Buchi Lyovapor L-300 User manual

Lyovapor™ L-300/L-300 Pro
Operation Manual
1153869 | D en

Imprint
Product Identification:
Operation Manual (Original) Lyovapor™ L-300/L-300 Pro
1153869
Publication date: 10.2022
Version D
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience,
especially with respect to structure, illustrations and technical details.
This manual is copyrighted. Information from it may neither be reproduced, distributed, or used for
competitive purposes, nor made available to third parties. The manufacture of any component with the
aid of this manual without prior written agreement is also prohibited.

Büchi Labortechnik AG Table of contents
Operation Manual Lyovapor™ L-300/L-300 Pro iii
Table of contents
1 About this document...........................................................................................................7
1.1 Connected devices ................................................................................................................7
1.2 Warning notices in this document..........................................................................................7
1.3 Symbols.................................................................................................................................7
1.3.1 Warning symbols ......................................................................................................7
1.3.2 Mark-ups and symbols .............................................................................................8
1.4 Trademarks ...........................................................................................................................8
2 Safety....................................................................................................................................9
2.1 Proper use .............................................................................................................................9
2.2 Use other than that intended .................................................................................................9
2.3 Staff qualification ...................................................................................................................9
2.4 Location of warning signs on the product ............................................................................10
2.4.1 Location of warning signs on the product (front view) ............................................10
2.4.2 Location of warning signs on the product (rear view) .............................................10
2.4.3 Location of warning signs on the ice condenser.....................................................11
2.5 Residual risks ......................................................................................................................12
2.5.1 Faults during operation...........................................................................................12
2.5.2 Glass and acrylic breakage ....................................................................................12
2.5.3 Low internal pressure .............................................................................................12
2.5.4 Cold and hot surfaces.............................................................................................12
2.6 Personal protective equipment ............................................................................................12
2.7 Modifications........................................................................................................................13
3 Product description...........................................................................................................14
3.1 Description of function .........................................................................................................14
3.1.1 Freezing phase.......................................................................................................14
3.1.2 Main drying phase ..................................................................................................14
3.1.3 Secondary-drying phase.........................................................................................15
3.2 Configuration .......................................................................................................................15
3.2.1 Front View ..............................................................................................................15
3.2.2 Rear view................................................................................................................17
3.2.3 Side connections ....................................................................................................18
3.2.4 Control panel ..........................................................................................................19
3.2.5 Pro control panel ....................................................................................................19
3.3 Type plate............................................................................................................................19
3.4 Scope of delivery .................................................................................................................20
3.5 Refrigerant Specification .....................................................................................................20
3.5.1 Refrigerant Specification (Low temperature) ..........................................................20
3.5.2 Refrigerant Specification (High temperature) .........................................................21
3.6 Technical data .....................................................................................................................21
3.6.1 Lyovapor™ L-300 ...................................................................................................21
3.6.2 Ambient conditions .................................................................................................23
3.6.3 Materials .................................................................................................................23
4 Transport and storage ......................................................................................................25
4.1 Transport .............................................................................................................................25
4.2 Storage ................................................................................................................................25

Table of contents Büchi Labortechnik AG
iv Operation Manual Lyovapor™ L-300/L-300 Pro
5 Installation..........................................................................................................................26
5.1 Installation site.....................................................................................................................26
5.2 Putting the instrument in operation......................................................................................27
5.2.1 Preparing the instrument ........................................................................................27
5.2.2 Establishing electrical connections.........................................................................27
5.2.3 Fitting the fresh water connections.........................................................................28
5.2.4 Fitting fill-level sensor in water tank (optional)........................................................29
5.2.5 Fitting the drain tubes .............................................................................................29
5.2.6 Fitting the fill-level sensor on the receiving vessel (optional) .................................30
5.2.7 Connecting the coolant...........................................................................................31
5.2.8 Fitting pressure sensors (option) ............................................................................31
5.2.9 Connecting inert gas (option) .................................................................................33
5.2.10 Fitting an air filter (option).......................................................................................34
5.3 Commissioning the vacuum pump ......................................................................................35
5.4 Establishing LAN connection...............................................................................................35
5.4.1 Requirements for local network settings.................................................................35
5.4.2 Preparing the instrument for app using ..................................................................36
5.4.3 Enabling BUCHI Cloud access...............................................................................36
5.5 Insert SD card (Pro control panel only) ...............................................................................36
6 Operating the control panel..............................................................................................38
6.1 Layout of the control panel ..................................................................................................38
6.2 Function bar.........................................................................................................................39
6.3 Menu bar .............................................................................................................................39
6.3.1 Start menu ..............................................................................................................40
6.3.2 Favourites menu..................................................................................................... 40
6.3.3 Configuration menu ................................................................................................40
6.3.4 Messages menu .....................................................................................................46
6.4 Status bar ............................................................................................................................47
6.5 Carrying out freeze-drying ...................................................................................................48
6.5.1 Preparing the instrument ........................................................................................48
6.5.2 Starting freeze-drying .............................................................................................49
6.5.3 Editing parameters while the process is running ....................................................49
6.5.4 Ending freeze-drying ..............................................................................................50
6.5.5 Shutting down the instrument .................................................................................50
6.5.6 Switching off the instrument ...................................................................................51

Büchi Labortechnik AG Table of contents
Operation Manual Lyovapor™ L-300/L-300 Pro v
7 Operating Pro control panel .............................................................................................52
7.1 Layout of Pro control panel..................................................................................................52
7.2 Function bar.........................................................................................................................52
7.3 Other symbols on the control panel.....................................................................................54
7.4 Menu bar .............................................................................................................................54
7.4.1 Start menu ..............................................................................................................54
7.4.2 Favourites menu..................................................................................................... 55
7.4.3 Method menu..........................................................................................................55
7.4.4 Configuration menu ................................................................................................55
7.4.5 Messages menu .....................................................................................................61
7.5 Status bar ............................................................................................................................62
7.6 Editing a method..................................................................................................................64
7.6.1 Creating a new method ..........................................................................................64
7.6.2 Changing the name of a method ............................................................................64
7.6.3 Setting the sample collapse temperature ...............................................................65
7.6.4 Setting the gas type................................................................................................65
7.6.5 Setting the shelf loading temperature..................................................................... 65
7.6.6 Setting the steps of a method................................................................................. 66
7.6.7 Setting the phases of a method.............................................................................. 67
7.7 Deleting a method ...............................................................................................................69
7.8 Setting end point definitions ................................................................................................69
7.8.1 Pressure difference test..........................................................................................70
7.8.2 Temperature difference test ...................................................................................71
7.8.3 Pressure rise test....................................................................................................72
7.9 Performing freeze-drying using a method [Pro control panel] .............................................74
7.9.1 Preparing the instrument ........................................................................................74
7.9.2 Selecting a method................................................................................................. 74
7.9.3 Starting freeze-drying .............................................................................................75
7.9.4 Changing parameters while the process is running................................................76
7.9.5 Ending freeze-drying ..............................................................................................76
7.9.6 Shutting down the instrument .................................................................................76
7.9.7 Switching off the instrument ...................................................................................77
7.10 Performing freeze-drying manually [Pro control panel] .......................................................77
7.10.1 Preparing the instrument ........................................................................................77
7.10.2 Starting freeze-drying .............................................................................................77
7.10.3 Editing parameters while the process is running ....................................................78
7.10.4 End point definition .................................................................................................78
7.10.5 Ending freeze-drying ..............................................................................................79
7.10.6 Shutting down the instrument .................................................................................79
7.10.7 Switching off the instrument ...................................................................................80
8 Operating top-mount drying racks ..................................................................................81
8.1 Operating stoppering acrylic drying chamber ......................................................................81
8.2 Operating manifold acrylic drying chamber (heatable shelves)........................................... 84
8.3 Operating manifold acrylic drying chamber (non-heatable shelf) ........................................87
8.4 Operating acrylic drying chamber (heatable shelf) .............................................................. 90
8.5 Operating acrylic drying chamber (non-heatable shelf)....................................................... 92
8.6 Operating manifold drying rack............................................................................................94
8.7 Determining the number of flasks........................................................................................96
8.8 Operating manifold valves ...................................................................................................96

Table of contents Büchi Labortechnik AG
vi Operation Manual Lyovapor™ L-300/L-300 Pro
9 Cleaning and servicing .....................................................................................................97
9.1 Regular maintenance work..................................................................................................97
9.2 Performing a vacuum test....................................................................................................98
9.3 Performing a leak test..........................................................................................................99
9.3.1 Performing a leak test with a drying chamber ........................................................99
9.3.2 Performing leak test with a manifold drying rack .................................................. 101
9.4 Cleaning the ice condenser ............................................................................................... 103
10 Help with faults ................................................................................................................104
10.1 Troubleshooting.................................................................................................................104
10.2 Faults, possible causes and remedies ..............................................................................104
10.3 Locating leaking manifold valve.........................................................................................105
10.4 Manually defrosting ice condenser .................................................................................... 105
10.5 Error messages .................................................................................................................106
11 Taking out of service and disposal................................................................................110
11.1 Disposal.............................................................................................................................110
11.2 Returning the instrument ...................................................................................................110
12 Appendix ..........................................................................................................................111
12.1 Spare parts and accessories ............................................................................................. 111
12.1.1 Accessories ..........................................................................................................111
12.1.2 Further accessories .............................................................................................. 111
12.1.3 Spare parts ........................................................................................................... 112
12.1.4 Top-mount drying rack accessories......................................................................114
12.1.5 Software ...............................................................................................................116

Büchi Labortechnik AG About this document | 1
Operation Manual Lyovapor™ L-300/L-300 Pro 7/118
1 About this document
This operation manual is applicable for all variants of the instrument.
Read this operation manual before operating the instrument and follow the
instructions to ensure safe and trouble-free operation.
Keep this operation manual for later use and pass it on to any subsequent user or
owner.
BÜCHI Labortechnik AG accepts no liability for damage, faults and malfunctions
resulting from not following this operation manual.
If you have any questions after reading this operation manual:
uContact BÜCHI Labortechnik AG Customer Service.
https://www.buchi.com/contact
1.1 Connected devices
In addition to these operating instructions, follow the instructions and specifications
in the documentation for the connected devices.
1.2 Warning notices in this document
Warning notices warn you of dangers that can occur when handling the device.
There are four danger levels, each identifiable by the signal word used.
Signal word Meaning
DANGER Indicates a danger with a high level of risk which could result in
death or serious injury if not prevented.
WARNING Indicates a danger with a medium level of risk which could result in
death or serious injury if not prevented.
CAUTION Indicates a danger with a low level of risk which could result in mi-
nor or medium-severity injury if not prevented.
NOTICE Indicates a danger that could result in damage to property.
1.3 Symbols
The following symbols are displayed in this operation manual or on the device:
1.3.1 Warning symbols
Symbol Meaning
General warning
Breakable items
Hand injuries

1 | About this document Büchi Labortechnik AG
8/118 Operation Manual Lyovapor™ L-300/L-300 Pro
Symbol Meaning
Hot surface
Explosive substances
Dangerous electrical voltage
Flammable substances
Instrument damage
1.3.2 Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
RThis character draws attention to a requirement that must be met before the
instructions below are carried out.
uThis character indicates an instruction that must be carried out by the user.
ðThis character indicates the result of a correctly carried out instruction.
Mark-up Explanation
Window
Software Windows are marked-up like this.
Tab
Tabs are marked-up like this.
Dialog
Dialogs are marked-up like this.
[Button] Buttons are marked-up like this.
[Field names] Field names are marked-up like this.
[Menu / Menu item] Menus or menu items are marked-up like this.
Status Status is marked-up like this.
Signal Signals are marked-up like this.
1.4 Trademarks
Product names and registered or unregistered trademarks that are used in this
document are used only for identification and remain the property of the owner in
each case.

Büchi Labortechnik AG Safety | 2
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2 Safety
2.1 Proper use
The Lyovapor™ L-300 is used for freeze-drying solid materials in ampoules, vials,
trays, round-neck or wide-neck flasks and is exclusively intended for that purpose.
The Lyovapor™ L-300 can be used in laboratories for the following tasks:
Sublimating and condensing water-based samples
Sublimating and condensing samples containing solvents
2.2 Use other than that intended
Use of any other kind than that described in the section Chapter2.1 "Proper use",
page9 and any application that does not comply with the technical specifications
(see Chapter3.6 "Technical data", page21) constitutes use other than that
intended.
In particular, the following applications are not permissible:
Use of the instrument in an environment with a potential risk of explosion or
areas which require explosion-safe apparatus.
Use of the instrument for processing substances outside of research and
development.
Production and processing of substances that can lead to spontaneous reactions,
such as explosives, metal hydrides or solvents that can form peroxides.
Processing with explosive gas mixtures.
Drying samples with high solvent concentrations without special safety
precautions.
Damage or hazards attributable to use of the product other than as intended are
entirely at the risk of the operator alone.
2.3 Staff qualification
Unqualified persons are unable to identify risks and are therefore exposed to greater
dangers.
The instrument may only be operated by suitably qualified laboratory staff.
These operating instructions are aimed at the following target groups:
Users
Users are persons that meet the following criteria:
They have been instructed in the use of the instrument.
They are familiar with the contents of these operating instructions and the
applicable safety regulations and apply them.
They are able on the basis of their training or professional experience to assess
the risks associated with the use of the instrument.

2 | Safety Büchi Labortechnik AG
10/118 Operation Manual Lyovapor™ L-300/L-300 Pro
Operator
The operator (generally the laboratory manager) is responsible for the following
aspects:
The instrument must be correctly installed, commissioned, operated and serviced.
Only suitably qualified staff may be assigned the task of performing the
operations described in these operating instructions.
The staff must comply with the local applicable requirements and regulations for
safe and hazard-conscious working practices.
Safety-related incidents that occur while using the instrument should be reported
to the manufacturer ([email protected]).
BUCHI service technicians
Service technicians authorized by BUCHI have attended special training courses and
are authorized by BÜCHI Labortechnik AG to carry out special servicing and repair
measures.
2.4 Location of warning signs on the product
2.4.1 Location of warning signs on the product (front view)
The following warning symbols are present on the instrument.
Fig.1: Location of warning signs on the product
General warning
2.4.2 Location of warning signs on the product (rear view)
The following warning symbols are present on the instrument.

Büchi Labortechnik AG Safety | 2
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4
5
Fig.2: Location of warning signs on the product
General warning Dangerous electrical voltage
Flammable substances Keep at least 40 cm clearance to pre-
vent overheating
2.4.3 Location of warning signs on the ice condenser
Fig.3: Location of warning signs on the product
Hand injuries Hot surface

2 | Safety Büchi Labortechnik AG
12/118 Operation Manual Lyovapor™ L-300/L-300 Pro
2.5 Residual risks
The device has been developed and manufactured using the latest technological
advances. Nevertheless, risks to persons, property or the environment can arise if
the device is used incorrectly.
Appropriate warnings in this manual serve to alert the user to these residual
dangers.
2.5.1 Faults during operation
If a device is damaged, sharp edges or exposed electrical wires can cause injuries.
uRegularly check device for visible damage.
uIf faults occur, switch off the device immediately, unplug the power cord and
inform the operator.
uDo not continue to use devices that are damaged.
2.5.2 Glass and acrylic breakage
Broken glass and acrylic can cause severe cuts.
Damaged glass and acrylic components may implode if subjected to a vacuum.
Minor damage to the ground joints impairs the sealing effect and may therefore
diminish sublimination capacity.
uHandle the flask and other glass and acrylic components carefully and do not
drop them.
uAlways place the flasks in a suitable holder when they are not mounted on the
Lyovapor™.
uAlways visually inspect glass and acrylic components for damage every time they
are to be used.
uDo not continue to use glass and acrylic components that are damaged.
uAlways wear protective gloves when disposing of broken glass and acrylic.
2.5.3 Low internal pressure
Evacuating the system reduces the pressure in the drying chamber. This reduced
pressure can cause glass and acrylic components to implode.
uMake sure that all glass and acrylic components are free of damage.
2.5.4 Cold and hot surfaces
The condenser coil and probes can be extremely cold. Heatable shelf areas can be
extremely hot. If touched, hot and cold surfaces can cause skin burns.
uDo not touch cold or hot surfaces or liquids and/or wear suitable protective
gloves.
2.6 Personal protective equipment
Depending on the application, hazards due to heat and/or corrosive chemicals may
arise.
uAlways wear appropriate personal protective equipment such as safety goggles,
protective clothing and gloves.
uMake sure that the personal protective equipment meets the requirements of
the safety data sheets for all chemicals used.

Büchi Labortechnik AG Safety | 2
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2.7 Modifications
Unauthorized modifications can affect safety and lead to accidents.
uUse only genuine BUCHI accessories, spare parts and consumables.
uCarry out technical changes only with prior written approval from BUCHI.
uOnly allow changes to be made by BUCHI service technicians.
BUCHI accepts no liability for damage, faults and malfunctions resulting from
unauthorized modifications.

3 | Product description Büchi Labortechnik AG
14/118 Operation Manual Lyovapor™ L-300/L-300 Pro
3 Product description
3.1 Description of function
The Lyovapor™ is a freeze-dryer in which frozen samples can be gently dried.
The basis of freeze-drying is sublimation. Sublimation refers to the process whereby
a substance transforms directly from the solid to the gaseous state.
The physical process of sublimation can be explained using the solvent water as an
example.
The water is frozen.
The frozen water is transformed into the gaseous state under vacuum at a
pressure below the triple point.
Thus, freeze-drying takes place in three phases:
1. Freezing phase: the sample is frozen at atmospheric pressure.
2. Main drying phase: heat is applied to the frozen sample under a vacuum. The
frozen water is removed by sublimation.
3. Secondary drying phase (only possible with heatable shelves): the trace levels
of water remaining are removed by heating.
The Lyovapor™ consists of an ice condenser and various top-mount drying racks. The
top-mount drying racks can be chosen to suit the availability of the sample being
dried and the requirements of the end product.
The following top-mount drying racks can be used:
Non-heatable and heatable shelves in rack
Trays in rack
Top-mount rack with manifold valves
3.1.1 Freezing phase
In the freezing phase, the liquid sample is transformed to a solid state. Freezing
takes place under atmospheric pressure using a separate freezer, a liquid nitrogen
bath, or a mixture of dry ice and alcohol.
The end of the freezing phase is reached as soon as the water or solvent contained
in the sample has fully crystallized and the entire sample is solidified.
3.1.2 Main drying phase
In the main drying phase, the ice crystals are removed from the sample by
sublimation. Sublimation in the Lyovapor™ takes place under a vacuum with the
addition of thermal energy.
The vacuum pressure is lowered to the level required for sublimation.
For water that is: less than 6.11mbar.
As the ice condenser is colder than the sample being dried, the vapour pressure in
the area of the ice condenser is lower than in the area of the sample. The water
vapour escaping from the sample therefore flows towards the ice condenser. The
water or solvent vapour condenses on the coil of the ice condenser.
If drying chamber without heating is used, heat transfer takes place by convection
and radiation from the surroundings. Control of the thermal energy transferred is
then difficult.

Büchi Labortechnik AG Product description | 3
Operation Manual Lyovapor™ L-300/L-300 Pro 15/118
If a drying chamber with heating is used, heat transfer takes place additionally by
direct contact. The temperature of the heatable shelves is controllable. Control of
the thermal energy transferred is then possible.
Controlling the heat transfer prevents the following critical temperatures for
amorphous and crystalline materials in the solidified sample being reached:
the glass transition temperature Tg' of the frozen sample.
the collapse temperature Tc.
the eutectic temperature Teu.
Above the glass transition temperature and the collapse temperature, the viscosity
of the frozen sample decreases. The reduced viscosity leads to the collapse of the
sample's matrix structure.
Above the eutectic temperature, the sample melts.
During the main drying phase, the product temperature must remain below the
collapse temperature for amorphous materials in the sample.
Sublimation of the ice crystals progresses downwards from the surface of the
product. Above the sublimation boundary, the product is dry ("freeze-dried cake"),
while further inside the product is still frozen.
The end of the main drying phase is reached when all ice crystals have been
removed from the sample.
After the main drying phase, the remaining fluid content in the sample can still be
between 5 to 10%.
3.1.3 Secondary-drying phase
In the secondary drying phase, the unfrozen water is removed from the sample by
desorption. The secondary drying function is performed by the heatable shelves in
the drying chamber of the Lyovapor™.
In the secondary drying phase, the temperature of the heatable shelves is raised and
held for several hours.
The end of the secondary drying phase is reached when the residual moisture in the
sample is between 1% and 5% or the end point determination is succeeded.
3.2 Configuration
3.2.1 Front View
NOTE
For technical specifications of connections, see Chapter3.6 "Technical data",
page21

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16/118 Operation Manual Lyovapor™ L-300/L-300 Pro
6
5
8
9
4
3
2
1
7
Fig.4: Front View
1 Connections for heated shelf
(Lyovapor™ L-300 Pro only)
2 Intermediate valve
3 Ice condenser 4 Optional mounting position for con-
trol panel
5 Ventilation slots 6 Castors
7 Castor brake 8 On/Off master switch
9 User interface

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3.2.2 Rear view
7
6
4
5
11
12
14
15
13
3
2
1
10 98
Fig.5: Rear view
1 Power isolating switch 2 Type plate/Refrigerant specifications
3 Connections for pressure sensors
(option)
4 Side connections
5 Connection for fresh water 6 Connection for condensate drain
hose I
7 Connection for condensate drain
hose II
8 Ventilation slots
9 Gas connection for venting valve 10 Gas connection for pressure regulat-
ing valve
11 Coolant outlet connection 12 Coolant inlet connection
13 Vacuum connection 14 Power cord
15 Vacuum pump connection

3 | Product description Büchi Labortechnik AG
18/118 Operation Manual Lyovapor™ L-300/L-300 Pro
3.2.3 Side connections
NOTE
For technical specifications of connections, see Chapter3.6 "Technical data",
page21
2
1
8
763
4
5
Fig.6: Side connections
1 Connection for pressure sensor
(option)
2 Connection for pressure sensor
(option)
3 Automatic stoppering connection 4 Connection for fresh water sensor
5 Connection for receiving vessel sen-
sor
6 Connection for external pressure
sensors (optional)
7 LAN port 8 Standard BUCHI communication port
(COM)

Büchi Labortechnik AG Product description | 3
Operation Manual Lyovapor™ L-300/L-300 Pro 19/118
3.2.4 Control panel
1
23
Fig.7: Control panel
1 View 2 Function buttons
3 Navigation control
3.2.5 Pro control panel
1
2
Fig.8: Pro control panel
1 Touch-screen display 2 Navigation control
3.3 Type plate
The type plate identifies the instrument. The type plate is located at the rear of the
instrument.

3 | Product description Büchi Labortechnik AG
20/118 Operation Manual Lyovapor™ L-300/L-300 Pro
Buchi Operations India Private Limited
394230 Surat / India
Type xxx
SN xxxxxxxx
Volt xxx-xxx
Freq xx
Power xxxx
Built 20xx
Designed by BUCHI in Switzerland
Made in India
6
5
4
1
3
2
7
8
910 9
Fig.9: Type Plate
1 Company name and address 2 Instrument name
3 Serial number 4 Input voltage range
5 Frequency 6 Power consumption maximum
7 Year of manufacture 8 Product code
9 Approvals 10 Symbol for "Do not dispose of as
household waste"
3.4 Scope of delivery
NOTE
The scope of delivery depends of the configuration of the purchase order.
Accessories are delivered as per the purchase order, order confirmation, and
delivery note.
3.5 Refrigerant Specification
The instrument uses 2 type of compressors to maintain the ice condenser
temperature. For details see Chapter3.6.1 "Lyovapor™ L-300", page21.
3.5.1 Refrigerant Specification (Low temperature)
The refrigerant details are shown on the back of the instrument.