavity and the white
PTFE covers.
4. Clean the door in the same way, also the contacting surfaces between door
and instrument.
6. Clean the sensors for the position recognition and for the protection lid
detection in the same way.
7. Let all parts and surfaces dry completely.
8. Check the microwave cavity and door for signs of damage or deformation.
Warning:
9. Check all other parts for signs of damage, like cracks or fissures. Replace
damaged parts.
10. Reassemble the drive base, drive star and turntable.
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8.5.6 Procedures After a Vessel Explosion
Although very unlikely, it may happen that a reaction vessel breaks during a run
instead of the safety disk. This may be caused by spontaneous exothermal
reactions, which are too fast for the safety disk, or by previously damaged vessel
jackets.
In case of a vessel breakage, solvent and reagents will be released together with
vessel debris inside the microwave cavity. This leads to contamination of the rotor,
the outer surfaces of the vessels as well as the microwave cavity.
For this reason, an extensive cleaning and checking is required.
Warning:
from the instrument. Refer to chapter 3, "Safety Instructions".
Take care of splinters and reagent residues.
Warning:
After a vessel breakage you have to contact an authorized service engineer
who has to perform a microwave leakage test. Do not use the instrument
before it has passed this test successfully.
Due to the explosion either the door or the microwave cavity might have been
deformed. Danger of microwave radiation leakage!
8.5.6.1 Immediately After the Explosion

3. Carefully remove the rotor. Take care of splinters!
4. Place the rotor under a fume hood, remove the rotor lid and vent the vessels
(refer to chapter 8.4.5.2, "To Vent and Open the Pressure Vessel").
5. Take care for splinters and reagent residues.
6. Take out and open the reaction vessels (refer to chapter 8.4.5.2, "To Vent
and Open the Pressure Vessel"). It is most probable that the synthesis was
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and a soft brush if necessary.

chapter 8.5.4.3, "To Clean and Check the PEEK Vessel Jacket" and chapter
8.5.4.1, "To Clean and Check the Liner").
Important:
1. Follow the instruction given in chapter 8.5.2.2, "To Clean the p/T Sensor
After Every Run" and chapter 8.5.3.2, "To Check the p/T Sensor After Every
Run".

Carefully remove splinters and debris from the microwave cavity and follow the
instructions given in chapter 8.5.4.6, "To Clean and Check the Microwave Cavity".
Important:
After every vessel explosion contact an authorized service technician to
perform a microwave leakage test.
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8.5.6.5 To Clean the Exhaust Channel
1. Remove the safety bracket and the cover from the exhaust channel at the
rear of Synthos 3000 by loosening the two nuts.
1 2
3 4
Fig. 8 - 36 Removing the safety bracket from the exhaust channel
2. Remove the foam part.
Foam part
Fig. 8 - 37 Removing the foam part
3. Clean the inside of the exhaust channel with a damp cloth and remove all
debris and reagent residues.
4. Reinstall the foam part or replace it if it is considerably contaminated.
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Foam Part
Fig. 8 - 38 Exhaust channel with foam part
Hint:
The foam part has to be installed distorted approximately 10 cm into the
exhaust channel and is for noise reduction.
5. Reinstall the cover and the safety bracket at the exhaust channel.
6. Check the proper installation of the foam seal between tube and exhaust
unit.
Fig. 8 - 39 Checking the proper installation of the foam seal
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8.5.6.6 To Disassemble the Rotor
1. Disassemble the three interlock bolts by turning them counterclockwise.
Hint:
When disassembling the three interlock bolts the interlock ring drops down at
the bottom side of the rotor.
Interlock bolts
Interlock ring
Fig. 8 - 40 Disassembling the interlock bolts
2. Remove the rotor tray by loosening the 8 Allen screws.
Fig. 8 - 41 Removing the rotor tray
3. Remove the vessel holders from the rotor inner base ring of the rotor.
4. Pull off the 16 silicone seals, which are mounted on the bottom of the vessel
holders in the center circle.
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Silicone seal
Fig. 8 - 42 Silicone seal on the bottom of the vessel holder
Important:
Do not dismount the 8 white reflective stripes at the bottom of the rotor body.
Do not dismount the black rotor center ring at the base of the rotor body.
1. Clean all parts under running water. Use a mild detergent and a soft brush if
necessary.
2. Remove splinters.
3. Wipe off any reagent spills with a damp cloth.
4. Let all parts dry completely.
5. Check all parts for damages, especially vessel holders, silicone seals and
the rotor tray. Immediately replace damaged or broken parts!
8.5.6.8 To Reassemble the Rotor
1. Plug the 16 silicone seals onto the bottom of the vessel holders and check
for proper installation. Note that the 16 silicone seals are only fixed on those
vessel holders, which have to be installed in the center circle of the rotor
inner base ring.
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Silicone seal
Fig. 8 - 43 Installing the vessel holder in the center circle
2. Start the assembly by fixing the first vessel holder (with silicone seal) in the
center circle. The two feet of the vessel holders have to fit exactly into the
appropriate boreholes.
Take care that the bigger opening of the vessel holder faces in clockwise
direction.
Important:
If the vessel holders are not positioned correctly, heating and cooling behavior
of the rotor may be adversely affected.
3. Continue the assembly by fixing two vessel holders (without silicone seal) in
the outer and inner base ring to form a triple formation.
Fig. 8 - 44 Assembling the vessel holder in the rotor inner base ring (1)
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center circle
outer ring
inner ring
"triple formation"
Fig. 8 - 45 Assembling the vessel holder in the rotor inner base ring (2)
Hint:
The bigger openings of the three vessel holders belonging to one triple
formation have to show towards each other.
4. After completion of this triple formation, continue with the assembly of the
remaining vessel holders in the same sequence.
Fig. 8 - 46 Assembling the next vessel holder
Fig. 8 - 47 Installing the 48 vessel holders in the rotor tray
5. Make sure that all vessel holders are engaged properly in their positions.
6. Put the rotor tray onto the vessel holders. Take care that the position one on
the tray fits to the reflector mark on the rotor body.
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1 Position 1 on the tray
reflector mark on the

rotor body
Fig. 8 - 48 Correct positioning of the rotor tray
7. Insert the 8 Allen screws into their threads.
Fig. 8 - 49 Inserting of the Allen screw
8. When all vessel holders are positioned correctly, fix the rotor tray by pressing
it down with your fingers and screw in the 8 Allen screws. Do not overtighten
the Allen screws!
Fig. 8 - 50 Screw down the Rotor 48 Tray
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9. Finally screw in the 3 interlock bolts. For that reason tilt the rotor body a little
bit and insert the interlock ring into the recess until it rests on the rotor base.
Now turn the interlock ring until the three bore holes on the interlock ring
correspond with the three bore holes on the rotor tray.
Interlock Ring 48
Fig. 8 - 51 Inserting the interlock ring
Interlock Bolt
Interlock Ring
Fig. 8 - 52 Fixing the interlock bolts
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8.6 Maintenance of the Pressure / Temperature

Sensor M50
In the following chapters you will find information on how to replace the seal and
safety disk, capillary and immersion tube of the p/T sensor.
8.6.1 Replacing Seal and Safety Disk
After rupture of the safety disk you have to replace seal, seal husk and safety disk.
Losses of reagents or visible mechanical damage also indicate the necessity of
replacement.
Important:
When you replace the seal or remove it for cleaning, always replace the seal
husk! When removing and inserting the seal husk, do not use sharp objects,
which could damage it.
8.6.1.1 To Remove the Seal
1. Put the unlock disk for seal onto the pressure jacket.
Unlock disk for seal
Fig. 8 - 53 Pressure vessel with unlock disk
2. Compress the conical seal by closing the pressure vessel with the unlock
disk in place. Close it a half turn further than hand-tight.
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Fig. 8 - 54 p/T sensor
3. Open the p/T sensor again and put in on a clean working bench.
4. Use the seal ejector to push the seal out of the p/T sensor via the two pins
(through the two boreholes).
Press the seal ejector carefully down, do not bend the PEEK tube.
Seal ejector
Fig. 8 - 55 Using the seal ejector pin to push out the seal for p/T sensor
5. When the seal is loosen pull it off.
6. Remove the seal carefully by sliding to the end of the immersion tube. Avoid
any scratches on the immersion tube.
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Seal ejector
PEEK tube
PEEK tube,
do not bend!
Seal for p/T sensor
Fig. 8 - 56 Removing the lip-type seal from the p/T sensor
7. Remove the vent pipe by pushing it downwards.
Vent pipe
Fig. 8 - 57 Removing the vent pipe from the p/T sensor
8.6.1.2 To Install the Seal for p/T Sensor
1. Stick the vent pipe with the corresponding O-ring into the seal.
Seal for p/T Sensor M50
O-ring
Vent pipe p/T Sensor M50
Fig. 8 - 58 Vent pipe with O-ring on the lip-type seal
2. Push the assembled seal carefully upwards the immersion tube.
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3. Take care that the vent pipe fits exactly into the appropriate borehole of the
seal holder. Do not twist the seal to avoid bending of the vent pipe!
Push the seal further upwards to the seal holder by the help of a liner
(without O-ring).
Vent pipe p/T Sensor M50
Seal for p/T Sensor M50
Immersion Tube Sapphire p/T M50
Fig. 8 - 59 Moving lip-type seal for positioning the vent pipe
Liner without O-ring

Liner F50-PFA
Fig. 8 - 60 Fixing the seal for p/T sensor with the liner
4. Install the new seal husk using the supplied husk assembly tool.
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Seal husk
Husk assembly tool
Fig. 8 - 61 Pushing the seal husk onto the immersion tube using the husk
assembly tool
Important:
The two ends of the seal husk have different diameters. Put the new seal husk
onto the immersion tube so that the wider end faces to the screw cap. To
provide good sealing properties, the dimensions of the seal husk are chosen
to fit tightly. Use the special husk assembly tool to slide the seal husk up to the
stop position.
5. Make sure that the lip of the seal is not damaged during the assembly.
Important:
After exchanging the seal, always carry out a performance run before the first
reaction to check the tightness of the seal. To do this, weigh the solution
before and after a performance run and check for losses. If the losses are
higher than 2% check the installation steps of the seal husk once again.
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8.6.2 Replacing the Thermometer Capillary
To protect the capillary from damage during regular use it is surrounded by a

immersion tube and a strong PEEK protection sleeve. If the capillary is damaged
as a result of excessive mechanical stress it has to be replaced.
Follow these instructions to ensure safe and proper operation.
Important:
After replacing the thermometer capillary you have to calibrate the
temperature sensor! Refer to chapter 6.7.5, "Temperature Sensor
Calibration with the Calibration Unit".
Carry out the steps described below only if you are able to perform a
temperature sensor calibration!
The capillary is very fragile. The most critical part is the connection between
the capillary and glass bulb, which can easily break.
If you are not completely sure how to replace the thermometer capillary
consult our local customer service.
8.6.2.1 To Replace the Thermometer Capillary
1. Unscrew the knurled nut of the capillary tube.
2. Pull the knurled nut back (together with the PEEK sleeve of the capillary
tube) and take it out of the screw-type fitting.
Fig. 8 - 62 Unscrewing the knurled nut
3. The PEEK sleeve has to be separated from the immersion tube. Pull the
PEEK tube out of the metal sleeve which is positioned at the top of the
immersion tube. The use of a vice or pliers is recommended.
Fix the PEEK tube in the vice as shown below. Squeeze with the help of a
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screw driver the sensor from the PEEK sleeve. Take care not to damage the
immersion tube.
Vice
Screwdriver
Fig. 8 - 63 Pulling the PEEK tube out of the metal sleeve
4. Completely remove the used thermometer capillary by gently pulling it out of

the sensor.
Check the immersion tube for any signs of damage or loose residues of the
old capillary.
5. Insert the new capillary very carefully.

Take care when inserting the glass bulb. This is a sensitive part!
Glass bulb
Fig. 8 - 64 Inserting the capillary with the glass bulb
6. Insert the end of the PEEK tube into the metal sleeve up to the mechanical
stop position (3 - 4 mm) (with the help of a vice). The tube is automatically
fastened with a snap-in connector. Be very careful not to break the capillary.!
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Fig. 8 - 65 Inserting the PEEK tube
7. Mount the new knurled nut (delivered with the new capillary) onto the metal
end of the capillary tube so that the metal end protrudes from the nut for
2 mm.
2 mm
Fig. 8 - 66 Inserting the knurled nut
8. Place the p/T sensor on the edge of a table to keep one hand free for
manipulation of the capillary.
9. Pull back the knurled nut a bit and insert it into the fitting of the p/T sensor
unit without changing the protruding length of the metal end.
10. Close the knurled nut hand-tight and perform a temperature sensor
calibration with the calibration unit. (Refer to chapter 6.7.5, "Temperature
Sensor Calibration with the Calibration Unit".)
8.6.3 Replacing the Immersion Tube
To protect the thermometer capillary from damage during regular use it is

surrounded by a immersion tube and a strong PEEK protection sleeve. However,
also the immersion tube can be break as a result of excessive mechanical stress.
In this case, the capillary and/or glass bulb might break too and both parts need
to be replaced.
If the capillary is not damaged and should be used together with a new immersion
tube, take care not to break the capillary while disassembling.
Remove the capillary tube as described in Chapter 8.6.2.1, "To Replace the
Thermometer Capillary".
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For replacing the immersion tube, follow the instructions below to ensure safe and
proper operation.
Important:
After replacing the immersion tube you have to calibrate the temperature
sensor!
When you replace the immersion tube, you also have to replace the seal
husk. When removing and inserting the seal husk, do not use sharp objects,
8.6.3.1 To Replace the Immersion Tube
1. Unscrew the upper part (PEEK) of the immersion tube counterclockwise

(against the resistance of the FEP sealing husk).
Fig. 8 - 67 Unscrewing the upper part of the immersion tube
2. Pull out the defective immersion tube.

When removing the immersion tube from the p/T sensor the used seal husk
will also fall down at the inner side of the seal.
Fig. 8 - 68 Removing the immersion tube
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3. Check the surfaces of the p/T sensor for splinters and contaminated parts
and clean the surfaces with a moist cloth, if necessary.
Important:
Never clean the p/T sensor under running water as this may damage the
sensor electronics.
4. Insert a new immersion tube into the p/T sensor and tighten the immersion
tube by turning it clockwise. Take care not to damage the sealing area of the
immersion tube.
sealing area
Fig. 8 - 69 Inserting the new immersion tube
5. Install the new seal husk. Refer to chapter 8.6.1.2, "To Install the Seal for p/T
Sensor".
6. Take care when inserting the capillary with the glass bulb through the metal
sleeve into the immersion tube. Refer to chapter 8.6.2.1, "To Replace the
glass bulb
7. Perform a temperature sensor calibration (refer to chapter 6.7.5,

"Temperature Sensor Calibration with the Calibration Unit").
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9 Rotor 16MF100 / 16HF100

The following chapters contain a description of both Rotor 16MF100 and
Rotor 16HF100 and provide information on handling, cleaning and maintenance.
Fig. 9 - 1 Rotor 16MF100 or 16HF100
Rotor 16 is used for a wide selection of synthesis applications, utilizing pressures

and temperatures of up to 40 bar and 240 °C. It can be operated with up to 16
pressure vessels of the type MF100 or HF100.
9.1 Technical Description of Rotor 16
Rotor 16 consists of a rugged and microwave-transparent polymer construction.

The rotor tray, which is inserted into the rotor body, holds the reaction vessels and
provides guiding of the cooling air.
The rotor lid with a bayonet locking closes the rotor and provides protection in
case of a sudden overpressure release (e.g. rupture of a safety disk). Additionally,
the rotor lid serves as a rack to hold the liners before and after the reaction. The
positions are numbered to avoid mixing up of samples.
Openings on the side of the rotor lid facilitate venting of the reaction vessels after
reaction directly inside Synthos 3000, without the need of handling pressurized
reaction vessels.
Principle of rotation allows extremely homogeneous heating characteristics as

long as the recommended loading patterns (refer to chapter 9.3.3.1, "To Load the
Vessels into the Rotor") are adhered to.
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Reactions are controlled via IR temperature measurement in every position and/

or via the Pressure / Temperature Sensor Accessory (p/T sensor) located in one
reference vessel.
Important:
Never attempt to change the rotor geometry or to bring metal parts into the
microwave field. This will cause serious damage.
Rotor lid
Reaction vessels
Liner extractor bolt
Rotor tray
Rotor body
Fig. 9 - 2 Rotor 16
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9.1.1 Vessels for Rotor 16
Depending on the application, two different types of pressure vessels are

available. Both include proven features:
• Fluoropolymers for the reaction vessel and for the self-sealing lip-type seal
• Vessel jacket for providing mechanical stability
• An easy-to-handle screw cap with venting system
• Metal safety disk for overpressure protection
The high-performance and easy-to-handle pressure vessels come with the

following technical data:
MF100 HF100
Liner Material Fluoropolymer Fluoropolymer
Vessel Jacket PEEK Ceramic
Max. Operating Pressure 20 bar (290 psi) 40 bar (580 psi)
Opening Pressure 70 bar (1000 psi) 70 bar (1000 psi)
a 190 °C, for 30 min 240 °C
Max. TINTERNAL
b 160 °C 210 °C
Max. TIR
Nominal Volume 100 mL 100 mL
Min. Filling Volume 6 mL 6 mL
c 60 mL 60 mL
Max. Filling Volume
Typical Applications Parallel reactions, Parallel reactions,
multi-gram library gen- multi-gram library gen-
eration, solid-phase eration, solid-phase
synthesis synthesis
a. Temperature inside the reference vessel, measured via the p/T sensor
sensor
c. The max. filling volume may exceed 60 mL for special methods after
consulting Anton Paar GmbH
Important:
When using a total volume of less than 6 mL, the amount of liquid phase in the
reaction vessel will be too low to absorb microwave energy sufficiently. As a
result, microwave energy will couple directly to parts of the vessel, the rotor or
the sample. This may cause damage to components or may lead to self-
ignition and damage of the pressure vessel.
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Safety disk holder Syringe connector

with O-ring
Safety disk M&H

Venting screw
Screw cap
Seal
Liner fluoropolymer
Vessel jacket:
MF100: PEEK
HF100: ceramic
Fig. 9 - 3 Pressure vessel MF100 / HF100
Important:
The ceramic vessel jackets (HF100) have to be handled with care. Avoid any
mechanical impact on these vessel jackets, otherwise crack growth will
increasingly occur, thus drastically raising the probability of a vessel
breakage.
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If you are more familiar with microwave synthesis, you should also perform a
blank run to clean the liner and seal (refer to Chapter 9.4.1.1, "To Perform a
Cleaning Run").

Important:
Always take care to select the appropriate vessel type in the method.
The maximum operating pressure and temperature values are defined within
the method.
Do not use both types of pressure vessel (MF100 and HF100) together!
9.2.1 To Prepare the First Run

the software (refer to chapter 6.6, "Setting Up the Instrument").
Hint:
Before the first reaction remove the test certificates from the ceramic vessel
jackets. Keep these test certificates with the other instrument documents.
2. Select either a cleaning or a performance method ("PQ MF" or "PQ HF",

depending on the used vessel type) from the method library.
3. When doing a performance method, prepare acidified water (10 mL water

and 100 µL of conc. nitric acid per vessel). Using this mixture will allow you
also to check the functioning of the pressure and temperature sensors.
Important:
Do not use deionized water due to the possible super-boiling effect, which
may result in a vessel explosion.
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9.3 Performing a Synthesis
This chapter provides the required information on how to perform a synthesis

reaction correctly. Follow these instructions to ensure safe and proper operation.
Warning:
Important:
Before the first experiment read chapter 11, "Applications" very carefully.
Do not fill less than 6 mL of sample and reagent into the vessel.
Performing a synthesis reaction consists mainly of the following steps:

• Venting the pressure vessels and unloading the rotor after the reaction
Guidelines for reagent mixtures are given in the method library of Synthos 3000.
Depending on possibly different reaction behavior of your reagent, the suggested
reagent mixture may have to be modified. The user is responsible for this
decision.
Important:
The use of the p/T sensor is highly recommended to thoroughly observe the
reaction.
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1. Weigh in the compounds into the liner.

Take care that no residues are sticking on the sealing area of the liner.
Take care that no residues are sticking on

the sealing area!
Fig. 9 - 4 Residues sticking on the sealing area
2. Add solvent.
Rinse the liner by adding the solvent to remove any material sticking on the
top of the liner wall. Make sure that no deposits remain on the wall of the
vessel.
9.3.2 Assembling the Vessels
The vessel is closed with a screw cap containing a self-sealing lip-type seal made
of PTFE-TFM. Due to the pressure build-up during the heating phase, the sealing
lip is pressed against the liner wall, thus providing tight closure of the vessel.
The seal is a sensitive part. To ensure proper functioning and to avoid losses of
reagents or analytes, the seal has to be handled carefully as described below.
Important:
Take care when handling and storing the seal! The sealing lip can be
damaged easily.
ensured any longer. As a consequence, damage to the instrument, rotor and
vessels may occur due to escaping reagents.
Never store the seal standing on its sealing lip!
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incorrect correct
Fig. 9 - 5 Incorrect and correct storage of the seals
The sealing lip has to be expanded shortly before use. To do so, you can use
either the seal forming tool or the optional seal forming device.
Important:
Do not start a run without having the seals properly expanded. In such a case
tightness of the vessel is not ensured any longer. As a consequence, damage
to the instrument, rotor and vessels may occur due to escaping reagents.
Seal forming tool
Seal forming device
Fig. 9 - 6 Seal forming tool and seal forming device
The seal forming device is used for the simultaneous expansion of 8 seals and for
safe storage. The sensitive sealing lip is protected and the working life of the seal
is extended. The design of the seal forming device allows you to expand and store
all types of seals for Rotor 16 and Rotor 8S.
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9.3.2.1 To Use the Seal Forming Tool
1. Press the screw cap completely onto the seal forming tool for at least 3 sec-
onds to expand the sealing lip. Expand new seals for at least 10 seconds.
Fig. 9 - 7 Handling the seal forming tool
2. Immediately close the pressure vessel (refer to chapter 9.3.2.3, "To Close
the Pressure Vessel").
Note that the seal will regain its original shape after some time, therefore you
have to start the reaction within approx. 15 minutes. Otherwise, re-expand
the seal.
3. Proceed with the p/T sensor in the same way.
Fig. 9 - 8 Expanding the seal of the p/T sensor
Important:
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9.3.2.2 To Use the Seal Forming Device
1. Ensure that the cones are mounted properly on both the intermediate panel
and the upper panel, depending on the seal type.
To form MF and HF seals, the longer, smaller cone must protrude upwards
from the panel. The seals are expanded by the shorter, bigger cone.
Fig. 9 - 9 Properly mounted cones for expanding of MF and HF seals (left)
2. Place four screw caps into the recesses of the lower panel with the seal
facing upwards.
Fig. 9 - 10 Placing the first screw caps into the seal forming device
3. Take the intermediate panel and carefully place it onto the seals.
Fig. 9 - 11 Placing the intermediate panel on the seal forming tool
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Important:
The cones have to fit exactly into the seals. Take care not to place the cones
onto the sealing lips, as this will damage the seals.
Check for correct positioning of the seals.
4. Place another four screw caps into the recesses of the intermediate panel.
5. Put the upper panel on the seals.

Make sure that it is placed properly. The words “THIS SIDE UP” must be
visible on the top.
This side up
Fig. 9 - 12 Putting the upper panel on the seals
correct
incorrect
Fig. 9 - 13 Correct and incorrect positioned screw caps
6. Tighten the handwheel clockwise until you feel resistance.

The seals remain inside the device until their next use.
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Correct Incorrect
Fig. 9 - 14 Correct and incorrect closing of the handwheel
7. To remove the seals, perform the steps previously described in reverse

order.
Immediately close the pressure vessel (refer to chapter 9.3.2.3, "To Close
the Pressure Vessel"). Additional forming with the seal forming tool is not
necessary.
1. Remove any solvent or reagent droplets from the vessel jacket and the outer
surface of the liner.
Important:
Take care that all vessel parts (liner, vessel jackets, screw caps) are
completely dry. Any residues of liquid between the liner and vessel jacket may
cause damage to the vessel.
3. Close the venting screw on the screw cap finger-tight.
Fig. 9 - 15 Closing the venting screw
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Important:
Close the venting screw finger-tight only without using a tool.
The supplied key is used for opening only. The tight closure during reaction is
ensured via the front side of the white PTFE-plug of the venting screw.
Fig. 9 - 16 Venting screw in closed position: The front side of the PTFE-plug
seals the outlet opening
4. Carefully apply the screw cap to the vessel.

Make sure that the seal of the screw cap has been expanded shortly before
and is inserted exactly into the liner.
Fig. 9 - 17 Closing the pressure vessel of Rotor 16
5. Close the screw cap by hand in clockwise direction until you reach the stop
position.
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9.3.2.4 To Apply the p/T Sensor
1. Remove any solvent or reagent droplets from the vessel jacket and the outer
3. Close the venting screw finger-tight.
Fig. 9 - 18 Closing the venting screw of the p/T sensor
Important:
4. Carefully apply the p/T sensor to the vessel.

Make sure that the seal of the sensor has been expanded (refer to chapter
9.3.2.1, "To Use the Seal Forming Tool") and is inserted exactly into the liner.
Take care that there are no residues between the lip and sealing area.
Important:
5. Close the screw cap by hand in clockwise direction until you reach the stop
position.
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Fig. 9 - 19 Closing the reference vessel with the p/T sensor
Important:
Be careful when inserting the immersion tube of the p/T sensor, especially if a
magnetic stir bar and/or a heating element is used. The immersion tube may
break!
6. For correct pressure measurement, reopen the screw cap for approx. 45°!
45°
Fig. 9 - 20 Reopening the p/T senor accessory of Rotor 16
Hint:
The seal of the p/T sensor is connected to the hydraulic system and thus
slightly movable. For correct pressure measurement in the reference vessel,
its screw cap has to be reopened from the stop position for approx. 45°. This
is equivalent to 1.5 ribs on the screw cap.
If the screw cap is not reopened properly, pressure will be applied already by
the vessel jacket. As a consequence, the pressure readout will not show the
correct reaction pressure inside the reference vessel.
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9.3.3 Loading Rotor 16
The following procedures describe how to load the reaction vessels into the rotor
and how to close and insert the rotor into Synthos 3000.

Important:
the method.
Do not use both types of pressure vessel (MF100 and HF100) together!
1. If applicable: Insert the reference vessel into position 1.
2. Place the other vessels into the rotor with the venting screws facing outward,
following the recommended loading patterns.
To ensure uniform temperature distribution during the reaction, the rotor has
to be loaded symmetrically. The recommended load patterns ensure uniform
heating of all vessels.
Venting screw
Fig. 9 - 21 Inserted vessels in Rotor 16
3. Reduce the max. power in the method when using less than 16 vessels. As a
guideline, limit the max. power output to 800 W (8 vessels) or 400-600 W
(4 vessels), respectively.
1400 W 800 W 400-600 W
Fig. 9 - 22 Recommended load patterns of Rotor 16
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4. If you have other numbers than the recommended ones to be processed, fill
the vacant positions pure solvent to obtain a symmetrical load pattern.
Important:
Never use less than 4 vessels to avoid overheating of rotor or vessel parts!
1. Put the protection lid on the rotor body.

Align the arrow on the outer side of the rotor lid with the word "OPEN" of the
rotor body.
close
Fig. 9 - 23 Closing Rotor 16
2. Rotate the lid clockwise until the arrow points to the word "CLOSE".
The bayonet locking is now engaged.
microwave cavity. The synthesis run is started from the software menu.
Synthos 3000 controls all parameters automatically and usually does not require
user intervention.
At the end of an experiment, the cooling starts automatically. The safety cooling
is also activated automatically if a run is aborted. The cooling is stopped as soon
as all vessels have cooled down to an internal temperature below 60 °C and an
IR temperature below 50 °C, depending on the installed sensors.
Warning:
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2. To put the loaded rotor into the microwave cavity, hold it with both hands at
Fig. 9 - 24 Placing the rotor into the microwave cavity

5. Start the experiment by pressing the green <Start> button after the system
reaction progress.
1. To interrupt (pause) the experiment, press the <Stop> button once to shut
ton.

The current run will be terminated and the safety cooling function will be
activated.
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• Review: View all relevant data of the last experiments on the

graphic display and allows to print them on a connected printer or
send them to an external computer.
current method.
9.3.5 Unloading Rotor 16
After the cooling has finished either vent the pressure vessels inside the
instrument or remove the rotor and vent the vessels under a fume hood.
Warning:
venting procedure.
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Important:
You must not open the venting screw completely, one turn counter clockwise is
sufficient!
The residual pressure is released via the syringe connector by opening a

connecting channel between venting screw and syringe connector. As soon as
the connecting channel is opened, all gases are released via the syringe
connector.
O-ring seals the exhaust pathway
Fig. 9 - 25 Correct maximum opening position: The O-ring seals the exhaust
pathway
When you open the venting screw for more than one turn the O-ring does not
seal anymore. The gases are additionally released via spaces between O-ring
and the thread of the venting screw. This may result in corrosion of the venting
screw and other parts of the seal holder.
O-ring does not seal the

exhaust pathway
Fig. 9 - 26 Incorrect opening position: The O-ring cannot seal the exhaust
pathway anymore
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9.3.5.1 To Vent Inside the Instrument
Warning:
1. Open the door of Synthos 3000 after the cooling has been finished. A pop-up
window will appear on the graphic display.
2. Select fan intensity.
3. Slowly open each venting screw through the rotor lid with the supplied key
until you hear the noise of releasing gases. Do not open the venting screw
for more than 1 turn!
Supplied key
Fig. 9 - 27 Venting the vessels inside the microwave cavity
4. Close the door and wait a few minutes for the released gases to be drawn
off.
5. Switch off the exhaust unit, remove the rotor from the oven cavity and place
it into a fume hood.
7. Lift off the lid and place it with the top facing upwards on a clean surface. You
may use the holes in the lid as a rack for the liners and screw caps later on.
8. Proceed with chapter 9.3.5.3, "To Open the Pressure Vessel".
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9.3.5.2 To Vent Under a Fume Hood
Warning:
Alternatively, you can vent the vessels after removing the rotor lid.
Supplied key
Fig. 9 - 28 Venting the vessels under the fume hood
may use the holes in the lid as a rack for the liners and screw caps later on.
5. Wait a few minutes for the released gases to be drawn off.
6. Proceed with chapter 9.3.5.3, "To Open the Pressure Vessel".
9.3.5.3 To Open the Pressure Vessel
1. Make sure that all vessels have been vented.
Hint:
also escape safely via the venting grooves in the liner.
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2. Carefully unscrew the vessels.
Warning:
Always open the vessel in a fume hood as noxious gases may be released.
Leakage may lead to chemical deposits on vessel or rotor parts.
3. Put the liners (with the screw caps) into an appropriate rack (like Rack 16) or
into the corresponding openings of the rotor lid. The openings are numbered
to avoid mixing up the samples.
4. If the liner is stuck in the vessel jacket, use the liner extractor bolt on the rotor
tray to push the liner out of the vessel jacket.
Liner
extractor bolt
Fig. 9 - 29 Using the liner extractor bolt
5. Store the vessel jackets in a safe place, e.g. Rack 16.
Important:
The ceramic vessel jackets have to be handled with care. Avoid any
mechanical impact on these parts.
Inappropriate storage of ceramic vessels, like putting them loosely into a

drawer, will drastically decrease the service life of these parts and increase
the probability of vessel breakage.
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and the vessels after every run, but also how to proceed after breakage of a safety
disk or vessel.
Additionally, you will find the description of an intensive cleaning procedure for
ceramic vessels, which should be performed on a regular basis.
the p/T sensor.
Important:
The most effective cleaning procedure for reaction vessels is to perform the
corresponding cleaning run in Synthos 3000.
tone, isopropanol).
3. Use the solvents only for one cleaning cycle.
4. If there are vacant positions during a synthesis, these positions can be filled
up with “solvent blanks”.
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Carefully clean the reaction vessels after every experiment to protect subsequent
vessel parts and rotor due to contamination with residues of reagents. This will
help to increase the service life of these parts.
Important:
overheating.
Warning:
9.4.2.1 To Clean the Vessels After Every Run
1. Rinse the liner thoroughly with deionized water and /or acetone.
2. Rinse the inner side of the seal thoroughly with deionized water and /or
acetone.
Fig. 9 - 30 Rinsing the seal
3. Remove any residues of reagents from the screw cap and if necessary rinse
the vessel jacket with deionized water and /or acetone. If required,
disassemble the screw cap completely (refer to chapter 9.4.4.2, "To
Disassemble the Screw Cap Assembly").

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Hint:
6. Keep the venting screws open (max. 1 turn) during storage to increase the
service life of both the seal and the venting screw.
9.4.2.2 To Clean the p/T Sensor After Every Run
Important:
tone.
2. Carefully rinse the immersion tube with deionized water and/or acetone.
Fig. 9 - 31 Rinsing the seal and the immersion tube
damp cloth. Do not use sharp tools! Stubborn residues are removed best
during a cleaning run.
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4. Remove any residues of reagents from the screw cap.
6. Keep the venting screw of the p/T sensor open (max. 1 turn) during storage
to increase the service life of both the seal and the venting screw.
1. Remove visible contaminations (e.g reagent spills) with deionized water or

using a damp cloth. Check the inner side of the rotor lid for reagent residues,
which might be due to the venting procedure.
cloth.
organic solvents.
Important:
reaction run.
Important:
1. Check the liner for scratches in the sealing area.

Replace liners with a scratched sealing area, as tightness during subsequent
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2. Depending on the type of reaction vessels, check the PEEK or ceramic

vessel jackets, respectively, for any sign of cracks and corrosion.
Damaged PEEK vessel

jacket
New PEEK vessel jacket
Fig. 9 - 32 Inspection of the PEEK vessel jacket
Cracks in the ceramic vessel

jacket
Fig. 9 - 33 Inspection of the ceramic vessel jacket
3. Check the sealing lip of the lip-type seal for any sign of damage, like
Fig. 9 - 34 Damaged sealing lip
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9.4.3.2 To Check the p/T Sensor After Every Run
3. Check the p/T sensor for oil leakage of the hydraulic system.
Potential oil leakage
Fig. 9 - 35 Potential oil leakage from the hydraulic system on the p/T sensor
4. Check the seal husk for correct positioning.
5. Proceed with chapter 9.5, "Maintenance of the Pressure / Temperature

Sensor Accessory" if the p/T sensor shows any damages.
9.4.3.3 To Check the Rotor After Every Reaction
1. Check both the rotor body and the rotor tray for any obvious sign of damage,
e.g. melting of the rotor tray.

erroneous data.
correct incorrect
Fig. 9 - 36 Alignment of the vessel holder
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failure.
Important:
overheating.
Warning:

soft brush.
Be careful not to scratch the sealing surface of the liner in order to avoid
leakage during subsequent runs. Do not use sharp objects!
Alternatively: Clean the liners in an ultrasonic bath.

Alternatively: Use a dishwasher for cleaning the liner.
Replace damaged liners immediately, as tightness during subsequent
experiment is not ensured anymore.
seal. Refer to chapter 9.4.1.1, "To Perform a Cleaning Run".
steaming apparatus.
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Important:
Do not store the liner in the vessel jacket. Acid residues may diffuse from the
liner material and lead to corrosion and subsequent damage of the vessel
jackets.
9.4.4.2 To Disassemble the Screw Cap Assembly
1. Thoroughly rinse the complete screw cap assembly under running water to
2. Remove the venting screw.
Venting screw
Fig. 9 - 37 Unscrewing the venting screw
3. Use the reverse side of the venting screw to unscrew the syringe connector.
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Syringe connector
Fig. 9 - 38 Unscrewing the syringe connector
4. Remove the seal and place it with the sealing lip facing upwards.
Important:
Do not mix up the seals and venting screws. Always keep the seal and its
venting screw in pairs.
Fig. 9 - 39 Removing the seal
5. Unscrew the safety disk holder using an appropriate screwdriver.
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Fig. 9 - 40 Unscrewing the safety disk holder
6. Remove the safety disk.
9.4.4.3 To Clean the Screw Cap Assembly
1. Clean the screw cap with water, a mild detergent and a soft brush. Remove
any deposits, especially from the inner side of the screw cap and from the
thread for the venting screw.
2. Thoroughly clean the thread of the venting screw. Take care not to damage
the O-ring.
3. Carefully remove any deposits from the seal, then rinse thoroughly with
deionized water.
Important:
Avoid any damage to the lip-type seal.
4. Clean all other parts (syringe connector, safety disk and safety disk holder)
thoroughly under running water, then rinse with deionized water. You may
use a mild detergent and a soft brush if necessary.
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9.4.4.4 To Check the Screw Cap
1. Check the screw cap for any sign of corrosion.

A slightly brownish discoloration inside the cap is normal due to acid vapors
and does not affect proper and safe functioning. Replace the screw cap if the
thread shows severe material degradation.
2. Check the screw cap for cracks.

Immediately replace the screw cap if you detect cracks in the thread of the
screw cap or around the seal.
Corroded thread
Crack
REPLACE!
Fig. 9 - 41 Corroded screw cap with a crack
3. Check the thread for the venting screw.

Remove any deposits from the thread before replacing the venting screw. If
the venting screw is not running smoothly anymore, replacement of the
venting screw alone will not restore proper functioning.
Corrosion!
Replace!
Fig. 9 - 42 Checking the thread for the venting screw
Hint:
Before replacing the venting screw, cleaning the thread using a screw cap is
recommended. An appropriate screw tap is available on request.
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9.4.4.5 To Check the Venting Screw
1. Check the O-ring of the venting screw.

Replace the venting screw if the O-ring is deformed or damaged.
Venting screw without damages

Damaged O-ring
Corroded thread
Fig. 9 - 43 Checking the O-ring of the venting screw
2. Check the thread of the venting screw. Replace the venting screw if the
thread is severely corroded or if it is not running smoothly.
9.4.4.6 To Check the Seal
1. Check the sealing lip for any sign of damages, like deformation or cuts.
A defective sealing lip does not ensure proper tightening of the reaction ves-
sels anymore. Replace damaged seals immediately to avoid cost-intensive
repairs.
Hint:
Avoid damage of the lip-type seal during storage by using the optional seal
forming device.
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Sealing lip damaged
Sealing lip ok
Damaged seals
Fig. 9 - 44 Checking the sealing lip for any damages
2. Check the spot where the safety disk is located.

Replace the seal if this spot is pressed out. In this case also check the safety
disk for damage and replace if necessary.
Seal OK Damaged seal
Fig. 9 - 45 Checking seals
Hint:
When replacing the seal, also replace the venting screw as well, otherwise
tightness of the reaction vessels may not be ensured.
Do not use new seals with old venting screws!
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9.4.4.7 To Check the Safety Disk
1. Check the safety disk for signs of corrosion.

Slight discoloration does not affect proper functioning of the safety disk.
Replace considerably corroded safety disks.
2. Check the safety disk for deformation.

A slight bulge is normal. Replace the safety disk if the bars start to break
already.
New safety disk Slightly bulged safety Opened safety disk,

disk, O.K. not O.K.
Fig. 9 - 46 Safety Disk M & H
9.4.4.8 To Reassemble the Screw Cap Assembly
1. Insert the safety disk into the screw cap with the label "M&H" facing out-
wards. Take care that the safety disk is positioned correctly. The holes in the
safety disk have to form a "C".
Fig. 9 - 47 Correct positioning of the safety disk
Important:
After the breakage of a safety disk, both safety disk and seal have to be
replaced. Also replace the venting screw. Do not use an old venting screw
together with a new seal to avoid leakiness.
2. Fix the safety disk by screwing-in the safety disk holder.
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Fig. 9 - 48 Fixing the safety disk with the safety disk holder
3. Insert the seal into the screw cap and fix it with the syringe connector and the
venting screw.
Venting screw
Syringe connector
Fig. 9 - 49 Reassembling the screw cap assembly
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9.4.4.9 To Clean and Check the PEEK Vessel Jacket (MF100)
1. Clean the vessel jacket with water, a mild detergent and a soft brush.
2. Thoroughly rinse with deionized water.
4. Check the vessel jacket for any sign of damage, like small cracks or
chemical attack.
A yellowish discoloration does not necessarily affect proper functioning, but it
is a strong indication for attack by acid vapors and therefore requires a
thorough inspection. Replace PEEK vessel jackets immediately if you detect
cracks or severe material degradation.
Damaged PEEK vessel

jacket
New PEEK vessel jacket
Fig. 9 - 50 Damaged and new PEEK vessel jacket
9.4.4.10 To Clean and Check the Ceramic Vessel Jacket (HF100)
1. Rinse the vessel jacket thoroughly with deionized water. Do not use any
detergents, as they might affect the heating behavior of these parts!
3. Check the vessel jacket for any sign of damage, like cracks or chipping.
Discoloration or chipping are indications for improper usage and for
significantly decreased mechanical strength of the vessel jacket. Do not use
such a vessel jacket unless it has been tested by Anton Paar.
4. For a more thorough cleaning procedure, refer to chapter 9.4.7, "Intensive

Cleaning of Ceramic Vessels".
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Important:
Run".

• Follow the instructions given in chapter 9.4.2.3, "To Clean the Rotor After
Every Run" and chapter 9.4.3.3, "To Check the Rotor After Every Reaction".
To clean and check the rotor follow the instructions given in chapter 9.4.5.4, "To
Clean and Check the Microwave Cavity".
9.4.5 Procedures After the Breakage of a Safety Disk
Warning:
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9.4.5.1 Immediately After the Breakage of a Safety Disk

3. Carefully remove the rotor, place it under a fume hood and vent the vessels
(refer to chapter 9.3.5.2, "To Vent Under a Fume Hood").
4. Remove the rotor lid. Take care for splinters and reagent residues.
5. Take out and open the reaction vessels (refer to chapter 9.3.5.3, "To Open
the Pressure Vessel"). It is most probable that the synthesis was incomplete,
so you may discard the solutions.
Important:
replaced.
(except for the ceramic vessel jackets) and a soft brush if necessary.

chapter 9.4.4, "Standard Cleaning and Maintenance Procedures").
Hint:
After breakage of a safety disk the liner might be deformed due to the rapid
pressure loss.
If the sealing area (approx. 2 cm from the top) is not affected, such a
deformed liner can be reshaped by performing a cleaning run.
Replace the liner if the deformation has affected also the sealing area.
Deformation
Fig. 9 - 51 Deformed liner
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If the safety disk of the p/T sensor breaks during the experiment, follow the
instructions given in chapter 9.5.1, "Replacing Seal and Safety Disk".
Important:
Run".

Sensor Accessory" if the safety disk of the p/T sensor has been broken or if
the sensor shows any damages.
cavity.
Fig. 9 - 52 Disassembling the turntable drive star and drive base
if necessary.
PTFE covers.
and instrument.
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Warning:
damaged parts.
reactions, which are too fast for the safety disk, or by previously damaged vessel
jackets.
Synthos 3000 is equipped with numerous safety features, which ensure that the
laboratory personnel is safely protected in case of such an incident.
In case of a vessel breakage, solvent and reagents will be released together with
vessel debris inside the microwave cavity. This leads to contamination of the rotor,
the outer surfaces of the vessels as well as the microwave cavity.
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Warning:
Take care of splinters and reagent residues.
Warning:

3. Carefully remove the rotor. Take care of splinters, especially when using
ceramic vessels!
4. Place the rotor under a fume hood and vent the vessels (refer to chapter
9.3.5.2, "To Vent Under a Fume Hood").
6. Take out and open the reaction vessels (refer to chapter 9.3.5.3, "To Open
the Pressure Vessel"). It is most probable that the synthesis was incomplete,
so you may discard the solutions.
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Hint:
If you are not sure if the ceramic vessel jackets (Rotor 16HF) have been
damaged during the explosion, you may send them to Anton Paar for
inspection.

Important:
Run".

To clean and check the microwave cavity, follow the instruction given in chapter
9.4.5.4, "To Clean and Check the Microwave Cavity".
To clean the exhaust unit, follow the instructions given in chapter 8.5.6.5, "To
Clean the Exhaust Channel".
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1. After all vessels have been removed and cleaned, remove the rotor tray. Pay
attention to any splinters and reagent deposits.
Fig. 9 - 54 Removing the rotor tray
2. Pull off the silicone seals from the lower end of the vessel holders.
Silicone seal
Fig. 9 - 55 Silicone seal on the bottom of the vessel holder
3. Remove the positioning ring.
Fig. 9 - 56 Removing the positioning ring
4. Remove the vessel holders if the rotor tray or vessel holders have been
damaged.
To do so, grip the vessel holder by the three tongues, which protrude from
the rotor tray and press them together. Push the vessel holder down and
remove it from the rotor tray.
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Fig. 9 - 57 Removing the vessel holder
Important:
Do not dismount the black rotor center ring at the base of the rotor body.
9.4.6.7 To Clean the Rotor
1. Clean all parts under running water. Use a mild detergent and a soft brush if
necessary.
2. If necessary wipe off any traces of non-digested sample material with a piece
of cloth moistened with isopropyl alcohol.
3. Let all parts dry completely. Take special care that the space between the
black center ring and the rotor body is dried completely. It is recommended to
use pressurized air for drying.
1. Replace damaged or broken parts.
2. Install the vessel holders into the rotor tray.

One of the three tongues has a small mark, which must point towards the
center of the rotor. Insert the three tongues from below into the rotor tray until
they engage.
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Fig. 9 - 58 Installing the vessel holder
3. Assemble the positioning ring on the lower side of the rotor tray.
Fig. 9 - 59 Putting the positioning ring onto the vessel holder
4. Plug the 16 silicone seals onto the base of the vessel holders and check for
proper installation. The silicone seal has to snap in completely. Defective
silicone seals can lead to incorrect IR measurement.
Silicone seal
Fig. 9 - 60 Putting the silicone seals onto the vessel holders
5. Put the assembled rotor tray into the rotor body.

The guide pin on the outer side of the rotor tray (between vessel position "1"
and "2") must engage into the appropriate recess in the rotor body.
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Fig. 9 - 61 Alignment of the rotor tray in the rotor body
Important:
erroneous data.
correct incorrect
Fig. 9 - 62 Correct and incorrect alignment of the rotor tray
9.4.7 Intensive Cleaning of Ceramic Vessels
Perform this procedure if the divergence between maximum and minimum IR

temperature values during a run starts to increase, although all vessels are
loaded identically with the same amount of solvent and reagents. The reason for
these divergences are contaminations of the vessel jacket or liner, which are not
removed by standard cleaning procedures.
The essential part of this procedure consists of a heating step. After a few pre-
cleaning steps, the ceramic vessel jackets and liners are heated to 250 °C for
several hours to reduce the amount of contaminations and to restore the original
operation behavior.
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9.4.7.1 To Clean the Ceramic Vessel Jacket and the Liner
1. Remove any visible impurities from the ceramic vessel jacket and the liner
with water, a mild detergent and a soft brush.
Hint:
Any sample residues or visible impurities, which are not removed thoroughly
before the heating step, will leave unsightly residues, which can be hardly
removed afterwards.
Alternatively: You may use a dishwasher for cleaning the liner, but not for
cleaning the ceramic vessel jacket.
2. Thoroughly rinse with distilled water.
3. If necessary, perform a cleaning run to remove any sample residues from the
liner. Take care that all parts have been dried completely before the run.
4. Place the ceramic vessel jacket and the liner into a drying furnace and heat
all parts for at least 4 hours at 250 °C.
Hint:
If you have to run this procedure at a reduced temperature (min. 200 °C),
extend the heating time (e.g. overnight). The efficiency of this procedure
decreases with lower temperature.
5. After the heating step is completed, let the vessel jacket and liner SLOWLY
cool down inside the oven (max. 100 °C/h).
Important:
Do not try to speed up the cooling process. This will cause severe damage to
the ceramic vessel jackets.
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9.5 Maintenance of the Pressure / Temperature

Sensor Accessory
In the following chapters you will find information on how to replace the seal and
safety disk, capillary and immersion tube of the p/T sensor.
9.5.1 Replacing Seal and Safety Disk
replacement.
Important:
When you replace the seal or remove it for cleaning, always replace the seal
husk! When removing and inserting the seal husk, do not use sharp objects,
Warning:
1. Remove the venting screw from the screw cap.
Fig. 9 - 63 Removing the venting screw
2. Use the reverse side of the venting screw as tool for unscrewing the syringe
connector.
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Syringe connector
3. Insert a flat screwdriver into the aperture of the syringe connector and
carefully lever the seal holder with the seal out of the screw cap as far as
possible.
Important:
Be careful not to scratch the immersion tube!
Seal holder
Fig. 9 - 65 Removing the seal holder with seal
4. Take the seal carefully without damaging its lip and slide the seal to the end
of the immersion tube. During this process do not tilt the seal to avoid
breakage of the immersion tube.
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Seal holder
Fig. 9 - 66 Disassembling seal holder with seal
5. Check the threads of the seal holder (especially the thread for the venting
screw) for any sign of corrosion or cracks. A damaged seal holder has to be
replaced immediately!
6. Check the inner side of the screw cap for any sign of corrosion or cracks. A
damaged screw cap has to be replaced immediately!
7. Remove the seal husk, which is located at the middle of the seal.
Seal husk
Fig. 9 - 67 Seal husk and seal
9.5.1.2 To Replace the Safety Disk
1. Remove the seal holder as described in chapter 9.5.1.1, "To Remove the
Seal".
2. Screw out the safety disk holder with an appropriate screwdriver or a similar
tool.
Fig. 9 - 68 Screwing out the safety disk holder
C49IB08A 257
9 Rotor 16MF100 / 16HF100
3. Remove the used safety disk.
4. Insert the safety disk into the screw cap with the label "M&H" facing
outwards. Take care that the safety disk is positioned correctly. The holes in
the safety disk have to form a "C".
Fig. 9 - 69 Positioning the safety disk
Important:
9.5.1.3 To Install the Seal
1. Mount the seal holder with the assembled safety disk and the seal onto the
immersion tube and push it into the screw cap to the stop position. Turn the
seal until the chamfered side fits to the inner side of the seal holder. Take
care not to damage the lip of the seal. It is recommended to use a liner to
push the seal into the seal holder.
Fig. 9 - 70 Reassembling the seal holder
2. Check that the openings for the syringe connector and venting screw
correspond to the openings in the screw cap. If necessary, turn the seal
holder until the boreholes face to the openings of the screw cap.
C49IB08A 258
9 Rotor 16MF100 / 16HF100
3. Fix the seal in the screw cap with the syringe connector and the venting
screw. Completely close the venting screw, then reopen it for one turn during
storage.
4. Push the new seal husk onto the immersion tube using the husk assembly
tool.
Important:
onto the immersion tube so that the wider end faces the screw cap. To provide
good sealing properties, the dimensions of the seal husk are chosen to fit
tightly. Use the special husk assembly tool (plastic tube) to slide the seal husk
up to the final stop position.
Seal husk Husk assembly tool
assembly tool
Important:
Never use sharp objects to push the seal husk onto the immersion tube.
Make sure that the seal is not damaged during assembly.
Important:
After replacing the seal, always carry out a performance run before the next
reaction to check the tightness of the seal. Weigh the solution before and after
the performance run and check for losses. If the losses are higher than 2%,
check the tightness of the seal and seal husk once again.
C49IB08A 259
9 Rotor 16MF100 / 16HF100
To protect the capillary from damage during regular use it is surrounded by a

immersion tube and a strong PEEK protection sleeve. If the capillary is damaged
as a result of excessive mechanical stress it has to be replaced.
Follow these instructions to ensure safe and proper operation.
Important:
Calibration with the Calibration Accessory" or to chapter 6.7.5,
"Temperature Sensor Calibration with the Calibration Unit".
Carry out the steps described below only if you are able to perform a
temperature sensor calibration!
1. Unscrew the knurled nut of the capillary tube.
2. Pull the knurled nut back (together with the PEEK sleeve of the capillary
tube) and take it out of the screw-type fitting.
knurled nut
Fig. 9 - 72 Unscrewing the knurled nut.
3. The PEEK sleeve has to be separated from the immersion tube. Pull the
PEEK tube out of the metal sleeve which is positioned at the top of the
immersion tube. The use of a vice or pliers is recommended.
C49IB08A 260
9 Rotor 16MF100 / 16HF100
Fig. 9 - 73 Pulling the PEEK tube with capillary out of the metal sleeve
4. Completely remove the used thermometer capillary by gently pulling it out of

the sensor.
Check the immersion tube for any signs of damage or loose residues of the
old capillary.
5. Insert the new capillary very carefully into the immersion tube.
Take care when inserting the glass bulb. This is a sensitive part!
6. Insert the end of the PEEK tube into the metal sleeve up to the mechanical
stop position (3 - 4mm) (with the help of a vice). The sleeve is automatically
fastened with a snap-in connector. The tube is automatically fastened with a
snap-in connector. Be very careful not to break the capillary!
C49IB08A 261
9 Rotor 16MF100 / 16HF100
Fig. 9 - 75 Inserting the PEEK tube
7. Mount the new knurled nut (delivered with the new capillary) onto the metal
end of the capillary tube so that the metal end protrudes from the nut for
2 mm.
2 mm
Knurled nut
8. Place the p/T sensor on the edge of a table to keep one hand free for
manipulation of the capillary.
9. Pull back the knurled nut a bit and insert it into the fitting of the p/T sensor
unit without changing the protruding length of the metal end.
10. Close the knurled nut hand-tight and perform a temperature sensor
calibration with the calibration accessory (refer to chapter 6.7.4,
"Temperature Sensor Calibration with the Calibration Accessory") or with the
calibration unit (refer to chapter 6.7.5, "Temperature Sensor Calibration with
the Calibration Unit").
C49IB08A 262
9 Rotor 16MF100 / 16HF100
9.5.3 Replacing the Immersion Tube
To protect the thermometer capillary from damage during regular use it is

surrounded by a immersion tube and a strong PEEK protection sleeve. However,
also the immersion tube can be break as a result of excessive mechanical stress.
In this case, the capillary and/or glass bulb might break too and both parts need
to be replaced.
If the capillary is not damaged and should be used together with a new immersion
tube, take care not to break the capillary while disassembling.
Remove the capillary tube as described in Chapter 9.5.2.1, "To Replace the
For replacing the immersion tube, follow the instructions below to ensure safe and
proper operation.
Important:
After replacing the immersion tube you have to calibrate the temperature
sensor!
When you replace the immersion tube, you also have to replace the seal
husk. When removing and inserting the seal husk, do not use sharp objects,
9.5.3.1 To Replace the Immersion Tube
1. Unscrew the upper part (PEEK) of the immersion tube counterclockwise

(against the resistance of the FEP sealing husk).
Fig. 9 - 77 Unscrewing the upper part of the immersion tube
2. Pull out the defective immersion tube.

When removing the immersion tube from the p/T sensor the used seal husk
will also fall down at the inner side of the seal.
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9 Rotor 16MF100 / 16HF100
3. Check the surfaces of the p/T sensor for splinters and contaminated parts
and clean the surface with a damp cloth, if necessary.
Important:
Never clean the p/T sensor under running water as this may damage the
sensor electronics.
4. Insert a new immersion tube into the p/T sensor and tighten the immersion
tube by turning it clockwise. Take care not to damage the sealing area of the
immersion tube.
sealing area
Fig. 9 - 78 Inserting the new immersion tube
5. Install the new seal husk. Refer to chapter 9.5.1.3, "To Install the Seal".
6. Take care when inserting the capillary with the glass bulb through the metal
sleeve into the immersion tube. Refer to chapter 9.5.2.1, "To Replace the
7. Perform a temperature sensor calibration with the calibration accessory

(refer to chapter 6.7.4, "Temperature Sensor Calibration with the Calibration
Accessory") or with the calibration unit (refer to chapter 6.7.5,
"Temperature Sensor Calibration with the Calibration Unit").
C49IB08A 264
10 Rotor 8SXF100 / 8SXQ80

The following chapters contain a description of both Rotor 8SXF100 and
Rotor 8SXQ80 and provide information on handling, cleaning and maintenance.
Fig. 10 - 1 Rotor 8SXF100 / 8SXQ80
Rotor 8S is used for a wide selection of applications, enabling pressures and

temperatures of up to 80 bar and 300 °C. It can be operated with up to 8 pressure
vessels of the type XF100 or XQ80.
10.1 Technical Description of Rotor 8S
Rotor 8S consists of a sophisticated metal construction, allowing to perform and

control microwave-assisted reactions up to 300 °C and 80 bar simultaneously.
The rotor upper plate made of aluminum contains a unique, patented hydraulic
pressure sensor for simultaneous measurement of all 8 vessels with wireless data
transmission to the oven.
The rotor can be closed easily by the fastening screws and a multifunctional
bayonet lid combined with a safety closure by a bolt. The lid serves as a protection
shield in case of a sudden overpressure release (e.g. rupture of a safety disk).
Additionally, the rotor lid serves as a rack for up to 8 vessels after the reaction.
The positions are numbered to avoid mixing up of samples.
Openings on the side of the rotor lid facilitate venting of the reaction vessels after
reaction directly inside Synthos 3000, without the need of handling pressurized
reaction vessels.
C49IB08A 265
Principle of rotation allows extremely homogeneous heating characteristics as

long as the recommended loading patterns (refer to chapter 10.3.3.1, "To Load
the Vessels into the Rotor") are adhered to.
Reactions are controlled via IR temperature measurement and via pressure

sensor in every position. Additionally, a T-probe can be used in one reference
vessel.
Important:
Never attempt to change the rotor geometry or to bring other metal parts into
the microwave field. This will cause serious damage.
Rotor 8S lid
Rotor upper plate 8S

(assembled)
Fastening screw
assembled
Pressure vessel XF100

or XQ80
Bottom guard
Bottom load ring
Fig. 10 - 2 Rotor 8S
C49IB08A 266
10.1.1 Vessels for Rotor 8S
Depending on the application, two different types of pressure vessels are

available:
• A reaction vessel made of fluoropolymer and supported by a ceramic vessel
jacket is suitable for most types of high pressure applications.
• A massive quartz vessel provides highest pressure and temperature stability
for the most demanding applications.
Both include proven features:

• Self-sealing lip-type seal, made of fluoropolymer
• Easy-to-handle seal holder with venting system
• Metal safety disk for overpressure protection
Important:
The quartz vessels and the ceramic vessel jackets have to be handled with
care. Avoid any mechanical impact on these parts, as this might raise the
probability of a vessel breakage.
The resultant high-performance and easy-to-handle pressure vessels come with

the following technical data:
XF100 XQ80
Liner Material Fluoropolymer ---------
Vessel Jacket Ceramic Quartz glass
Max. Operating Pressure 60 bar (870 psi) 80 bar (1160 psi)
Opening Pressure 120 bar (1740 psi) 120 bar (1740 psi)
a 260 °C 300 °C
Max. TINTERNAL
b 240 °C 280 °C
Max. TIR
Nominal Volume 100 mL 80 mL
Min. Filling Volume 6 mL 6 mL
cMax. Filling Volume 60 mL 60 mL
Typical Applications Parallel scale-up, prepressurized
prepressurized reactions, "Green
reactions Chemistry" approach,
near critical water
chemistry
a. Temperature inside the reference vessel, measured via the T-probe
sensor
c. The max. filling volume may exceed 60 mL for special methods after
consulting Anton Paar GmbH
C49IB08A 267
Important:
When using a volume of less than 6 mL, the amount of liquid phase in the
reaction vessel will be too low to absorb microwave energy sufficiently. As a
result, microwave energy will couple directly to parts of the vessel, the rotor or
the sample. This may cause damage to rotor components or pressure
vessels.
Protective cap
Syringe connector with
O-ring
Safety disk holder "X"
Venting screw
Safety disk "X"
Seal holder X
Seal for M+H+XF
Liner fluoropolymer
Vessel jacket ceramics
Center ring
Protective casing with

base plate
Fig. 10 - 3 Pressure vessel XF100
C49IB08A 268
Protective cap
Syringe connector with
O-ring
Safety disk holder "X"
Venting screw
Safety disk "X"
Seal holder X
Seal for XQ
Quartz vessel XQ80
Center ring
Protective casing with

base plate
Fig. 10 - 4 Pressure vessel XQ80
C49IB08A 269
If you are more familiar with microwave synthesis, you should also perform a
blank run to clean the liner and seal (refer to chapter 10.4.1.1, "To Perform a
Cleaning Run").

Important:
the method.
Do not use both types of pressure vessel (XF100 and XQ80) together!
10.2.1 To Prepare the First Run

the software (refer to chapter 6.6, "Setting Up the Instrument").
Hint:
Before the first reaction remove the test certificates from the ceramic vessel
jackets or the quartz glass vessels, respectively. Keep these test certificates
with the other instrument documents.
2. Select either a cleaning or a performance method ("PQ XF" or "PQ XQ",

depending on the used vessel type) from the method library.
3. When doing a performance method, prepare acidified water (10 mL water

and 100 µL of conc. nitric acid per vessel). Using this mixture will allow you
also to check the functioning of the pressure and temperature sensors.
Important:
Do not use deionized water due to the possible super-boiling effect, which
may result in a vessel explosion.
C49IB08A 270
10.3 Performing a Synthesis
This chapter provides the required information on how to perform a synthesis

correctly. Follow these instructions to ensure safe and proper operation.
Warning:
Important:
Before the first experiment read chapter 11, "Applications" very carefully.
Performing a microwave synthesis consists mainly of the following steps:

• Venting the pressure vessels and unloading the rotor after the reaction
Guidelines for reagent mixtures are given in the method library of Synthos 3000.
Depending on a possibly different reaction behavior of your reagents, the
suggested mixture may have to be modified. The user is responsible for this
decision.
1. Weigh in the reagents into the liner / quartz glass vessel.

Take care that no residues are sticking on the sealing area of the liner /
quartz glass vessel.
C49IB08A 271
Take care that no residues are sticking on

the sealing area!
Fig. 10 - 5 Residues sticking on the sealing area
2. Add solvent.
Rinse the liner / quartz glass vessel by adding the solvent to remove sample
material sticking on the top of the liner wall / quartz glass vessel wall. Make
sure that no deposits remain on the wall of the vessel.
10.3.2 Assembling the Vessels
The vessel is closed with a seal holder containing a self-sealing lip-type seal
made of PTFE-TFM. Due to the pressure build-up during the heating phase, the
sealing lip is pressed against the liner wall / quartz glass vessel wall, thus
providing tight closure of the vessel.
The seal is a sensitive part. To ensure proper functioning and to avoid losses of
reagents, the seal has to be handled carefully as described below.
Important:
Take care when handling and storing the seal! The sealing lip can be
damaged easily.
ensured any longer. As a consequence, damage to the instrument, rotor and
vessels may occur due to escaping solvents.
Never store the seal standing on its sealing lip!
Starting a run without properly expanded seals may damage the seals.
C49IB08A 272
incorrect
incorrect correct
correct
Fig. 10 - 6 Incorrect and correct storage of the seals
The sealing lip has to be expanded shortly before use. To do so, you can use
either the seal forming tool or the optional seal forming device.
Seal forming tool Seal forming device
Fig. 10 - 7 Expanding the sealing lip
The seal forming device is used for the simultaneous expansion of 8 seals and for
safe storage. The sensitive sealing lip is protected and the working life of the seal
is extended. The design of the seal forming device allows you to expand and store
all types of seals for Rotor 16, Rotor 16 SOLV and Rotor 8S.
10.3.2.1 To Use the Seal Forming Tool
1. Press the seal holder with seal completely onto the seal forming tool for at
least 3 seconds to expand the sealing lip. Expand new seals for at least 10
seconds.
Seal forming tool for Rotor 8S
Fig. 10 - 8 Handling the seal forming tool
C49IB08A 273
2. Immediately close the pressure vessel (refer to chapter 10.3.2.3, "To Close
the Pressure Vessel").
Note that the seal will regain its original shape after some time, therefore you
have to start the reaction within approx. 15 minutes. Otherwise, re-expand
the seal.
3. If applicable: proceed with the immersion tube in the same way (see also
chapter 10.3.3.2, "To Apply the T-Probe").
Fig. 10 - 9 Expanding the seal with the immersion tube (XF100 / XQ80)
Important:
Make sure not to damage the immersion tube when handling the seal forming
tool.
10.3.2.2 To Use the Seal Forming Device
1. Ensure that the cones are mounted properly on both the intermediate panel
and the upper panel, depending on the seal type.
To expand XF seals, the longer, smaller cone must protrude upwards from
the panel. To expand XQ seals, the shorter, bigger cone must protrude
upwards from the panel.
C49IB08A 274
Expanding of XF seals Expanding of XQ seals
Fig. 10 - 10 Properly mounted cones for expanding of XF seals (left) and XQ

seals (right)
2. Place four seal holders with seal into the recesses of the lower panel with the
seal facing upwards.
Fig. 10 - 11 Placing the first four seal holders into the seal forming device
Hint:
After a reaction, rinse the seals thoroughly with acetone and allow them to dry
before placing them into the seal forming device.
3. Take the intermediate panel and carefully place it onto the seals.
Important:
The cones have to fit exactly into the seals. Take care not to place the cones
onto the sealing lips, as this will damage the seals.
Check for correct positioning of the seals.
C49IB08A 275
Fig. 10 - 12 Placing the intermediate on the seal forming tool
4. Place another four seal holders into the recesses of the intermediate panel.
Fig. 10 - 13 Placing the next four seal holders into the seal forming device
5. Put the upper panel on the seals.

Make sure that it is placed properly. The words “THIS SIDE UP” must be
visible on the top.
This side up
Fig. 10 - 14 Putting the upper panel on the seals
6. Check for correct positioning of the seals.
C49IB08A 276
This side up
Fig. 10 - 15 Closing the seal forming device
7. Tighten the handwheel clockwise until you feel resistance.

The seals remain inside the device until their next use.
Correct Incorrect
Fig. 10 - 16 Correct and incorrect closing of the handwheel
Important:
The seal XQ is expanded too much when closing the seal forming device
hand tight. For this reason it is necessary to tighten the handwheel clockwise
until you feel resistance but then reopen it approximately 180° (1/2 turn)
otherwise the XQ seals will be deformed and damaged.
8. To remove the seals, perform the steps previously described in reverse

order.
Immediately close the liner or the quartz glass vessel with the seal holder
(refer to chapter 10.3.2.3, "To Close the Pressure Vessel"). Additional
forming with the seal forming tool is not necessary.
C49IB08A 277
1. Remove any droplets from the vessel jacket and the outer surface of the liner
or from the quartz glass vessel.
Important:
Take care that all vessel parts (liner, vessel jackets, quartz vessels, seal
holder assemblies) are completely dry. Any residues of liquid between the
liner and vessel jacket may cause damage to the vessel.
2. Close the venting screw on the seal holder finger-tight.
Fig. 10 - 17 Closing the venting screw
Important:
Fig. 10 - 18 Venting screw in closed position: The front side of the PTFE-plug
seals the outlet opening
3. Close the liner or the quartz glass vessel with the seal holder.
Make sure that the seal of the seal holder has been expanded shortly before
and is inserted exactly into the liner or the quartz glass vessel.
C49IB08A 278
4. XF: Put the liner with the seal holder into the vessel jacket and place it into
the protective casing so that the venting screw rests on the strap of the
protective casing.
XQ: Place the quartz glass vessel with the seal holder into the protective
casing so that the venting screw rests on the strap of the protective casing.
5. Put the protective cap onto the protective casing. The distance between the
cap and the casing should not exceed 2 mm.
Seal holder
Liner
Ceramic vessel
Protective casing
Distance between
cap and vessel holder
less than 2 mm
Fig. 10 - 19 Assembling the pressure vessel of Rotor 8S
10.3.2.4 To Close the Reference Vessel
1. Remove any droplets from the vessel jacket and the outer surface of the liner
or from the quartz glass vessel. Liquid residues between liner and vessel
jacket or on the quartz glass vessel may cause overheating and damage to
the reaction vessel!
2. Close the venting screw on the seal holder finger-tight.
Important:
C49IB08A 279
3. Close the liner or the quartz glass vessel with the immersion tube with seal.
Make sure that the seal of the immersion tube has been expanded shortly
before and is inserted exactly into the liner or the quartz glass vessel.
Fig. 10 - 20 Expanding the immersion tube with seal
4. XF: Put the liner with the seal holder into the vessel jacket and place it into
the protective casing so that the venting screw rests on the strap of the
protective casing.
XQ: Place the quartz glass vessel into the protective casing so that the
venting screw rests on the strap of the protective casing.
5. Put the protective cap onto the protective casing. The distance between the
cap and the casing should not exceed 2 mm.
Hole for the T-probe
Fig. 10 - 21 Closing the reference vessel
C49IB08A 280
10.3.3 Loading Rotor 8S
The following procedures describe how to load the reaction vessels into the rotor,
the use of the T-probe and how to close and insert the rotor into Synthos 3000.
1. Put the vessels into the assigned rotor positions with the venting screws fac-
ing outwards. The vessels have to engage into position.
Important:
Take care that the vessels are positioned properly, otherwise there could
arise serious damages to the vessels and rotor during reaction. Additionally
incorrect positioning may lead to erroneous pressure values.
Fig. 10 - 22 Inserting vessels in Rotor 8S
Important:
Load Rotor 8S with 4 or 8 vessels only for proper functioning.
To ensure accurate pressure measurement during the process the rotor has
to be loaded symmetrically.
Reduce the max. power in the method when using less than 8 vessels. As a
guideline, limit the max. power output to 800 W for 4 vessels.
If you have less than 4 or 8 samples to be processed, fill the vacant positions
with blank solvent.
C49IB08A 281
1400 W 800 W
Fig. 10 - 23 Load patterns of Rotor 8S
2. When using the T-probe:

Insert the reference vessel (equipped with immersion tube with seal) into
position 1.
Insert the glass rod through the opening of the rotor upper plate into the
borehole of the reference vessel.
glass rod
Fig. 10 - 24 Inserting the glass rod
3. To close the rotor, screw down the rotor upper plate (with the glass rod, if
applicable) until the vessels are fixed.
Important:
The initial pressure of Rotor 8S has to be between 2 and 10 bar. If the
pressure is out of this range reassamble the rotor.
C49IB08A 282
Fig. 10 - 25 Screwing down the upper plate of Rotor 8S
4. Check all vessels for proper positioning and correct centering.
Correct! Incorrect!
Fig. 10 - 26 Correct and incorrect positioning of the vessel
10.3.3.2 To Apply the T-Probe
1. Before inserting the T-probe into the reference vessel, use the glass rod to
make sure that the vessel is positioned correctly. If there is any resistance
when inserting the rod, adjust the vessel positioning and try it again. Repeat
the procedure until you feel no resistance when inserting the rod.
Important:
Do not introduce the T-probe until the above test was successful, otherwise
the capillary of the T-probe may break when inserted into the vessel.
2. Remove the glass rod.
3. Insert the T-probe very carefully through the hole of the upper plate of the
rotor into the vessel at position 1.
C49IB08A 283
Important:
The torus-shaped part of the T-probe is placed on the central rotor sensor
module.
The arm of the T-probe has to fit exactly into the recesses of the fastening
screws of the rotor upper plate.
Never insert the T-probe unless the rotor top plate is correctly fixed. The glass
bulb and the capillary may break!
1. Put the rotor lid on the rotor so that the top of the fastening screws protrude
through the holes in the lid.
Fig. 10 - 28 Closing Rotor 8S with the protection lid
2. Close the rotor by turning the lid clockwise until you reach the stop position.
C49IB08A 284
Important:
The locking button near the “Warning” symbol must engage.
"Warning" symbol
Locking button
Fig. 10 - 29 Closed Rotor 8S
microwave cavity. The run is started from the software menu. Synthos 3000
controls all parameters automatically and usually does not require user
intervention.
At the end of a run, the cooling starts automatically. The safety cooling is also
activated automatically if a run is aborted. The cooling is stopped as soon as all
vessels have cooled down to an internal temperature below 60 °C and an IR
temperature below 50 °C, depending on the installed sensors.
Warning:
2. Put the loaded rotor into the microwave cavity.

To put the loaded rotor into the microwave cavity, hold it with both hands at
C49IB08A 285
Fig. 10 - 30 Placing the rotor into the microwave cavity

5. Start the program by pressing the green <Start> button after the system
reaction progress.
1. To interrupt (pause) the program, press the <Stop> button once to shut
ton.

The current reaction run will be terminated and the safety cooling function
will be activated.

C49IB08A 286
• Review: View all relevant data of the last experiments on the

graphic display and allows to print them on a connected printer or
send them to an external computer.
current method.
10.3.5 Unloading Rotor 8S
After the cooling has finished either vent the pressure vessels inside the
instrument or remove the rotor and vent the vessels under a fume hood.
Warning:
venting procedure.
C49IB08A 287
Important:
You must not open the venting screw completely, one turn counter clockwise is
sufficient!
The residual pressure is released via the syringe connector by opening a

connecting channel between venting screw and syringe connector. As soon as
the connecting channel is opened, all gases are released via the syringe
connector.
O-ring seals the exhaust pathway
Fig. 10 - 31 Correct maximum opening position: The O-ring seals the exhaust
pathway
When you open the venting screw for more than one turn the O-ring does not
seal anymore. The gases are additionally released via spaces between O-ring
and the thread of the venting screw. This may result in corrosion of the venting
screw and other parts of the seal holder.
O-ring does not seal the

exhaust pathway
Fig. 10 - 32 Incorrect opening position: The O-ring cannot seal the exhaust
pathway anymore
C49IB08A 288
10.3.5.1 To Vent Inside the Instrument
1. Open the door of Synthos 3000 after the cooling has been finished. A pop-up
window will appear on the graphic display.
2. Select fan intensity.
Venting with the

supplied key
Fig. 10 - 33 Venting inside the instrument
4. Close the door and wait a few minutes for the released gases to be drawn
off.
5. Switch off the exhaust unit, remove the rotor from the oven cavity and place
it into a fume hood.
may use the holes in the lid as a rack for the liners and seal holders.
8. Proceed with chapter 10.3.5.3, "To Remove the T-Probe".
10.3.5.2 To Vent Under a Fume Hood
Warning:
Take care of hot and pressurized vessels after removing the rotor from the
oven cavity!
Alternatively, you can vent the vessels after removing the rotor lid.
C49IB08A 289
Venting with the

supplied key
either with or
without the rotor
lid
Fig. 10 - 34 Venting the vessels under the fume hood
3. Press the locking button and turn the bayonet lid of the rotor
counterclockwise to the stop position.
Fig. 10 - 35 Opening the rotor lid
4. Carefully lift off the lid and place it with the top facing upwards on a clean
surface. You may use the holes in the lid as a rack for the liners and seal
holders later on.
5. Wait a few minutes for the released gases to be drawn off.
10.3.5.3 To Remove the T-Probe
1. If a T-probe was used, carefully remove it before opening the rotor fastening
screws. Hold the T-probe by the sensor head and sensor arm and pull the
unit carefully straight upwards out of the vessel.
Important:
Do not take out the reference vessel until the T-probe has been removed.
Otherwise the capillary of the T-probe will be damaged.
C49IB08A 290
Fig. 10 - 36 Removing the T-probe
2. Store the T-probe in a safe place.
10.3.5.4 To Open the Pressure Vessel
1. Make sure that all vessels have been vented.
Hint:
also escape safely via the venting grooves in the liner of XF vessels.
Warning:
Always open the vessels in a fume hood as noxious gases may be released.
2. Open the rotor fastening screws slowly until all vessels can be removed
easily!
3. Take the vessels out of the rotor and place them nearby.
C49IB08A 291
Fig. 10 - 37 Taking the vessels out of the rotor
4. Remove the protective cap.
5. When using XQ vessels:

Remove the quartz glass vessels from the protective casing and put them in
an appropriate rack, like Rack 16. Alternatively, leave them in the protective
casing.
6. When using XF vessels:

Remove the vessel jacket from the protective casing and remove the liner
from the vessel jacket. If the liner is stuck in the vessel jacket, use the liner
extractor bolt on the rotor tray to push the liner out of the vessel jacket.
Fig. 10 - 38 Using the liner extractor bolt
7. Put the vessel jacket back into the protective casing.
8. Put the liners (with the seal holder) into an appropriate rack (like Rack 16) or
into the corresponding openings of the rotor lid. The openings are numbered
to avoid mixing up the samples.
C49IB08A 292
Fig. 10 - 39 Liner and seals in the openings of the rotor lid
Important:
Both the ceramic vessel jackets and the quartz glass vessels have to be
handled with care. Avoid any mechanical impact on these parts, like hitting
them together.
Inappropriate storage of ceramic and quartz vessels, like putting them loosely
into a drawer, will drastically decrease the service life of these parts and
increase the probability of vessel breakage.
C49IB08A 293

and the vessels after every run, but also how to proceed after breakage of a safety
disk or vessel.
Additionally, you will find the description of an intensive cleaning procedure for
ceramic vessels, which should be be performed on a regular basis.
the T-probe and the immersion tube with seal.
Important:
Important:
Only clean the quartz glass vessels with a soft brush, never use metal parts or
tools, respectively. Try to avoid using mechanical force as this could damage
the vessels by causing scratches. Never use damaged or scratched vessels
for reactions, as the pressure resistance is not longer guaranteed.
The most effective cleaning procedure for reaction vessels is to perform a blank
run in Synthos 3000.
tone, isopropanol etc.).
Refer to chapter 6.4, "Library Menu".
3. Use the solvents only for one cleaning cycle.
4. If there are vacant positions during a run, these positions can be filled up
with blank solvent.
C49IB08A 294
Carefully clean the reaction vessels after every experiment to protect subsequent
vessel parts and rotor due to contamination with residues reagents. This will help
to increase the service life of these parts.
Important:
overheating.
Warning:
10.4.2.1 To Clean the Vessels After Every Run
1. Rinse both liner and quartz glass vessel thoroughly with deionized water
and/or acetone.
2. Rinse the inner side of the seal thoroughly with deionized water and/or
acetone.
Fig. 10 - 40 Rinsing the seal with deionized water
3. Remove any residues of reagents from the seal holder and the vessel jacket
with deionized water. If necessary, disassemble the seal holder completely
(refer to chapter 10.4.4.4, "To Disassemble the Seal Holder Assembly").

C49IB08A 295
Hint:
6. Keep the venting screws open (max. 1 turn) during storage to increase the
service life of both the seal and the venting screw.
10.4.2.2 To Clean the Immersion Tube with Seal After Every Run
tone.
Fig. 10 - 41 Rinsing the inner side of the seal
2. Carefully rinse the immersion tube with deionized water and/or acetone.
C49IB08A 296
damp cloth. Do not use sharp tools! Stubborn residues are removed best
during a cleaning run.
Important:
If the immersion tube is removed from the seal by mistake, the seal husk has
to be replaced.
4. Remove any residues of reagents from the seal holder.
1. Remove visible contaminations (e.g reagent spills) with a damp cloth. Never
rinse Rotor 8S with running water. Check the inner side of the rotor lid for
reagent residues, which might be due to the venting procedure.
cloth.
organic solvents!
Important:
experiment.
Important:
C49IB08A 297
1. Check the liner for scratches in the sealing area.

Replace liners with a scratched sealing area, as tightness during subsequent
2. Check the quartz glass vessel for any sign of damage, like cracks, scratches
or blurred surfaces. Check for any sign of devitrification. Replace damaged
parts, alternatively send them to our local customer service for inspection.
Chipped-off quartz
glass vessel
Replace
immediately!
Fig. 10 - 43 Inspection of the quartz glass vessel
3. Check the ceramic vessel jacket for cracks.
Cracks in the ceramic vessel

jacket
Fig. 10 - 44 Inspection of the ceramic vessel jacket
4. Check the sealing lip of the lip-type seal for any sign of damage, like
C49IB08A 298
Fig. 10 - 45 Damaged sealing lips
10.4.3.2 To Check the Immersion Tube with Seal After Every Run
3. Check the seal husk for any sign of damage and for correct positioning.
4. Proceed with chapter 10.5, "Maintenance of the T-Probe and the Immersion
Tube with Seal XF / XQ" if the T-probe or immersion tube shows any
damages.
10.4.3.3 To Check the Rotor After Every Run
1. Check both the rotor and the rotor lid for any obvious sign of damage.
2. Check the hydraulic system for oil leakage.

Fig. 10 - 46 Potential spots for oil leakage of the hydraulic system
C49IB08A 299
failure.
Important:
overheating.
Warning:

soft brush.
Be careful not to scratch the sealing surface of the liner in order to avoid
leakage during subsequent runs. Do not use sharp objects!
Alternatively: Clean the liner in an ultrasonic bath.

Alternatively: Use a dishwasher for cleaning the liner.
4. Replace damaged liners immediately, as tightness during subsequent

Escaping acid fumes will then lead to corrosion of other parts.
the seal. Refer to chapter 10.4.1.1, "To Perform a Cleaning Run".
steaming apparatus.
C49IB08A 300
Hint:
Do not store the liner in the vessel jacket. Acid residues may diffuse from the
liner material and lead to corrosion and subsequent damage of the vessel
jackets
10.4.4.2 To Clean and Check the Ceramic Vessel Jacket
1. Let the vessel jacket cool down to ambient temperature.
2. Rinse the vessel jacket thoroughly with deionized water. Do not use any
detergents, as they might affect the heating behavior of these parts!
4. If the vessel jacket requires a more thorough cleaning procedure, refer to

chapter 10.4.7, "Intensive Cleaning of Ceramic Vessels".
5. Check the vessel jacket for any sign of damage, like cracks or chipping.
Discoloration or chipping are indications for improper usage and for
significantly decreased mechanical strength of the vessel jacket. Do not use
such a vessel jacket unless it has been tested by Anton Paar.
10.4.4.3 To Clean and Check the Quartz Glass Vessel
1. To remove stubborn residues on the quartz glass vessel, fill some 2% hydrof-
luoric acid into the vessel and place it into an ultrasonic bath for approx. 10-
15 minutes. Do not exceed the maximum time of 15 minutes as the hydroflu-
oric acid may attack the quartz glass.
2. Rinse the quartz glass vessel thoroughly with deionized water.
3. Check the quartz glass vessel for any sign of damage, like deformations,
cracks or scratches and check for any sign of devitrification.
C49IB08A 301
Chipped-off
quartz glass
vessel
Replace
immediately!
Fig. 10 - 47 Damaged quartz glass vessels
4. Replace damaged quartz glass vessel immediately, as mechanical strength

during subsequent runs is not ensured anymore.
Alternatively send the damaged vessels to our local customer service for
inspection.
5. Perform a cleaning run to remove any detergent residues from the quartz
glass vessel and the seal. Refer to chapter 10.4.1.1, "To Perform a Cleaning
Run".
Alternatively: Steam the quartz glass vessel with nitric acid vapors overnight
using a steaming apparatus.
6. Store the quartz glass vessel in a dry and clean place.
10.4.4.4 To Disassemble the Seal Holder Assembly
1. Thoroughly rinse the complete seal holder assembly under running water to
2. Remove the venting screw.
Venting screw
Fig. 10 - 48 Unscrewing the venting screw
3. Use the reverse side of the venting screw to unscrew the syringe connector.
C49IB08A 302
Syringe connector
4. Remove the seal and place it with the sealing lip facing upwards.
Fig. 10 - 50 Removing the seal
Important:
Do not mix up the seals and venting screws. Always keep the seal and its
venting screw in pairs.
If applicable: Carefully pull out the immersion tube from the seal and remove the
seal husk from the immersion tube.
C49IB08A 303
Seal husk
Fig. 10 - 51 Removing the immersion tube from the seal
5. Unscrew the safety disk holder using an appropriate screwdriver.
Safety disk
Fig. 10 - 52 Unscrewing the safety disk holder
6. Remove the safety disk.
10.4.4.5 To Clean the Seal Holder Assembly
1. Clean the seal holder with water, a mild detergent and a soft brush. Remove
any deposits, especially from the inner side of the seal holder and from the
thread for the venting screw.
2. Thoroughly clean the thread of the venting screw. Take care not to damage
the O-ring.
3. Carefully remove any deposits from the seal, then rinse thoroughly with
deionized water and/or acteone.
C49IB08A 304
4. Clean all other parts (syringe connector, safety disk and safety disk holder)
thoroughly with deionized water and/or acetone. You may use a mild
detergent and a soft brush if necessary.
10.4.4.6 To Check the Seal Holder
1. Check the seal holder for any sign of corrosion.

A slightly brownish discoloration inside the seal holder is normal due to acid
vapors and does not affect proper and safe functioning. Replace the seal
holder if the inside shows severe material degradation.
Fig. 10 - 53 Corroded seal holder
2. Check the seal holder for cracks.

Immediately replace the seal holder if you detect any cracks inside the seal
holder.
Crack
Fig. 10 - 54 Seal holder with a crack
3. Check the thread for the venting screw.

Remove any deposits from the thread before replacing the venting screw.
If the venting screw is not running smoothly anymore, replacement of the
venting screw alone will not restore proper functioning.
C49IB08A 305
Corroded thread
Fig. 10 - 55 Checking the thread for the venting screw
Hint:
Before replacing the venting screw, cleaning the thread using a screw tap is
recommended. An appropriate screw tap is available on request.
10.4.4.7 To Check the Venting Screw
1. Check the O-ring of the venting screw.

Replace the venting screw if the O-ring is deformed or damaged.
2. Check the thread of the venting screw.

Replace the venting screw if the thread is severely corroded or if it is not
running smoothly, even if the thread in the seal holder has been recut.
Venting screw without damages
Damaged O-ring
Corroded thread
Fig. 10 - 56 New and damaged venting screw
C49IB08A 306
10.4.4.8 To Check the Seal
1. Check the sealing lip for any sign of damages, like deformation or cuts.
A defective sealing lip does not ensure proper tightening of the reaction ves-
sels anymore. Replace damaged seals immediately to avoid cost-intensive
repairs due to escaping acid vapors during subsequent runs.
Hint:
Avoid damage of the lip-type seal during storage by using the optional seal
forming device.
Sealing lip damaged
Sealing lip ok
Fig. 10 - 57 Checking the sealing lip for damages
2. Check the spot where the safety disk is located.

Replace the seal if this spot is pressed out. In this case also replace the
safety disk.
Hint:
When replacing the seal, replace the venting screw as well, otherwise
tightness of the reaction vessels may not be ensured.
Do not use new seals with old venting screws!
Seal OK Damaged seal
Fig. 10 - 58 Damaged seal
C49IB08A 307
10.4.4.9 To Check the Safety Disk
1. Check the safety disk for signs of corrosion.

Slight discoloration does not affect proper functioning of the safety disk.
Replace considerably corroded safety disks.
2. Check the safety disk for deformation.

A slight bulge is normal. Replace the safety disk if the bars start to break
already.
New safety disk Slightly bulged safety Opened safety disk,

disk, O.K. not O.K.
Fig. 10 - 59 Safety Disk X
10.4.4.10 To Reassemble the Seal Holder Assembly
1. Insert the safety disk into the seal holder with the label "X" facing outwards.
Take care that the safety disk is positioned correctly. The holes in the safety
disk have to form a "C".
Fig. 10 - 60 Positioning of the safety disk
Important:
2. Fix the safety disk by screwing in the safety disk holder.
C49IB08A 308
Fig. 10 - 61 Fixing the safety disk with the safety disk holder
3. Insert the seal into the seal holder and fix it with the syringe connector and
the venting screw.
10.4.4.11 To Reassemble the Immersion Tube with Seal
1. Before inserting the seal in the seal holder, take the immersion tube and
push it into the new lip-type seal from the top downwards until approx. 5 mm
of the immersion tube sticks out of the top of the seal. Take care not to dam-
age the sealing lip.
5 mm
Fig. 10 - 62 Inserting the immersion tube into the seal
Fig. 10 - 63 Reassembling the seal holder assembly
2. Fix the seal by screwing in the venting screw and the syringe connector.
Reopen the venting screw for one turn during storage.
C49IB08A 309
3. Push a new seal husk provided with the seal onto the immersion tube.
Important:
onto the immersion tube so that the wider end faces the seal holder. To
to fit tightly. Use the special husk assembly too to slide the seal husk up to the
final stop position.
Seal husk
Husk
assembly
tool
assembly tool
4. Fix the immersion tube while carefully removing the husk assembly tool.
Important:
experiment to check the tightness of the seal. Weigh the solution before and
after the performance run and check for losses. If the losses are higher than
2%, check the tightness of the seal and seal husk once again.
10.4.4.12 To Clean Rotor 8S
1. Clean the protection lid with a damp cloth.
2. Remove all fastening screws and remove the rotor upper plate.
3. Pull the PEEK bushings out of the hole.
C49IB08A 310
Bushings made of PEEK
Fig. 10 - 65 Aluminum upper plate of Rotor 8S with PEEK bushings
Important:
Do not operate Rotor 8S with deformed or without bushings!
4. Remove deposits from the PEEK bushings either with a soft cloth, moistened
with acetone, under running water or in an ultrasonic bath.
5. Remove any metallic residue from the fastening screw. The best way is to
knock the fastening screw with the thread facing down against a hard
surface (e.g. table).
6. Replace damaged PEEK bushings.
7. Remove visible contaminations (e.g reagent spills) with a damp cloth.

Never rinse Rotor 8S under running water!
8. Remove the 8 silicon protection hoses from the tension bars and clean them
under running water with a mild detergent.
Fig. 10 - 66 Removing the protection hoses from the tension bars
9. Wipe the tension bars and the rotor bottom plate with a damp cloth. Remove
any metallic residues, which may come from the fastening screws.
C49IB08A 311
11. Reassemble the rotor in reversed order.
10.4.4.13 To Check the Rotor
1. Check both the rotor and the rotor lid for any obvious sign of damage.
2. Check the hydraulic system for oil leakage.

Fig. 10 - 67 Potential spots for oil leakage of the hydraulic system
3. Check the correct position of the position marker labels underneath the
bottom load ring.
To clean and check the microwave cavity, follow the instructions given in chapter
10.4.5 Procedures After the Rupture of a Safety Disk
For this reason, extensive cleaning and checking procedures are required.
Warning:
C49IB08A 312
10.4.5.1 Immediately After the Breakage of a Safety Disk

3. Carefully remove the rotor, place it under a fume hood and vent the vessels
(refer to chapter 10.3.5.2, "To Vent Under a Fume Hood").
5. If applicable: Carefully remove the T-probe before opening the fastening

unit carefully straight upwards out of the vessel (refer to chapter 10.3.5.3, "To
Remove the T-Probe").
6. Open the rotor and remove the reaction vessels (refer to chapter 10.3.5.4,
"To Open the Pressure Vessel"). It is most probable that the synthesis was
Important:
replaced.

Hint:
After breakage of a safety disk the liner might be deformed due to the rapid
pressure loss.
If the sealing area (approx. 2 cm from the top) is not affected, such a
deformed liner can be reshaped by performing a cleaning run.
Replace the liner if the deformation has affected also the sealing area.
C49IB08A 313
Deformation
Fig. 10 - 68 Deformed liner
10.4.5.3 To Clean and Check the Immersion Tube with Seal and the T-
Probe
1. Follow the instruction given in chapter 10.4.3.2, "To Check the Immersion
Tube with Seal After Every Run" and chapter 1.7, "Immersion Tube with Seal
XF/XQ-Maintenance".
2. Clean the T-probe using a damp cloth.
Important:
Do not wet the electronic module of the T-probe when cleaning the sensor.
Do not clean the capillary, as this part might break easily.
• Refer to chapter 10.4.4.12, "To Clean Rotor 8S" and chapter 10.4.4.13, "To
Check the Rotor".
cavity.
Fig. 10 - 69 Disassembling the turntable drive star and drive base
C49IB08A 314
if necessary.
PTFE covers.
and instrument.
Warning:
damaged parts.
C49IB08A 315
Fig. 10 - 71 Assembling the drive base, drive star and turntable
reactions, which are too fast for the safety disk or by previously damaged vessel
jackets.
Synthos 3000 is equipped with numerous safety features, which ensure that the
laboratory personnel is safely protected in case of such an incident.
In case of a vessel breakage, solvent and reagents reagents will be released

together with vessel debris inside the microwave cavity. This leads to
contamination of the rotor, the outer surfaces of the vessels as well as the
microwave cavity.
For this reason, extensive cleaning and checking procedures are required.
Warning:
Warning:
C49IB08A 316

In this case, the safety cooling does not switch off automatically.
3. Carefully remove the rotor. Take care of splinters, especially when using
ceramic vessels!
4. Place the rotor under a fume hood and vent the vessels (refer to chapter
10.3.5.2, "To Vent Under a Fume Hood").
6. If applicable: Carefully remove the T-probe before opening the fastening

unit carefully straight upwards out of the vessel (refer to chapter 10.3.5.3, "To
Remove the T-Probe").
7. Open the rotor and remove the reaction vessels (refer to chapter 10.3.5.4,
"To Open the Pressure Vessel"). It is most probable that the synthesis was

Hint:
If you are not sure if the ceramic vessel jackets have been damaged during
the explosion, you may send them to Anton Paar for inspection.
10.4.6.3 To Clean and Check the Immersion Tube with Seal and the T-
Probe
1. Follow the instruction given in chapter 10.4.3.2, "To Check the Immersion
Tube with Seal After Every Run" and chapter 10.5, "Maintenance of the T-
Probe and the Immersion Tube with Seal XF / XQ".
C49IB08A 317
2. Carefully clean the T-probe using a damp cloth.
Important:
Do not wet the electronic module of the T-probe when cleaning the sensor.
Do not clean the capillary, as this part might break easily.
To clean and check the microwave cavity, follow the instructions given in chapter
To clean the exhaust channel, follow the instructions given in chapter 8.5.6.5, "To
Clean the Exhaust Channel".
1. Refer to chapter 10.4.4.12, "To Clean Rotor 8S" and chapter 10.4.4.13, "To
Check the Rotor".
2. In case of heavy contamination, also disassemble and clean the rotor bottom
plate. Proceed with chapter 10.4.6.7, "To Disassemble the Rotor".
1. After all vessels have been removed and cleaned, remove the fastening
screws and lift off the rotor upper plate. Do not disassemble the rotor upper
plate. In case of a hydraulic oil leakage, the rotor has to be sent to
Anton Paar GmbH for service.
C49IB08A 318
Fig. 10 - 72 Removing the fastening screws and lifting off the rotor upper plate
2. Remove the protection hoses from the tension bars.
Fig. 10 - 73 Removing the protection hoses from the tension bars
3. Unscrew the bottom guard from the bottom load ring (with an Allen screw
driver, 4 mm).
C49IB08A 319
Bottom guard
Fig. 10 - 74 Unscrewing the bottom guard
4. Remove all eight base rings.
Base ring
Fig. 10 - 75 Disassembling the bottom load ring
10.4.6.8 To Clean the Rotor Bottom Plate
1. Clean all parts under running water or use a damp cloth. Use a mild deter-
gent and a soft brush if necessary.
2. Remove splinters.
3. Wipe off any traces of non-decomposed sample material with a piece of cloth
moistened with isopropyl alcohol.
5. Check the correct position of the position marker labels on the bottom side of
the rotor.
C49IB08A 320
Position 1
Fig. 10 - 76 Checking the correct position of the position marker label
1. Replace damaged or broken parts.
2. Start the reassembling by putting the clean base rings onto the bottom load
ring.
Fig. 10 - 77 Putting the base rings onto the bottom load ring
3. Put the bottom guard onto the bottom load ring and fix it with the screws.
Take care of the right positioning. Position 1 of the bottom guard has to
correspond with the position 1 of the bottom load ring (marked with the larger
position marker label).
C49IB08A 321
Position marker labels Position 1
Bottom guard
Fig. 10 - 78 Screwing on the bottom guard
4. Assemble the protection hoses on the tension bars.
Fig. 10 - 79 Assembling the protection hoses onto the tension bars
5. Put the rotor upper plate on the tension bars and fix it with the fastening
screws. Take care of the right position of the rotor upper plate. The white
opening in the upper plate has to correspond with the position 1 in the
bottom guard.
C49IB08A 322
Position 1
Fig. 10 - 80 Putting the rotor upper plate on the tension bars and fixing it with the
rotor fastening screws
10.4.7 Intensive Cleaning of Ceramic Vessels
For proper maintenance of the ceramic vessels refer to chapter 9.4.7, "Intensive
Cleaning of Ceramic Vessels".
Important:
This cleaning procedure is intended only for users of ceramic vessel jackets
(8SXF100) and does not apply to quartz glass vessels!
C49IB08A 323
10.5 Maintenance of the T-Probe and the Immersion

Tube with Seal XF / XQ
10.5.1 Replacing the Seal and Safety Disk
replacement.
Important:
When you replace the seal or immersion tube you have to replace the seal
husk as well! When removing and inserting the seal husk, do not use sharp
objects, which could damage it.
Warning:
1. Remove the venting screw from the seal holder.
Fig. 10 - 81 Removing the venting screw
2. Use the reverse side of the venting screw as tool for unscrewing the syringe
connector.
C49IB08A 324
Fig. 10 - 82 Disassembling the syringe connector
3. Check the venting screw, the O-ring, the threads of the venting screw and
syringe connector and the syringe connector carefully. If you observe any
signs of deformation or corrosion, replace these components.
4. Pull the seal out of the seal holder.
5. Remove the immersion tube from the seal by pulling it out.
Seal husk
Fig. 10 - 83 Removing the immersion tube from the seal
6. Remove the seal husk.
10.5.1.2 To Replace the Safety Disk
1. Unscrew the safety disk holder with a large screwdriver or a similar tool.
Important:
Take care not to damage the seal when unscrewing the safety disk holder!
C49IB08A 325
Fig. 10 - 84 Replacing the safety disk
2. Insert the safety disk into the screw cap with the label "X" facing outwards.
Take care that the safety disk is positioned correctly. The holes in the safety
disk have to form a "C".
10.5.1.3 To Assemble the Immersion Tube with Seal
1. Before inserting the seal in the seal holder, take the immersion tube and
push it into the new lip-type seal from the top downwards until approx. 5 mm
of the immersion tube sticks out of the top of the seal. Take care not to dam-
age the sealing lip.
5 mm
Fig. 10 - 85 Inserting the immersion tube into the seal
Fig. 10 - 86 Reassembling the seal holder assembly
C49IB08A 326
2. Fix the seal by screwing in the venting screw and the syringe connector.
Reopen the venting screw for one turn during storage.
3. Push a new seal husk provided with the seal onto the immersion tube.
Important:
onto the immersion tube so that the wider end faces the seal holder. To
to fit tightly. Use the special husk assembly tool to slide the seal husk up to the
final stop position.
Seal husk
Husk
assembly
tool
assembly tool
4. Fix the immersion tube while carefully removing the husk assembly tool.
Important:
Never use sharp objects to push the seal husk onto the immersion tube.
Make sure that the seal is not damaged during assembly.
Important:
reaction to check the tightness of the seal. Weigh the solution before and after
the performance run and check for losses. If the losses are higher than 2%,
check the tightness of the seal and seal husk once again.
C49IB08A 327
Important:
Calibration with the Calibration Accessory" or to chapter 6.7.5, "Temperature
Sensor Calibration with the Calibration Unit". Carry out the steps described
below only if you are able to perform a temperature sensor calibration!
1. Remove the PEEK screw (fixing screw), which holds the capillary onto the
arm of the T-Probe.
PEEK screw (Fixing screw)
Fig. 10 - 88 Unscrewing the PEEK screw
2. Unscrew the knurled nut of the capillary tube, pull it back and take it out of
the screw-type fitting.
Remove the knurled nut from the capillary.
C49IB08A 328
Knurled nut
Fig. 10 - 89 Unscrewing the knurled nut
3. Remove the complete thermometer capillary by pulling it carefully

downwards.
Fig. 10 - 90 Removing the capillary
4. Remove the small ferrule by tapping it out of the fitting on the electronics
module. The complete sealing part consists of two parts: knurled nut and
ferrule.
Capillary PEEK screw Knurled nut with ferrule (sealing parts)
Fig. 10 - 91 Capillary, PEEK screw and knurled nut with ferrule
C49IB08A 329
5. Replace the old capillary by a new one.

The new capillary is delivered with a new knurled nut and ferrule. Take the
sensor in one hand and the new capillary with the glass bulb in the other.
The glass bulb has to face downward.
6. Assemble the new capillary very carefully in reverse order.
7. Mount the knurled nut (delivered with the new capillary) and ferrule on the
capillary so that the metal end protrudes from the nut for 2 mm.
8. Fix the capillary finger-tight with the knurled nut.
9. Screw on the PEEK screw (fixing screw), which holds the capillary.
10. Perform a temperature sensor calibration.
Important:
The thermometer capillary must not be longer than 215 mm! (measured from
the sensor arm to the glass bulb)
2 mm
Ferrule Knurled nut

215 mm
C49IB08A 330
PEEK screw (Fixing screw)
Fig. 10 - 93 Screwing the PEEK screw
C49IB08A 331
11 Applications
11 Applications
11.1 General Information
Synthos 3000 is delivered with a selected method library stored in the instrument.
The examples represent model reaction types, which are frequently performed in
synthesis laboratories. The programs listed in the method library are tested and
contain the following information:
- Rotor type
- Vessel type
- Number of vessels used
- Method name
- Batch size
- Required reagents
- Temperature or power program
When carrying out similar experiments, those are useful standard conditions to
start with. Any existing method from other microwave devices, which has been
optimized, can be entered in the database to be used with Synthos 3000. The
user is responsible for the consequences when carrying out reactions, which
have not been tested by Anton Paar.
Important:
The reaction behavior of sample materials may differ significantly from the
examples listed in the library, even if the sample designation is the same.
For optimal synthesis of your samples, you should generate and store your
own methods.
Although Synthos 3000 is verified for direct scalability of small batch sizes up to
large batch sizes, you should first test your new synthesis with small amounts to
document the reaction behavior in the microwave field.
The syntheses which are listed in the method library describe reaction types
which are frequently performed in synthesis laboratories. If you want to carry out
similar reactions, these are useful standard conditions for investigating reactions.
If you already have a method which has been optimized for small amounts, you
can enter this protocol in the database and use it with whichever amount you
require.
The user is responsible for the consequences of carrying out reactions which
have not been tested by Anton Paar.
C49IB08A 332
11 Applications
11.1.1 Basics of Microwave Heating
Microwave-assisted chemistry relies on the efficient heating of materials by an

electromagnetic microwave field. The electric component of the electromagnetic
field accomplishes heating by two main mechanisms:
Dipolar Polarization: Dipolar molecules try to align accordingly in an applied

electric field. As the field oscillates the dipoles re-orientate permanently, but
anyhow a phase difference is generated between the orientation of the field and
the dipole, respectively. This phase difference results in energy loss by molecular
friction and collisions, expressed in heat.
Ionic Conduction: Dissolved charged particles oscillate under the influence of the
microwave field causing continual collisions with neighboring molecules. Similar
to the dipolar polarization, this extensive motion causes heat.
The ability of solvents to convert the introduced electromagnetic energy into heat
is determined by the loss factor (tan d), which is expressed as the following
quotient:
Definition of the loss factor:
The dielectric loss ε‘‘ indicates how efficiently a substance converts

electromagnetic radiation into heat, whereas the dielectric constant ε´ describes
the polarizability of molecules in the electric field. By definition, solvents with tan δ
< 0.1 (at 20 °C, see table below) are so-called low-absorbing agents. Compounds
without a permanent dipole like CCl4 or dioxane are more or less microwave
transparent (tan δ n.d.). Since the dielectric constant is dependent on
temperature, the tan δ changes with rising temperature, but only water shows a
significant variation at higher temperatures. A comprehensive list showing tan δ
of common solvents can be found in relevant microwave literature.
Materials with insulating properties, like polymers, quartz or types of ceramics,

usually have a very low loss tangent. Such materials are more or less microwave
transparent and are thus preferably used for the construction of reaction vessels.
The major benefits in performing microwave-assisted reactions are:

- Rate enhancement: reaction times can be drastically reduced from hours
to minutes
- Increased yield: short reaction times minimize unwanted side reactions
- Improved purity: less by-products result in simplified purification
C49IB08A 333
11 Applications
Solvent bp (°C) tan δ MW absorbance
Ethylene Glycol 179 1.350 Very good
DMSO 189 0.825 good
Ethanol 78 0.941 good
Methanol 65 0.659 good
NMP 202 0.275 medium
DMF 153 0.161 medium
Water 100 0.123 medium
Acetonitrile 81 0.062 medium
THF 65 0.047 low
Dichloromethane 40 0.042 low
Toluene 110 0.040 Very low
Dioxane 106 n.d. Very low
Ref. Microwaves in Organic and Medicinal Chemistry, C.O. Kappe, A. Stadler, Wiley-VCh, 2005
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11.1.2 Hazards During Microwave Synthesis
The immediate and rapid heating of the sample using microwave irradiation
considerably accelerates the reaction. However, this direct heating method
involves possible dangers:
• Metals
Metals interact directly with microwave irradiation, which may result in

electrostatic discharge. Thus, metals should only be used as fine granules or
powdered. Moreover, the mixture must be stirred sufficiently to avoid the
formation of metal layers on the vessel surface.
Hint:
Never carry out synthesis reactions without stirring. Stirring increases the
efficiency by mixing the reaction partners thoroughly. It also prevents
undesired super heating effects (when the solvent is heated above its boiling
point although it does not show signs of boiling). When solutions are in a
super heated state they can boil explosively and destroy the vessels.
• Stir bars
The metallic core of a stir bar can act as an antenna and may intensively interact
with the microwave field. This can lead to hotspots and sparks. Only use stir bars
<3 cm (1/4 of wavelength) to ensure safe performance of microwave reactions.
• Operating error
Only trained personnel with sufficient experience should work with chemicals
under microwave conditions. It is the responsibility of the laboratory manager to
make sure that the relevant safety regulations are observed and that personnel
wear appropriate protective clothing.
Noxious reagents and substances which tend to form explosive reaction products,
require more strict safety regulations.
• Insufficient load
This is particularly problematic when using weak coupling substances. If you try
to heat a small amount of sample to high temperatures so that the magnetrons
continuously operate at high power, the microwave energy will be taken up by the
instrument and accessories. This can cause sparks, thermal deformation of the
rotor lid and other damage to the instrument. The magnetrons are effectively
protected against overheating so that no damage can occur to the magnetrons.
To avoid these effects, never use less than 4 vessels. If the reaction mixtures are
completely non-polar, we recommend using passive heating elements (refer to
chapter 11.1.3.1, "Solvents").
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• Explosive mixtures
If the sealing lip is not formed sufficiently or the the screw caps are not sealed
tightly enough, solvent may leak into the microwave cavity. As many organic
solvents can form explosive mixtures and microwave irradiation represents a
permanent source of ignition, it is essential that the vessels are leak-tight.
• Overloading
If the filling volulme is too large or the concentration too high, the safety limit may
be exceeded. If extreme pressure peaks or violent exothermal reactions occur,
this can lead to rupture of the safety disks and/or vessel explosion.
Hint:
Explosive substances in large amounts in the microwave field may lead to

serious accidents. Using these substances is the responsibility of the user.
• Pressure
Very reactive reagents or rapid heating rates can lead to the formation of high
pressures during the reaction which exceed the permitted limit. Thus, Synthos
3000 is equipped with numerous safety systems such as monitoring of the
pressure increase rate, patented cooling system, specially designed rotor
geometry and safety door. In normal use, any overpressure build-up is controlled
those safety measures.
• Temperature
Steep heating ramps increase the risk of spontaneous reactions (overpressure).

The experiment may have to be aborted, especially if the reaction is exothermal.
The integrated security cooling always runs at a low level during a reaction. This
prevents overheating by exhausting the reaction heat. Most microwave-assisted
organic syntheses operate in the 100 to 220 °C range, which poses no problem
for Synthos 3000.
Hint:
For uniform heating distribution, the vessels should be loaded symmetrically
into the rotor. If the number of vessels used does not allow symmetrical
loading, we recommend charging the missing positions with blanks (pure
solvent). Never use less than 4 vessels in any of the rotors. When
programming a power profile, always take care to adapt the programmed
power to the number of used vessels.
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During tough high-temperature applications (e.g. near-critical water chemistry),

thermal damage to the instrument components can be prevented by
programming suitable temperature and power limits. As water loses its good
coupling properties with increasing temperature and therefore microwave energy
is increasingly absorbed by instrument components, the duration of a run should
be limited to max. 60 minutes. This helps reduce the risk of damage, especially to
the rotor lid.
• Superheating
Microwave energy can heat solvents far above their classical boiling point.
Solvents in a superheated state can suddenly and explosively boil up and
therefore cause the reaction vessels to rupture. For this reason, never carry out
organic synthesis without a magnetic stirrer.
Solvent Kp Kp
(classical) (superheating)
Dichloromethane 40 °C 55 °C
Methanol 65 ° C 98 °C
Ethanol 78 °C 104 °C
Acetonitrile 81 °C 109 °C
Water 100 °C 104 °C
Chlorobenzene 132 °C 150 °C
• Local overheating
If microwave energy couples directly with a component, strong local overheating

may occur in the reaction vessels and result in destruction of the vessel. This
phenomenon can also be reduced by stirring.
Important:
After every metal catalyzed reaction, check for deposits on the vessel surface
and clean the quartz vessels thoroughly. Do not carry out metal catalyzed
reactions in PTFE vessels, otherwise the liner may be permanently
contaminated due to adsorption.
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11.1.3 Reagents
Important:
Always wear protective glasses, gloves and the appropriate protective
clothing when handling chemicals. Observe the relevant national regulations.
11.1.3.1 Solvents
In general, microwave-assisted reactions can be performed using the same

solvent as with conventional heating. However, solvents interact differently with
microwaves, according to their dielectric properties. Most effective solvents are
those with good microwave absorbance (see table), generally polar ones. Low
absorbing (unpolar) solvents are poorly heated when used pure. However, as
reaction mixtures are usually containing various (polar) reagents there should be
enough potential for efficient microwave coupling.
If this should not be the case, Anton Paar offers re-usable passive heating
elements made of silicon carbide (SiC), to be used as additives in low-absorbing
mixtures. Silicon carbide converts microwave energy very effectively into heat
and, being an excellent conductor, provides to achieve appropriate heat transfer
within the mixture. Thus, heating rates are highly comparable with direct
microwave heating. Furthermore, SiC is chemically inert and does not interfere
with the reagents nor contaminate the products. After the experiment, the heating
elements can be easily removed with tweezers and cleaned by simply rinsing with
any appropriate solvent.
Fig. 11 - 1 Heating Elements
Using passive heating elements allows using even microwave-transparent

solvents, such as toluene or dioxane, in microwave-mediated processes at
temperatures far above their boiling points (see table 11.1), opening completely
new avenues for method development.
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Entry Solvent bp Tempa Amount

1 DCM 40 °C 148 °Cb 4 x 50 mL
2 Chloroform 62 °C 229 °C 4 x 50 mL
3 THF 67 °C 210 °C 4 x 50 mL
4 CCl4 77 °C 143 °C 10 x 10 mL
5 Acetonitrile 81 °C 241 °Cc 4 x 50 mL
6 H 2O 100 °C 280 °Cd 4 x 15 mL
7 Dioxane 102 °C 170 °C 4 x 50 mL
8 Toluene 111 °C 193 °C 4 x 50 mL
a.Temperature after 10 min at 800 W
b.Temperature after 3 min at 800 W
c.Temperature after 7.5 min at 800 W
d.Temperature after 10 min at 1400 W
Table 11.1: Heating of low-absorbing solvents (one heating element per vessel)
Hint:
The microwave characteristics of solvents change at high temperatures.
Usually, their polarity decreases and their coupling properties deteriorate.
Take this into consideration when developing new methods.
The properties of water become comparable with those of organic solvents. It
is therefore possible to carry out high-temperature syntheses (>250 °C) in
water, which would not be possible or would not run well in organic solvents.
Whereas low boiling solvents like THF, ethanol or acetonitrile work nicely under
elevated microwave conditions some other organic solvents, such as DMF,
DMSO and NMP, decompose at high temperatures. This can be detected by
some brownish color and an unpleasant smell generated. For this reason, only
open and vent vessels containing these solvents under a well-functioning fume
hood. However, the generally short reaction times for microwave synthesis
prevent the decomposition of these substances progressing too far, so that it has
no negative effects on the reactions.
Important:
Utilizing low-boiling solvents may result in a significant pressure increase at
elevated temperatures. Therefore it is crucial to observe the operation limits of
the equipment used.
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11.1.3.2 Solventless Reactions
Microwave-mediated reactions can also be carried out solventless ("neat" or "dry-

media" reactions). As no additional solvent is involved the pressure built-up is
rather low or even negligible.
Whereas neat reactions employ only the reagents without additional solvent
(maximized concentration) dry-media reactions utilize reagents pre-absorbed on
a solid support. Frequently used absorbing materials are silica gel, alumina, clays
(microwave transparent), graphite or charcoal (strongly absorbing).
Important:
Dry-media reactions can easily be locally overheated as stirring and accurate
temperature measurement can be rather difficult. Thus, degradation or
decomposition of reagents may likely be observed performing this kind of
reactions
11.1.3.3 Solid Phase Synthesis
Synthos 3000 is also suitable for microwave-assisted solid phase organic

synthesis (SPOS). The powerful magnetic stirring ensures efficient mixing of the
reaction partners. Damage to the solid phase materials caused by the magnetic
stirrer is minimized due to the drastically reduced reaction times. The frequently
used polystyrene resins (e.g. Merrifield resin) can be stirred in the microwave field
for up to one hour at up to 200 °C without negative effects on their capacity and
reactivity.
Hint:
As polystyrene resins swell in organic solvents, do not add more than 5 g dry
resin per vessel (max. 1 g in MF50 vessels). This guarantees adequate
mixing and effective yield.
Other solid phase materials, such as lanterns, crowns or tubes can only be used
in small amounts due to their geometric form and volume. Problems may occur
when stirring in the reference vessel containing the internal temperature sensor.
The above-mentioned solid supports are not as temperature-stable as
polystyrene resins and therefore should not be used under the same conditions
as applied with polystyrene resins.
11.1.3.4 Corrosive Reagents
Large amounts of corrosive reagents (e.g. mineral acids and alkalis) are seldom
used in organic synthesis. Usually those chemicals are only used in small
amounts as catalysts or mediators. Synthos 3000 and all the accessories are
also designed for use with such reagents. If you observe the relevant cleaning
and maintenance instructions, the parts are ensured a long service life.
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Examples of frequently used corrosive reagents in organic synthesis:
Nitric acid HNO3 Trifluoroacetic acid CF3COOH
Sulfuric acid H2SO4 Triethylamine (C2H5)3N
Hydrochloric acid HCl Sodium hydroxide NaOH

solution
Phosphoric acid H3PO4 Potassium hydroxide KOH

solution
Hydrofluoric acid HF
Important:
Never use strong bases such as concentrated potassium hydroxide and
sodium hydroxide in quartz vessels as those reagents will harm the glass
surface at high temperatures. Also hydrofluoric acid in high concentration will
attack quartz glass severely.
Some substrates can also be corrosive but they are usually converted to other
products, with other properties, during the reaction. These substances therefore
pose no danger with normal operation. If a safety disk ruptures, follow the
appropriate safety measures.
11.1.3.5 Gases
Synthos 3000 allows the use of gaseous reagents for microwave-mediated

synthesis. Up to 20 bar of either inert gas (argon, nitrogen) or reactive gas (CO2,
Cl2, ethylene etc.) can be applied to each vessel prior to reaction.
Hint:
For detailed information on the gas loading equipment refer to the
corresponding product information (B83IE36B).
This feature can be easily achieved with the aid of the Anton Paar Gas Loading
accessory. The assembly consists of the special Rotor Lid Gas for Rotor 8S and
a 4-way valve station for gas supply with a corresponding gas loading nozzle.
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Rotor Lid Gas
Loading Nozzle
4-way valve
Fig. 11 - 2 Gas loading accessory
The loading nozzle is a simple male bayonet adaptor to be connected with a

female adaptor counterpart, mounted on each reaction vessel (Fig. 11 - 3). This
is a screw-on tool replacing the regular syringe adapter on the seal holder.
Furthermore the final set-up requires a protective cap gas for each reaction
vessel.
Fig. 11 - 3 Seal holder with gas loading adapter, reaction vessel closed with
protective cap gas and vessel arranged in Rotor 8S
The 4-way valve station enables simultaneous connection to inert gas, reactive
gas and even a vacuum pump. This allows removing air from the vessels and
protecting sensitive reagents effectively.
Gas Loading procedure:
1. Charge each vessel with the reagents and solvents and seal properly with
the modified seal holder (Fig. 11 - 3/1).
2. Close the reaction container with the protection lid (Fig. 11 - 3/2) and place
the vessels in the Rotor (Fig. 11 - 3/3)
3. Put on the protection lid gas and place the rotor inside the Synthos 3000.
4. Attach the 4-way valve to the gas supply and connect the Loading nozzle
with the first reaction vessel via the appropriate opening of the rotor lid.
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11 Applications
Click
Twist 90°
Fig. 11 - 4 Connecting the Loading nozzel via the protection lid
5. Use the venting key to open the venting screw (Fig. 11 - 4 b). Open the gas
supply and flush the vessel for a few seconds.
6. Close the venting screw with the key and apply the required amount of gas
(max. 20 bar). Use the pressure controller of your gas supply to adjust the
appropriate pressure level.
Important:
Do not use too much force when closing the venting screw with the supplied
key. Fingertight closure is sufficient. Any more force applied may strain the
sealing O-ring.
7. When the required pressure level is reached, close the gas supply and
disconnect the bayonet link.
8. Move the rotor manually to get access to the next vessel and proceed
according to steps 4-7. When done with all vessel start your experimental
procedure.
Hint:
To have the maximum of 20 bar pre-pressurizing available software v.2.0 or
higher is required.
Flushing with inert gas (nitrogen, argon) is also possible for reaction vessels of
Rotor 16. Therefore, the corresponding loading adaptors Gas 16 are required
(Fig. 11 - 5). This is achieved outside the cavity before closing the rotor lid,
following step 5 in the above description. Flush the vessel for approximately 90
sec or perform 3 cycles applying vacuum and inert gas alternately for a proper
inert gas atmosphere.
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Fig. 11 - 5 Applying inert gas on Rotor 16 vessels
Observe the general safety regulations when using reactive gases such as
ethylene or oxygen and take into consideration the maximum pressure load of the
vessels.
Warning:
Explosive mixtures always pose an operational risk in the microwave field. To
avoid such conditions, we do not recommend to use hydrogen gas for
microwave-mediated reactions. Extreme care has to be taken! The user is
responsible for occuring consequences when utilizing dangerous reagents.
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11.1.4 Reaction Vessels
The following vessel types are available with the Synthos 3000:
Vessel type MF50 MF100 HF100 XF100 XQ80
Vessel material PFA TFM TFM TFM Quartz
Operating pressure 20 bar 20 bar 40 bar 60 bar 80 bar
Max. internal temp. 200 °C 200 °C 240 °C 260 °C 300 °C
Max. IR temp. 140 °C 160 °C 210 °C 240 °C 280 °C
Volume 50 mL 100 mL 100 mL 100 mL 80 mL
Operating volume 6-25 mL 6-60 mL 6-60 mL 12-60 12-60

mL mL
PFA and TFM vessels:
These vessels are suitable for standard synthesis, in which the pressure and
temperature does not rise into extreme ranges. We also recommend these
vessels for solid phase synthesis as the solid phase components do not adhere
to the vessel surface and can therefore be handled easier.
Quartz vessels:
These vessels were specially designed for applications under extreme conditions.
Pressures up to 80 bar at temperatures up to 300 °C can be reached easily and
safely. However, when using weak coupling solvents the operating time should
not be longer than 60 minutes at 300 °C due to the thermal stress for rotor parts.
To avoid any damage, the use of passice heating elements is recommended in
this case.
Important:
Do not use stir bars when applying SiC heating elements with quartz vessels.
The glass surface may be scratched and pressure stability can not be
generated anymore.
The quartz vessels are also suitable for metal catalyzed reactions as any
elementary metal which is produced can be easily removed from the surface and
there is no vessel contamination due to adsorption.
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Hint:
Only clean the quartz vessels with a soft brush; never use a metal spatula. Try
to avoid using mechanical force as this could damage the vessels by causing
scratches. Never use damaged or scratched vessels for reactions as the
pressure resistance is no longer guaranteed. Very dirty vessels can be
cleaned in Synthos 3000 in a cleaning run (refer to chapter 10.4.4, "Standard
Cleaning and Maintenance Procedures").
Rotor load:
For uniform heating distribution, the vessels should be loaded symmetrically into
the rotor. Thus, always adhere to the recommended loading paterns of the
respective rotor type (refer to chapter 8.4.3, "Loading Rotor 48", chapter 9.3.3,
"Loading Rotor 16" and chapter 10.3.3, "Loading Rotor 8S"). If the number of
used vessels does not allow symmetrical loading we recommend loading the
missing vessel positions with blanks (pure solvent).
• Never use less than 4 vessels.
• When programming a power profile, always take care to adapt the

programmed power to the number of used vessels. The lower the number of
vessels used, the lower the max. programmed power.
• When programming a temperature profile, the programmed temperature is

independent of the number of used vessels.
Hint:
We always recommend to perform synthesis applications with inner
temperature measurement.
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11.2 Performing Synthesis
11.2.1 General
• There are different sensor types available for Synthos 3000. These allow
optimal control of the reactions. Rotor 16 and Rotor 48, respectively enable
you to use a combined immersing pressure/temperature sensor in one
reference vessel. Rotor 8S has a hydraulic sensor incorporated, which
measures the pressure at every position. An additional temperature probe is
also available which measures the inside temperature of the reference
vessel. Furthermore, Synthos 3000 is equipped with an IR temperature
sensor, which measures the external vessel temperature of each vessel.
• Due their individual physical properties, chemicals react differently in the

microwave field. This can be useful for certain reactions. For example: using
weak coupling solvent means that the maximum energy is absorbed by the
reagents only and the non-polar solvents acts as kind of a heat sink. On the
other hand, adding substances which couple extremely well (e.g. ionic
liquids) enables you to reach an extremely high heating rate and elevated
temperatures easily.
• Reactions which are known to be strongly exothermal should be carried out

in fairly low concentrations to avoid overheating or excessive pressure
increase and the resulting termination of the reaction. It is possible to control
exothermal reactions by programming a plane power profile.
• The length of a reaction depends on the optimized conditions and the

desired reaction results. The normal duration of a classical synthesis,
including cooling, is between 30 and 60 minutes, whereby the cooling time
depends on the maximum temperature reached.
Hint:
Many solvents and reagents used in organic synthesis are highly
inflammable and require special safety measures.
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11 Applications
11.2.2 Operation Without an Internal Temperature Sensor
• In principle it is possible to perform reactions just by using the IR Sensor

Accessory. This is a cost effective option for routine standard reactions which
occur under well-defined conditions and do not require permanent control of
the internal temperature.
• Please note that, due to the continuous flow of air from the cooling system,
the measured surface temperature is always lower than the reaction
temperature inside the vessel. Take this into consideration when
programming a method without internal temperature sensor.
Hint:
Each Synthos 3000 is delivered with an IR sensor as standard. We
recommend additionally using the optional internal temperature sensor.
However, it is not essential for achieving good synthesis results. The decision
should be made by the user.
11.2.3 Operating With Sensors
• For comprehensive documentation and traceability of synthesis reactions

optimal pressure and temperature measurement is essential. The precise
methods stored in Synthos 3000 enable trouble-free adaptation of synthesis
specifications for the different systems of different manufacturers.
• The creation of new methods requires only a few steps (refer to chapter 6,
"Software"). Even with unknown, reactive reactions, the automatic system
control prevents vessel limits being exceeded. The optimal conditions are
therefore achieved easily and safely.
11.2.3.1 Power/Temperature-controlled Methods
• When using sensors, you can choose between two different profiles: power
profile and temperature profile.
Hint:
As synthesis reactions are highly dependent on the temperature, we
recommend using an internal temperature sensor to ensure optimal reaction
conditions during large scale operations.
• Both the power profile and temperature profile allow you to adapt methods
from other manufacturers and from the small scale range. When using a
power profile, always set the programmed power according to the number of
vessels used (the lower the number of vessels used, the lower the power).
C49IB08A 348
11 Applications
Hint:
Be aware that power values of monomode instruments can not be directly
applied similarily in multimode equipments. Due to the different filed density
the heating rates will differ.
• For most syntheses we recommend a temperature profile as the optimal

progress of a reaction is very dependent on the reaction temperature. The
temperature is controlled by a p/T-sensor in Rotor 16 and Rotor 48 and the
T-probe in Rotor 8S.
• An optional calibration unit is available which allows automatic calibration of

all sensors in the laboratory by the user. This enables you to monitor
syntheses according to ISO standards, for example. The pressure sensor
requires no maintenance and does not need to be calibrated.
11.2.3.2 Creating Your Own Synthesis Methods
• Particularly in the field of research and development (R&D) it is becoming

increasingly popular to develop new syntheses using microwave technology.
The simplest way of creating new methods is to adapt an existing method
which uses similar chemistry, i.e. similar reaction partners, under
comparable conditions. This makes the optimization phase very short.
• For completely new syntheses, we recommend starting with small amounts

and diluted solutions to investigate the behavior of the reaction mixture in the
microwave field. Any spontaneous reactions or unexpected occurences in
the reaction can be intercepted by the safety systems.
• Due to the pressure control at every position, Rotor 8S enables you to use
different reagent mixtures in one run. This allows you to determine the
suitable proportions of reaction partners. The minimum volume of 12 mL also
helps keep the consumption of chemicals as low as possible. Once you have
found the ideal ratio, you can optimize the time/temperature or pressure
profile. The optimized method can then be stored in the method library for
future use.
• The adaptation of known, conventional (thermal) syntheses can be

performed according to general guidelines for the transformation of thermal
methods to microwave-assisted reactions. This often requires changing the
solvent in the protocol to make use of the effectiveness of microwave
irradiation. Take the changing temperature and pressure properties into
consideration (low boiling point, higher vapor pressure, changed polarity,
etc.). This adaptation requires a high degree of experience and intuition from
someone skilled in organic synthesis. Anton Paar cannot give any
recommendations here.
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11.2.3.3 Reagents and Sample Volumes
• The operating volume of the reaction vessels is limited to 60 mL to prevent

pressure building up too rapidly. In theory, reactions in high-boiling solvents
which build up no or only low pressure can be carried out in larger volumes.
However, there is always the risk of spontaneous reactions and sudden
pressure peaks. We therefore recommend not to exceed the defined
maximum loperating volume.
• The minimum filling volume of the reaction vessels is 6 mL unless you use
the internal T-probe in Rotor 8S - then the minimum filling volume is 12 mL in
the reference vessel. However, to make sure that the weight is evenly
distributed, all vessels should be filled with the same volume.
• Unlike Rotor 8S, Rotor 16 and Rotor 48 allows pressure measurement in

only one reference vessel. For this reason make sure that the most
concentrated or most reactive sample is filled into the reference vessel.
Although Rotor 16 and Rotor 48 allow the parallel synthesis of varying
compounds, do not use completely different reaction mixtures in the same
run.
• As well as the volume, the amount of substrate is also limited, especially

when it is a solid. To ensure sufficient mixing and optimal reagent
conversion, we recommend to apply max. 5 g solid substrates per vessel.
• If the reaction results in precipitating product upon cooling, the batch size
should be selected to form no more than 20 g of product per vessel.
11.2.3.4 Power Profile
• When programming a new method, always perform preliminary experiments

to gain information about the behavior of the reaction mixture. Start this
pretest with small amounts of diluted solutions and a long ramp; select the
power so that it is not too high. Check the pressure and temperature during
the reaction and check the vessels and materials after the experiment. If the
synthesis gives the desired results, you can move up to more concentrated
solutions and begin to optimize the temperature and time conditions.
11.2.3.5 Temperature Profile
• In contrast to the power profile, the temperature profile is independent of the

number of used vessels. However, it is best to start the pretest with small
amounts of diluted solutions and a long ramp to the desired end
temperature. This allows safe determination of any temperature peaks due
to exothermal reactions. These temperature peaks should be taken into
consideration when programming the method to prevent overheating and
destruction of used substrates.
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11.2.3.6 Spontaneous Reactions
• To prevent spontaneous reactions, you can either define a longer ramp or

add an intermediate step. This allows the samples to heat up slowly and start
the reaction. When developing new methods or new synthesis approaches,
in particular, spontaneous reactions may occur. In low concentration
solutions these spontaneous reactions are not problematic. In concentrated
solutions they may lead to rupture of the safety disk or damage to vessels.
Always begin to test new reaction mixtures in small amounts. Spontaneous
reactions can usually be minimized by changing the reaction mixtures and
optimizing the reaction conditions.
11.2.4 Interpretation of Results
• The reaction progress is usually checked after the experiment using

conventional analysis methods (DC, HPLC, LCMS, etc.).
• If the result of the reaction fails to meet expectations, this can be due to any
of the following reasons:
- if the conversion is incomplete, the reaction time is too short and/or the
temperature is too low
- if the substrate is destroyed, the temperature is too high
- the reaction mixture is unsuitable. Consider using catalysts, passive
heating elements or changing the solvent
• If the synthesis was successful, work up the reaction mixture according to

your synthesis specifications.
Hint:
Do not use mechanical force when transferring the sample. Only use a soft
plastic spatula in order not to damage the liner or quartz vessels.
Damaged or scratched vessels should not be used as the pressure safety
limit is no longer guaranteed.
11.2.5 Power Reduction by the Instrument
By analyzing the control parameters of the instrument, the reaction behavior of a

sample can be described very precisely.
The time required to reach the first limit is defined as the "power reduction time"
and is indicated in mm:ss together with the abbreviation of the control
parameter.
The most important abbreviations for control parameters are listed below:
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• T: Internal temperature control
• I: Infrared temperature control
• P: Pressure limit control
• r: Pressure rate control (software, range between 0.1 – 3.0 bar/s)
• R: Pressure rate alarm (hardware, > 3.0 bar/s)
• S: Power consumption control
• O: Overrange (p-, T- or IR-limit significantly exceeded)
• o: Overheating of the pressure sensor (Rotor 8S)
• U: User terminates the program
• M: Magnetron overtemperature
Knowledge of the activated control parameters is advantageous for further

method development and method optimizing.
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12 Appendix
12.1 Addresses
Anton Paar GmbH
Anton-Paar-Str. 20
A-8054 Graz / AUSTRIA - EUROPE
Tel: +43 316 257-0
Fax: +43 316 257 257
info@anton-paar.com
www.anton-paar.com
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12.2 Packing the Synthos 3000 and the Rotors
12.2.1 Packing the Instrument
If you need to transport the instrument, use the original packaging. This is the best
protection against transport damages.
1. Place the accessory parts such as the exhaust hose, mains cable and the
seal forming tool into the supplied accessory carton. Close the carton and
seal it using adhesive tape.
2. Do not use metal clamps to avoid scratches on the PTFE surface of the
instrument!
Fig. 12 - 6 Standard accessories
3. Open the door of the instrument and place the carton inside the microwave
cavity of Synthos 3000.
4. Apply the protective sheet to the inner side of the door and close the door.
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12 Appendix
carton with accessories
protective sheet
Fig. 12 - 7 Instrument with protective sheet and carton
5. Insert the transport lock (white L-shaped foam part) of the exhaust unit at the
rear of Synthos 3000. Insert the white foam piece between the top of the
exhaust unit and the top cover.
Transport lock between

the exhaust module
and top cover.
Fig. 12 - 8 Transport lock of the exhaust module
6. Place the wooden pallet on the floor and position the bottom carton on the
pallet. Insert the bottom foam piece into the bottom carton. The recess for
the exhaust unit helps you identify the front and rear of the foam piece.
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12 Appendix
rear
recess for the

exhaust unit
front
Fig. 12 - 9 Inserting the bottom foam piece into the carton
Warning:
Do not use the door for lifting or carrying the instrument!
Lift and carry the instrument by gripping the base at the right and left side (2
people are required).
7. Insert the instrument into the carton. Do not lift or carry the instrument by the
door.
8. Put the carton sleeve on the instrument. Ensure that the bottom corners of
the carton sleeve fit inside the carton.
Fig. 12 - 10 Putting the carton sleeve on the instrument
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12 Appendix
9. Place the foam piece on the instrument.
Fig. 12 - 11 Inserted foam piece
10. Close the carton and seal it using adhesive tape. Use belts to secure the
carton on the wooden pallet.
11. The instrument is now ready for shipment.
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12.2.2 Packing the Rotors
The rotors are delivered in a separate shipping cartons. All rotors are packed
similarly. The instructions below are shown with Rotor 16 but can be applied to all
other rotor types.
1. Open the rotor by removing the lid. Put the foam piece (transport lock) on the
rotor and close the rotor with the rotor lid. (Hint: Rotor 8S is delivered without
this foam piece)
Fig. 12 - 12 Putting on the transport lock
2. Put the rotor in the carton.
Fig. 12 - 13 Putting the rotor in the carton
3. Put the packaging foam piece on the rotor.
C49IB08A 358
12 Appendix
Fig. 12 - 14 Putting on the foam piece
4. Close the top of the carton.
Fig. 12 - 15 Closing the carton with the rotor
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12 Appendix
12.3 Technical Data of the Instrument
12.3.1 Synthos 3000 Microwave Oven
Power supply: AC 230 V ± 10 % 50 Hz ± 0.3 Hz or

AC 230 V ± 10 % 60 Hz ± 0.3 Hz
Power consumption: 3680 VA
Installed microwave power: 1700 W, delivered from 2 magnetrons
Microwave output power: 1400 W, limitations for increased service life

of magnetrons
Microwave power control: Unpulsed control mode over whole power

range. Adjustable in 1 W increments.
Magnetron frequency: 2455 MHz
Mass: 74 kg
Dimensions (WxDxH): 60 x 72 x 74 cm
(23.6 x 28.3 x 29 inch)
Cavity dimensions (WxDxH): 45 x 42 x 35 cm

(17.7 x 16.5 x 13.8 inch)
Cavity volume: 66 L
Cavity material: Stainless steel with multilayer fluoropolymer

coating
Exhaust unit capacity: 190 m3/h max., adjustable in 4 steps
Rotor speed: 3 rpm
System control: Microprocessor (Motorola 68xxx series)

Library of tested methods, freely extendable
by the user (up to 600 methods)
Storage of last 9 hours of operation (if max.
240 methods used) (5 hours storage if 600
methods used).
Display: Illuminated LCD, 240 x 128 pixel

(40 characters x 16 lines)
Input elements: Spill-proof keypad, 8 keys (Start, Stop, Esc,

5 function keys)
External keyboard: AT 5-pin DIN 41524 connector
Serial interface: RS 232C, 9-pin SUB-D (2x); male
Parallel printer interface: Centronics 25-pin SUB-D; female
Calibrator: 15-pin SUB-D; female
Auxiliary (AUX): 25 pin; male; Connection for accessory

(Solvent Sensor Accessory)
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12 Appendix
Fuses: T 16 A thermal (in the mains switch)

T 6.3 A / 250 V
T 2.5 A / 250 V
T 2 A / 250 V
T 1 A / 250 V
T 4 A / 250 V (in the exhaust unit)
F 4 A / 250 V
T 500 mA / 250 V
Ambient temperature: 15 to 35 °C
Relative humidity max.: 80 %, non-condensing
Altitude: 0-2000 m
Noise level / 66 dBA / 0.04 Pa under optimal installation

sound pressure level: conditions, cooling at fan step 2 (120° phase
angle), measured at the front.
Overvoltage class: II
Pollution degree: 2
Protection class: I, according to VDE 0106
Protection degree: IP 20, according to IEC 144
EMC ambient conditions: Laboratory use
Complies with: Electromagnetic compatibility (89/336/EEC

+ changes 92/31/EEC, 93/68/EEC)
Equipment for laboratory use
EN 61326 + A1 + A2:2001
RF emissions EN 50081-1: 1993
RF susceptibility EN 50082-1: 1997
ISM equipment FCC part 18
Low Voltage Directive (73/23/EEC + change
93/68/EEC)
Safety EN 61010-1:2001+
EN 61010-2-081:2002 +
EN 61010-2-010:2003
Safety of laser products (LED)
IEC 60825-1:1993 + A2:2001
EN 60825-1:1994 + A11:1996 + A2:2001
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12 Appendix
12.3.2 Options
p/T-sensor accessory: For one reference vessel in 16-position and

in 48-position rotor.
Temperature measuring range: 0 to 280 °C
Uncertainty: ± 1%
Pressure measuring range: 0 to 86 bar
Uncertainty: ± 0.2 bar
T-probe S: For precise temperature measurement in

one reference vessel in Rotor 8S. Requires
a seal holder with immersion tube for
operation.
Temperature measuring range: 0 to 300 °C
Uncertainty: ± 1%
Temp. calibration accessory: Calibration tool for automated calibration of

all temperature sensors of the
Synthos 3000.
The software supported calibration can be
performed by the customer in 15 min in a
range between 40 °C and 220 °C (for inner
temperature sensors) and 100 °C and 220 °C
(for IR temperature sensor).
12.3.3 Rotor 48MF50
Number of vessels: 48
Vessel design: PEEK pressure jacket with PFA liner

Screw cap with metal safety disk and
directed gas release
Volume: 50 mL
Controlled operation 20 bar (290 psi)

pressure:
Pressure max.: 30 bar (435 psi)
Test pressure: 140 bar (2000 psi) / 1 min.
Temperature max.: 200 °C for 30 minutes at 20 bar
Overpressure protection: Metal safety disk
Reaction control: Reference vessel with pressure and

temperature sensor
Dimensions (D x H): 41´ x 33 cm (16´ x 13 inch)
Mass: 13.1 kg
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12 Appendix
12.3.4 Rotor 16 MF100
Vessel design: PEEK pressure jacket with PTFE-TFM liner

Screw cap with metal safety disk and venting
screw
Volume: 100 mL

pressure:
Temperature max.: 190 °C for 30 minutes at 20 bar
Reaction control: Optional reference vessel with p/T sensor

accessory; IR sensor
Dimensions (D x H): 40 x 33 cm (15.7 x 13 inch)
Mass: 10.5 kg
12.3.5 Rotor 16 HF100
Vessel design: Ceramic pressure jacket with PTFE-TFM

liner
Screw cap with metal safety disk and venting
screw
Volume: 100 mL

pressure:
Temperature max.: 240 °C, at 40 bar
Reaction control: Optional reference vessel p/T sensor

accessory; IR sensor
Dimensions (D x H): 40 x 33 cm (15.7 x 13 inch)
Mass: 13.8 kg
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12 Appendix
12.3.6 Rotor 8SXF100
Vessel design: Ceramic pressure jacket with PTFE-TFM

liner; Seal holder with safety disk and
venting screw; Vessel jacket consisting of
protective casing and protective cap.
Volume: 100 mL

pressure:
Temperature max.: 260 °C at 60 bar
Reaction control: Simultaneous pressure sensor for all

vessels; IR sensor and optional T-Probe for
one reference vessel
Dimensions (D x H): 39 x 32 cm (15.3 x 12.6 inch)
Mass: 14.9 kg
12.3.7 Rotor 8SXQ80
Vessel design: Quartz reaction vessel; Seal holder with

safety disk and venting screw; Vessel jacket
consisting of protective casing and
protective cap.
Volume: 80 mL

pressure:
Temperature max.: 300 °C at 80 bar
Reaction control: Simultaneous pressure sensor for all

vessels; IR sensor and optional T-Probe for
one reference vessel
Dimensions (D x H): 39 x 32 cm (15.3 x 12.6 inch)
Mass: 14.8 kg
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12 Appendix
12.4 List of Spare Parts
Detailed information about the Spare Parts for Synthos 3000 can be found in the
Product Description List which is additionally stored on the CD.
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12 Appendix
12.5 Safety Certification
Fig. 12 - 16 ETL-Certification
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Fig. 12 - 17 GS-Certification
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12 Appendix
12.6 CE Declaration of Conformity
Fig. 12 - 18 Declaration of Conformity
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12 Appendix
12.7 Safety Declaration for Repair and Malfunction

Report
If you experience technical problems with Synthos 3000, Anton Paar GmbH
provides quick and expert support. For technical support, contact our local
representative or Anton Paar GmbH directly.
If you have a technical question or complaint, please fill in both, the Safety
Declaration for Repair form and the Malfunction Report as detailed as possible
and send it (with the defective part, if possible) to our local representative or to
Anton Paar GmbH directly.
Filling the Malfunction Report in completely simplifies troubleshooting and speeds

up the repair process.
C49IB08A 369
12 Appendix
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12 Appendix
C49IB08A 371

Synthos 3000 Reference Manual

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Published by Anton Paar

Address: Anton Paar GmbH

Document number C49IB08A

Synthos 3000 is a scale-up-instrument for microwave-assisted chemical

Fig. 1 - 1 Synthos 3000

Parallel rotors with up to 48 positions can be used to carry out temperature-

Synthos 3000 excels in:

This makes Synthos 3000 a high-performance instrument for the production of

2.1 Symbols in the Instruction Manual

2.2 Safety Symbols Applied to the Instrument

Warning screen located on the front door of the instrument.

Symbol located on the rotors: Refer to the manual!

Warning screen located on Rotor 48.

Symbol located on the calibration accessory: Caution - hot surface!

3.1 General Safety Instructions for Synthos 3000

• The operation of the pressure vessels may be liable to individual national

• This instrument is not designed for operation in an explosive atmosphere.

• Synthos 3000 is equipped with strong permanent magnets. Keep the

magnetic read-write band, pacemakers or similar items, magnetic storage

• Do not lift or carry the instrument by its door.

• Under adverse conditions chemical syntheses may lead to violent,

• The hood must be closed immediately after starting an experiment.

• Do not to store containers with flammable reagents or other ignitable

• Indoor use only!

• Synthos 3000 should be supervised at all times during operation.

leakage may consist. Do not continue to operate Synthos 3000 unless an

3.2 Safety Instructions for Chemical Synthesis

• Synthos 3000 is a scale-up instrument for use with optimized microwave

• Never carry out syntheses in open vessels in the Synthos 3000.

• Do not mark plastic parts of pressure vessels or rotors of microwave systems

• Make sure to apply reaction mixtures with adequate coupling efficiency. If

• Allow the vessels to cool down to a vessel interior temperature below 60 °C

• Do not operate Synthos 3000 if a fault is suspected.

• After a (very unlikely) explosion of a vessel, do not continue with synthesis

3.3 Unexpected Operation Behavior

Although highly unlikely, it is still possible that a reaction procedure is terminated

After a power failure:

Fig. 3 - 1 Manual activation of safety ccoling

After an exhaust unit failure:

After a system failure:

In case of fire inside the microwave cavity:

• As a precaution keep a fire extinguisher ready or call for corresponding

• Due to the possibility of escaping fumes it is recommended to switch on the

4 Technical Description of Synthos 3000

4.1 Working Principle

A built-in microcontroller controls the reaction processes, stores a method library

In addition the surface temperature of the reaction vessels is measured using an

4.2 Fields of Application

• unpulsed continuously adjustable microwave energy over the whole power

• direct scalability, from milliliters to liters without changing the reaction

• the highest available pressure and temperature limits

• innovative and practical rotor and vessel design

• efficient vessel cooling

• easy-to-operate program functions.

As well as conventional microwave-assisted synthesis, the following applications

• Reactions under pressure with individually applied reactant or inert gas

• Efficient high-temperature synthesis with low absorbing solvents utilizing

• Near critical water chemistry

4.3 Technical Description of the Instrument

Door opener button

Graphic display Keypad foil * (not visible)

Space for the

Fig. 4 - 1 Front view of Synthos 3000