Page 1
Lyovapor™ L-300/L-300 Pro
Operation Manual
1153869 | C en
Page 2
Imprint
Product Identification:
Operation Manual (Original) Lyovapor™ L-300/L-300 Pro
1153869
Publication date: 01.2020
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: quality@buchi.com
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.
Page 3
BÜCHI Labortechnik AG Table of contents
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 .................................................................................................................................... 11
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...................................................................................................................................... 12
3 Product description...........................................................................................................13
3.1 Description of function ....................................................................................................................... 13
3.1.1 Freezing phase ...................................................................................................................... 13
3.1.2 Main drying phase..................................................................................................................13
3.1.3 Secondary-drying phase........................................................................................................14
3.2 Configuration ..................................................................................................................................... 14
3.2.1 Front View..............................................................................................................................14
3.2.2 Rear view ...............................................................................................................................16
3.2.3 Side connections....................................................................................................................17
3.2.4 Control panel..........................................................................................................................17
3.2.5 Pro control panel....................................................................................................................18
3.3 Type plate.......................................................................................................................................... 18
3.4 Scope of delivery ............................................................................................................................... 19
3.5 Refrigerant Specification.................................................................................................................... 19
3.5.1 Refrigerant Specification (Low temperature) .........................................................................19
3.5.2 Refrigerant Specification (High temperature).........................................................................19
3.6 Technical data ................................................................................................................................... 19
3.6.1 Lyovapor™ L-300 ..................................................................................................................19
3.6.2 Ambient conditions.................................................................................................................21
3.6.3 Materials ................................................................................................................................21
4 Transport and storage ......................................................................................................22
4.1 Transport ........................................................................................................................................... 22
4.2 Storage .............................................................................................................................................. 22
Operation Manual Lyovapor™ L-300/L-300 Pro iii
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Table of contents BÜCHI Labortechnik AG
5 Installation..........................................................................................................................23
5.1 Installation site................................................................................................................................... 23
5.2 Putting the instrument in operation.................................................................................................... 24
5.2.1 Preparing the instrument........................................................................................................24
5.2.2 Establishing electrical connections ........................................................................................ 24
5.2.3 Fitting the fresh water connections ........................................................................................ 25
5.2.4 Fitting fill-level sensor in water tank (optional).......................................................................26
5.2.5 Fitting the drain tubes ............................................................................................................26
5.2.6 Fitting the fill-level sensor on the receiving vessel (optional).................................................27
5.2.7 Connecting the coolant .......................................................................................................... 28
5.2.8 Fitting pressure sensors (option) ...........................................................................................28
5.2.9 Connecting inert gas (option).................................................................................................30
5.2.10 Fitting an air filter (option) ...................................................................................................... 31
5.3 Commissioning the vacuum pump..................................................................................................... 31
5.4 Establishing LAN connection............................................................................................................. 32
5.4.1 Requirements for local network settings................................................................................32
5.4.2 Preparing the instrument for app using..................................................................................33
5.4.3 Enabling BUCHI Cloud access .............................................................................................. 33
5.5 Insert SD card (Pro control panel only).............................................................................................. 33
6 Operating the control panel.............................................................................................. 35
6.1 Layout of the control panel ................................................................................................................ 35
6.2 Function bar....................................................................................................................................... 35
6.3 Menu bar............................................................................................................................................ 36
6.3.1 Start menu .............................................................................................................................37
6.3.2 Favourites menu .................................................................................................................... 37
6.3.3 Configuration menu................................................................................................................37
6.3.4 Messages menu.....................................................................................................................42
6.4 Status bar .......................................................................................................................................... 43
6.5 Carrying out freeze-drying ................................................................................................................. 44
6.5.1 Preparing the instrument........................................................................................................44
6.5.2 Starting freeze-drying.............................................................................................................45
6.5.3 Editing parameters while the process is running ...................................................................45
6.5.4 Ending freeze-drying..............................................................................................................45
6.5.5 Shutting down the instrument ................................................................................................46
6.5.6 Switching off the instrument...................................................................................................46
iv Operation Manual Lyovapor™ L-300/L-300 Pro
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BÜCHI Labortechnik AG Table of contents
7 Operating Pro control panel .............................................................................................47
7.1 Layout of Pro control panel................................................................................................................ 47
7.2 Function bar....................................................................................................................................... 47
7.3 Other symbols on the control panel................................................................................................... 49
7.4 Menu bar............................................................................................................................................ 49
7.4.1 Start menu .............................................................................................................................49
7.4.2 Favourites menu .................................................................................................................... 50
7.4.3 Method menu.........................................................................................................................50
7.4.4 Configuration menu................................................................................................................50
7.4.5 Messages menu.....................................................................................................................55
7.5 Status bar .......................................................................................................................................... 56
7.6 Editing a method................................................................................................................................ 57
7.6.1 Creating a new method..........................................................................................................57
7.6.2 Changing the name of a method............................................................................................58
7.6.3 Setting the sample collapse temperature...............................................................................58
7.6.4 Setting the gas type ............................................................................................................... 59
7.6.5 Setting the shelf loading temperature .................................................................................... 59
7.6.6 Setting the steps of a method ................................................................................................ 59
7.6.7 Setting the phases of a method ............................................................................................. 61
7.7 Deleting a method.............................................................................................................................. 63
7.8 Setting end point definitions............................................................................................................... 63
7.8.1 Pressure difference test.........................................................................................................63
7.8.2 Temperature difference test...................................................................................................64
7.8.3 Pressure rise test ...................................................................................................................65
7.9 Performing freeze-drying using a method [Pro control panel] ........................................................... 67
7.9.1 Preparing the instrument........................................................................................................67
7.9.2 Selecting a method ................................................................................................................ 67
7.9.3 Starting freeze-drying.............................................................................................................67
7.9.4 Changing parameters while the process is running...............................................................68
7.9.5 Ending freeze-drying..............................................................................................................68
7.9.6 Shutting down the instrument ................................................................................................69
7.9.7 Switching off the instrument...................................................................................................69
7.10 Performing freeze-drying manually [Pro control panel]...................................................................... 69
7.10.1 Preparing the instrument........................................................................................................69
7.10.2 Starting freeze-drying.............................................................................................................70
7.10.3 Editing parameters while the process is running ...................................................................70
7.10.4 End point definition ................................................................................................................71
7.10.5 Ending freeze-drying..............................................................................................................71
7.10.6 Shutting down the instrument ................................................................................................71
7.10.7 Switching off the instrument...................................................................................................72
8 Operating top-mount drying racks ..................................................................................73
8.1 Operating stoppering acrylic drying chamber .................................................................................... 73
8.2 Operating manifold acrylic drying chamber (heatable shelves)......................................................... 76
8.3 Operating manifold acrylic drying chamber (non-heatable shelf) ...................................................... 79
8.4 Operating acrylic drying chamber (heatable shelf) ............................................................................ 81
8.5 Operating acrylic drying chamber (non-heatable shelf)..................................................................... 83
8.6 Operating manifold drying rack.......................................................................................................... 85
8.7 Determining the number of flasks...................................................................................................... 86
8.8 Operating manifold valves ................................................................................................................. 87
Operation Manual Lyovapor™ L-300/L-300 Pro v
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Table of contents BÜCHI Labortechnik AG
9 Cleaning and servicing .....................................................................................................88
9.1 Regular maintenance work................................................................................................................ 88
9.2 Performing a vacuum test.................................................................................................................. 89
9.3 Performing a leak test........................................................................................................................ 90
9.3.1 Performing a leak test with a drying chamber........................................................................90
9.3.2 Performing leak test with a manifold drying rack ...................................................................92
9.4 Cleaning the ice condenser ............................................................................................................... 93
10 Help with faults ..................................................................................................................95
10.1 Troubleshooting................................................................................................................................. 95
10.2 Faults, possible causes and remedies............................................................................................... 95
10.3 Locating leaking manifold valve......................................................................................................... 96
10.4 Manually defrosting ice condenser .................................................................................................... 96
11 Taking out of service and disposal.................................................................................. 97
11.1 Disposal............................................................................................................................................. 97
11.2 Returning the instrument ................................................................................................................... 97
12 Appendix ............................................................................................................................98
12.1 Spare parts and accessories ............................................................................................................. 98
12.1.1 Accessories............................................................................................................................98
12.1.2 Further accessories ...............................................................................................................98
12.1.3 Spare parts ............................................................................................................................99
12.1.4 Top-mount drying rack accessories.....................................................................................101
12.1.5 Software...............................................................................................................................104
vi Operation Manual Lyovapor™ L-300/L-300 Pro
Page 7
BÜCHI Labortechnik AG About this document | 1
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:
u Contact BÜCHI Labortechnik AG Customer Service.
https://www.buchi.com/contact
1.1 Connected devices
In addition to these operating instructions, you should also 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
WARNING Indicates a danger with a medium level of risk which could result in
CAUTION Indicates a danger with a low level of risk which could result in mi-
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
death or serious injury if not prevented.
death or serious injury if not prevented.
nor or medium-severity injury if not prevented.
General warning
Breakable items
Hand injuries
Hot surface
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1 | About this document BÜCHI Labortechnik AG
Symbol Meaning
Explosive substances
Dangerous electrical voltage
Flammable substances
Device damage
1.3.2 Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
R This character draws attention to a requirement that must be met before the in-
structions below are carried out.
u This character indicates an instruction that must be carried out by the user.
ð This character indicates the result of a correctly carried out instruction.
Mark-up Explanation
Win dow Software Windows are marked-up like this.
Tab Tabs are marked-up like this.
Dia log 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.
8/106 Operation Manual Lyovapor™ L-300/L-300 Pro
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BÜCHI Labortechnik AG Safety | 2
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 Chapter2.1 "Proper use",
page9 and any application that does not comply with the technical specifications
(see Chapter3.6 "Technical data", page19) 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 develop-
ment.
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 precau-
tions.
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 device 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 device.
They are familiar with the contents of these operating instructions and the applica-
ble 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 device.
Operation Manual Lyovapor™ L-300/L-300 Pro 9/106
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2 | Safety BÜCHI Labortechnik AG
Operator
The operator (generally the laboratory manager) is responsible for the following aspects:
The device 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 device should be reported to the
manufacturer (quality@buchi.com).
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.
10/106 Operation Manual Lyovapor™ L-300/L-300 Pro
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BÜCHI Labortechnik AG Safety | 2
5
5
Fig.2: Location of warning signs on the product
General warning Dangerous electrical voltage
Flammable substances
2.4.3 Location of warning signs on the ice condenser
Fig.3: Location of warning signs on the product
Hand injuries Hot surface
2.5 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.
Operation Manual Lyovapor™ L-300/L-300 Pro 11/106
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2 | Safety BÜCHI Labortechnik AG
2.5.1 Faults during operation
If a device is damaged, sharp edges or exposed electrical wires can cause injuries.
u Regularly check device for visible damage.
u If faults occur, switch off the device immediately, unplug the power cord and in-
form the operator.
u Do 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.
u Handle the flask and other glass and acrylic components carefully and do not drop
them.
u Always place the flasks in a suitable holder when they are not mounted on the Ly-
ovapor™.
u Always visually inspect glass and acrylic components for damage every time they
are to be used.
u Do not continue to use glass and acrylic components that are damaged.
u Always 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.
u Make 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.
u Do 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.
u Always wear appropriate personal protective equipment such as safety goggles,
protective clothing and gloves.
u Make sure that the personal protective equipment meets the requirements of the
safety data sheets for all chemicals used.
2.7 Modifications
Unauthorized modifications may impair safety and lead to accidents.
u Use only genuine BUCHI accessories, spare parts and consumables.
u Technical modifications to the device or accessories should only be carried out
with the prior written approval of BÜCHI Labortechnik AG and only by authorized
BUCHI technicians.
BUCHI accepts no liability whatsoever for damage arising as a result of unauthorized
modifications.
12/106 Operation Manual Lyovapor™ L-300/L-300 Pro
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BÜCHI Labortechnik AG Product description | 3
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 pres-
sure 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.
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 a manifold-valve rack is used, heat transfer takes place by convection and radiation
from the surroundings. Control of the thermal energy transferred is then difficult.
If using a drying chamber with heatable shelves, heat transfer takes place by direct
contact. The temperature of the heatable shelves is controllable. Control of the thermal energy transferred is then possible.
Operation Manual Lyovapor™ L-300/L-300 Pro 13/106
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3 | Product description BÜCHI Labortechnik AG
Controlling the heat transfer prevents the following critical temperatures for amorphous and crystalline materials 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%.
3.2 Configuration
3.2.1 Front View
NOTE
For technical specifications of connections, see Chapter3.6 "Technical data",
page19
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BÜCHI Labortechnik AG Product description | 3
6
5
8
9
4
32
1
7
Fig.4: Front View
1 Connections for heated shelf
2 Intermediate valve
(Lyovapor™ L-300 Pro only)
3 Ice condenser 4 Optional mounting position for control
panel
5 Ventilation slots 6 Castors
7 Castor brake 8 On/Off master switch
9 User interface
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3 | Product description BÜCHI Labortechnik AG
7
6
4
5
12
13
15
16
14
3
2
1
11
10
9
8
3.2.2 Rear view
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
9 Gas connection for venting valve 10 Gas connection for pressure regulat-
8 Ventilation slots
ing valve
11 Inscription: Connect nitrogen when
12 Coolant outlet connection
using organic solvents.
13 Coolant inlet connection 14 Vacuum connection
15 Power cord 16 Vacuum pump connection
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Page 17
BÜCHI Labortechnik AG Product description | 3
2
1
8
7
6
3
4
5
1
2
3
3.2.3 Side connections
NOTE
For technical specifications of connections, see Chapter3.6 "Technical data",
page19
Fig.6: Side connections
1 Connection for pressure sensor
(option)
3 Automatic stoppering connection 4 Connection for fresh water sensor
5 Connection for receiving vessel sen-
sor
7 LAN port 8 Standard BUCHI communication port
3.2.4 Control panel
2 Connection for pressure sensor
(option)
6 Connection for external pressure sen-
sors (optional)
(COM)
Fig.7: Control panel
1 View 2 Function buttons
3 Navigation control
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Page 18
3 | Product description BÜCHI Labortechnik AG
1
2
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
9
10
9
3.2.5 Pro control panel
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.
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"
18/106 Operation Manual Lyovapor™ L-300/L-300 Pro
Page 19
BÜCHI Labortechnik AG Product description | 3
L-xxx xxHz LT
Cooling System Refrigerant: Rxxx
Filling: xxx g
Global Warming Potential (GWP): xx tCO2
High Side Design Pressure: xxxx
Low Side Design Pressure: xxxx
5
3
1
2
4
6
L-xxx xxHz HT
Cooling System Refrigerant: Rxxx
Filling: xxx g
Global Warming Potential (GWP): xx tCO2
High Side Design Pressure: xxxx
Low Side Design Pressure: xxxx
5
3
1
2
4
6
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
3.5.1 Refrigerant Specification (Low temperature)
The refrigerant details are shown on the back of the instrument.
Fig.10: Refrigerant details
1 Instrument name 2 Refrigerant details
3 Filling capacity 4 Global warming potential
5 High-pressure system design pres-
6 Low-pressure system design pres-
sure
3.5.2 Refrigerant Specification (High temperature)
The refrigerant details are shown on the back of the instrument.
Fig.11: Refrigerant details
1 Instrument name 2 Refrigerant details
3 Filling capacity 4 Global warming potential
5 High-pressure system design pres-
6 Low-pressure system design pres-
sure
sure
sure
3.6 Technical data
3.6.1 Lyovapor™ L-300
Operation Manual Lyovapor™ L-300/L-300 Pro 19/106
Specification L-300 for 50Hz L-300 for 60Hz
Dimensions without drying attachments (W x D x H)
710 x 1000 x 900mm 710 x 1000 x 900mm
Page 20
3 | Product description BÜCHI Labortechnik AG
Specification L-300 for 50Hz L-300 for 60Hz
Weight 272 kg 272 kg
Minimum clearance on all sides 400mm 400mm
Power supply 380 – 400 V 3N~ 208 – 220 V 3~
Power consumption
6000 VA 5000 VA
(maximum)
Lug 16 A 16 A
Frequency 50 Hz 60 Hz
Max. current for all connections 0.5 A 0.5 A
Voltage per connection 24 V 24 V
Connection voltage for each heat-
48 V 48 V
able shelf
(Lyovapor™ L-300 Pro only)
Max. current for each connection
max. 3 A max. 3 A
heatable shelf
(Lyovapor™ L-300 Pro only)
Overvoltage category II II
Protection rating IP20 IP20
Pollution degree 2 2
Condensing capacity
≥ 12 kg/24 h ≥ 12 kg/24 h
at 25 °C ambient temperature
Lowest condenser temperature
-105 °C -105 °C
(without samples)
Temperature divergence ± 3.0 °C ± 3.0 °C
Condenser capacity Unlimited
(2 x ≤ 1 kg)
Condenser surface area 2 x 1280 cm
2
Unlimited
(2 x ≤ 1 kg)
2 x 1280 cm
2
Number of compressors 2 2
Refrigerant 1 R507 CFC-free R507 CFC-free
Refrigerant 1 quantity 790 g 790 g
Refrigerant 2 Ethylene CFC-free Ethylene CFC-free
Refrigerant quantity 2 98 g 98 g
Drying shelf temperature to 60 °C to 60 °C
Drying shelf temperature tolerance ± 1.0 °C ± 1.0 °C
Inert gas pressure
max. 0.5bar max. 0.5bar
(relative pressure)
EMC to EN 61326 Class B Class B
Coolant pressure
< 4 bar < 4 bar
(relative pressure)
Coolant connection DN10 mm DN10 mm
Inlet water temperature 15 - 25°C 15 - 25°C
Cooling capacity of condenser for
Min. 350 W Min. 350 W
water cooling
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BÜCHI Labortechnik AG Product description | 3
Specification L-300 for 50Hz L-300 for 60Hz
Vacuum generation time to 0.1
Typically ≤ 15 min Typically ≤ 15 min
mbar*
Volume-based leakage rate* Typically ≤ 0.001
Minimum system vacuum* Typically ≤ 30 mTorr Typically ≤ 30 mTorr
Vacuum control range* 50 to 750 mTorr 50 to 750 mTorr
Noise emission to DIN 45635 ** Typically < 68 dB(A) Typically < 68 dB(A)
* With default vacuum pump / without samples
** Without vacuum pump
3.6.2 Ambient conditions
For indoor use only.
Max. altitude above sea level 2000 m
Ambient temperature 15 - 30°C
Maximum relative humidity 80 % for temperatures up to 30°C
Storage temperature max. 45°C
3.6.3 Materials
Component Materials of construction
Lyovapor™ housing Steel 1.4301/304 with powder coating
mbar x L/sec
Typically ≤ 0.001
mbar x L/sec
Vacuum chamber and components Steel 1.4301/304
Main connector PMMA GS
Drying chamber tube and cover PMMA GS
Seals FKM
Manifold drying rack Steel 1.4301/304
Manifold valves Natural rubber, PP
Cooling medium circuit Copper for freezing applications
EN 12735-1
Steel 1.4301/304
Vacuum clips Aluminium
Condensate drain tube Silicone
Condensate drain and venting valve Brass with EPDM seal
Regulating valve EN 1.4301
PBT
Silicone
Steam generation EN 1.4301
EPDM seal
Silicone
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4 | Transport and storage BÜCHI Labortechnik AG
4 Transport and storage
4.1 Transport
NOTICE
Risk of breakage due to incorrect transportation
Make sure that the instrument is fully dismantled.
Pack every instrument components properly to prevent breakage. Use the original
packaging whenever possible.
Avoid sharp movements during transit.
u After transporting, check the instrument and all glass components for damage.
u Damage that has occurred in transit should be reported to the carrier.
u Keep packaging for future transportation.
4.2 Storage
u Make sure that the ambient conditions are complied with (see Chapter3.6 "Tech-
nical data", page19).
u Wherever possible, store the device in its original packaging.
u After storage, check the device, all glass components, seals and tubing for dam-
age and replace if necessary.
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BÜCHI Labortechnik AG Installation | 5
5 Installation
5.1 Installation site
The installation site must meet the following requirements:
DANGER
Risk of explosion from flammable gas-and-air mixtures
The potential consequences are death or extremely serious injury.
u Do not damage the refrigerant circuit piping.
u Store and operate the instrument in a room with a volume of at least 16.6 m
that an ignitable gas-and-air mixture cannot develop.
3
so
NOTICE
Instrument damaged if switched on too early.
After transporting, wait twelve hours before switching on the instrument. The fluid in
the cooling system requires twelve hours to collect in the refrigerant compressor.
Firm, level surface
Minimum space requirements: 810 mm x 1000 mm x 1000 mm (W x D x H).
Take into account the maximum product dimensions and weight.
Take into account the 1100 mm operating height of the drying attachments.
The clearance from the air inlets and outlets to the wall should be at least 40 cm.
The clearance ensures air circulation and prevents the instrument from overheating.
Do not place loose papers or cloths below or to the sides of the instrument, as
these could impede the air circulation if drawn in.
Operate the instrument at an ambient temperature of +15°C to +30°C.
Make sure that the temperature of the cooling air drawn in is between +15 °C and
+30 °C.
Do not expose the instrument to any external thermal loads, such as direct solar
radiation.
At ambient temperatures upwards of 25°C use water cooling.
Make sure the castor brakes are locked or make sure the castor brakes are on.
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5 | Installation BÜCHI Labortechnik AG
Fig.12: Castor brake
NOTE
Make sure that the power supply can be disconnected at any time in an emergency.
NOTE
Depending on the ambient conditions, condensation may form on any cold surface
on the unit.
5.2 Putting the instrument in operation
NOTICE
Instrument damaged if restarted too early
Wait ten minutes before restarting the instrument. The oil in the refrigerant compressor requires ten minutes to return to the collection tank.
5.2.1 Preparing the instrument
u Clean the instrument with a damp cloth before commissioning.
u Check all sealing surfaces for scratches, dust, and cleanliness.
5.2.2 Establishing electrical connections
NOTE
Observe the regulatory provisions when connecting the Lyovapor™ to the power
supply.
4 Use additional electrical safety features (e.g., residual-current circuit breakers) to
comply with local laws and regulations.
The power supply must fulfil the following conditions:
1. Provide the mains voltage and frequency specified on the type plate of the instrument.
2. Be designed for the load imposed by the instruments connected.
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1
3
2
3. Be equipped with suitable fuses and electrical safety features.
4. Be equipped with a proper earthing.
u Make sure that all connected devices are earthed.
u Make sure that the power plug is freely accessible at all times.
u Insert the power plug into the power socket.
5.2.3 Fitting the fresh water connections
NOTICE
Risk of instrument damage from scale formation
u Use distilled water.
u Do not connect to mains water supply.
NOTE
4 Use only the containers supplied.
4 Place container at the same level as the instrument.
Fig.13: Fitting the fresh water connections
1 Side connections
2 Tube for fresh water
See Chapter3.2.3 "Side connections", page17
3 Connection for fresh water
Precondition:
R The coolant connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Switch the On/Off master switch to Off.
u Fit the inlet tube (4) onto the connection marked Fresh Water (5).
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5 | Installation BÜCHI Labortechnik AG
u Fit the fresh water level sensor (optional). See Chapter5.2.4 "Fitting fill-level sen-
sor in water tank (optional)", page26
5.2.4 Fitting fill-level sensor in water tank (optional)
Fig.14: Fitting the fresh water level sensor
u Switch the On/Off master switch to Off.
u Fit the sensor on the fresh water container above the inlet tube.
u Plug the fresh water sensor electrical connection into the socket marked Defrost
Water.
5.2.5 Fitting the drain tubes
CAUTION
Risk of scalding by hot water
u Make sure the condensate drain hose is not loose.
NOTE
4 Use only the containers supplied.
4 Place container at the same level as the instrument.
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1
3
2
Fig.15: Fitting the drain tube
1 Side connections
2 Drain tube
See Chapter3.2.3 "Side connections", page17
3 Connection for condensate drain tube
u Switch the On/Off master switch to Off.
u Fit the drain tube (4) onto the connection marked Drain 1 (5).
u Fix the drain tube in place with a hose clip.
u Fit another drain tube onto the connection marked Drain 2.
5.2.6 Fitting the fill-level sensor on the receiving vessel (optional)
Fig.16: Position of fill-level sensor in receiving vessel
u Fix the sensor on the receiving vessel below the condensate drain tube.
u Plug the receiving vessel sensor electrical connection into the socket marked
Waste Water.
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5 | Installation BÜCHI Labortechnik AG
3
4
2
1
5.2.7 Connecting the coolant
Fig.17: Connecting the coolant
1 Coolant inlet connection 2 Coolant outlet connection
3 Drain tube 4 Inlet tube
Precondition:
R The coolant connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Make sure that the instrument is not connected to the power supply.
u Fit the inlet tube (4) onto the coolant inlet connection (1).
u Fix the inlet tube (4) in place with a hose clip.
u Fit the drain tube (3) onto the coolant drain connection (2).
u Fix the drain tube (3) in place with a hose clip.
5.2.8 Fitting pressure sensors (option)
The pressure sensors measure the pressure in the top-mount drying rack.
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9
10
7
6
5
2
1
3
4
8
Fig.18: Fitting the pressure sensors
1 Pressure sensor 2 Pressure sensor
3 Clamp, ISO-KF 16 4 Clamp, ISO-KF 16
5 Seal, ISO-KF 16 6 Connection for pressure sensor
7 Seal, ISO-KF 16 8 Connection for pressure sensor
9 Connection 10 Connection
Fitting pressure sensor one
u Switch the On/Off master switch to Off.
u Remove the shipping cap from the pressure sensor connection (6).
u Fit the pressure sensor (1) and seal (5) to the pressure sensor connection (6) and
fix with the clamp (3).
u Plug the connecting lead connection into the socket (10) on the pressure sensor
u Plug the connecting lead connection into the socket marked Vacuum Sensor 1.
u Select the sensor from the submenu [[Settings]] on the control panel.
(1).
Fitting pressure sensor two
u Switch the On/Off master switch to Off.
u Remove the blanking cap from the pressure sensor connection (8).
u Fit the pressure sensor (2) and seal (7) to the pressure sensor connection (8) and
fix with the clamp (4).
u Plug the connecting lead connection into the socket (9) on the pressure sensor
(2).
u Plug the connecting lead connection into the socket marked Vacuum Sensor 2.
u Select the sensor from the submenu [[Settings]] on the control panel.
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5 | Installation BÜCHI Labortechnik AG
3
2
1
6
5
4
5.2.9 Connecting inert gas (option)
Fig.19: Connecting inert gas
1 Inert gas tube 2 Tube clip
3 Gas connection for pressure regulat-
4 Gas connection for venting valve
ing valve
5 Tube clip 6 Inert gas tube
Connecting the inert gas to the pressure regulating valve
Precondition:
R The gas connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Switch the On/Off master switch to Off.
u Fit the inert gas tube (1) onto the gas connection for the pressure regulating valve
(3).
u Fix the inert gas tube (1) with the tube clip (2).
Connecting the inert gas to the venting valve
Precondition:
R The gas connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Switch the On/Off master switch to Off.
u Fit the inert gas tube (6) onto the gas connection for the venting valve (4).
u Fix the inert gas tube (6) with the tube clip (5).
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5
4
3
2
1
10
9
8
7
6
5.2.10 Fitting an air filter (option)
Fig.20: Fitting an air filter
1 Air filter 2 Tube clip
3 Tubing 4 Tube clip
5 Gas connection for pressure regulat-
6 Gas connection for venting valve
ing valve
7 Tube clip 8 Tubing
9 Tube clip 10 Air filter
Fitting an air filter for the pressure regulating valve
Precondition:
R The gas connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Switch the On/Off master switch to Off.
u Fit the tube (3) onto the gas connection for the pressure regulating valve (5).
u Fix the tube (3) with the tube clip (4).
u Fit the air filter (1) onto the tube (3).
u Fix the air filter (1) with the tube clip (2).
Fitting an air filter for the venting valve
Precondition:
R The gas connection complies with the specified parameters. See Chapter3.6
"Technical data", page19
u Switch the On/Off master switch to Off.
u Fit the tube (8) onto the gas connection for the venting valve (6).
u Fix the tube (8) with the tube clip (7).
u Fit the air filter (10) onto the tube (8).
u Fix the air filter (10) with the tube clip (9).
5.3 Commissioning the vacuum pump
The vacuum pump evacuates the top-mount drying rack during the freeze-drying
process.
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5 | Installation BÜCHI Labortechnik AG
1
2
NOTICE
Closed gas ballast valve when using solvent.
A closed gas ballast valve when using solvents can cause damage to the instrument.
u When using solvents, keep the gas ballast valve open.
NOTE
To increase the service life of the vacuum pump, operate the vacuum pump with an
open gas ballast valve.
NOTE
Prepare the vacuum pump according to the manufacturer's instructions. See relevant
documentation.
Fig.21: Connections for vacuum pump
1 Vacuum pump connection 2 Vacuum tube connection,
ISO-KF 25
u Switch the On/Off master switch to Off.
u Connect the vacuum pump vacuum tube to the vacuum tube connection (2).
u Plug the vacuum pump electrical connection into the socket marked Vacuum
Pump.
5.4 Establishing LAN connection
5.4.1 Requirements for local network settings
u The following port has to be enabled in the firewall settings on the internet gate-
way:
TCP (HTTPS) traffics through remote port 443
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BÜCHI Labortechnik AG Installation | 5
u In order to use the BUCHI Cloud a DNS server must be configured on the instru-
ment.
NOTE
If there is no DNS server available enter the IP address for the BUCHI Cloud connection manually.
NOTE
If there is no DHCP server available enter the IP address, gateway subnet mask and
DNS server manually.
5.4.2 Preparing the instrument for app using
NOTICE!Do not unplug the LAN cable
while the device is connected to the
BUCHI Cloud Services
u Connect the instrument with the LAN
network.
Navigation path
➔ ➔ [Settings] ➔ [Network]
u Navigate to the action [Network].
u Enable the function [DHCP].
ð The instrument is prepared.
5.4.3 Enabling BUCHI Cloud access
Enable access to BUCHI Cloud in order to use the BUCHI Monitor App.
Navigation path
➔ ➔ Settings ➔ Network ➔ BUCHI Cloud
u Navigate to the action [[BUCHI Cloud]] via the navigation path.
u Select the option [Yes].
ð The instrument is connected to the BUCHI Cloud.
5.5 Insert SD card (Pro control panel only)
NOTE
Only insert or remove the SD card in Standby mode.
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5 | Installation BÜCHI Labortechnik AG
u Fold the control panel forward.
u Insert the SD card on the underside.
u Switch on the instrument.
ð The status bar shows the SD
card symbol.
The following data is stored on the SD card:
Numbering
Date
Time
Set pressure
Current pressure in the ice condenser
Inlet temperature of the ice condensers
Set drying shelf temperature
Current temperature of the drying shelves
Current sample temperatures
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32
1
6
5
6 Operating the control panel
This section describes the operation of the instrument using the control panel.
CAUTION
Risk of injury from glass splinters
Sharp objects can damage the display.
u Keep sharp objects away from the display.
6.1 Layout of the control panel
Fig.22: Layout of the control panel
No. Description Function
1 Status bar Shows the current status of the instrument.
2 Menu bar Shows symbols representing the menus.
3 Content area Shows current settings, submenus or actions
4 Function bar Shows functions that can be performed ac-
5 Navigation control Used for navigating the user interface.
6 Function buttons Pressing a function button performs the as-
6.2 Function bar
The function bar shows available functions according to the current operation.
The functions on the function bar are executed by tapping the relevant function buttons or pressing the navigation control.
depending on current operation.
cording to the current operation.
Pressing the control performs the assigned
function on the function bar.
signed function on the function bar.
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6 | Operating the control panel BÜCHI Labortechnik AG
E S C
O K
E D I T
M E N U
S AV E
OFF
S TAR T
SKIP
OPEN
CLOSE
General function buttons
Symbol Description Meaning
[Back] The display reverts to the previous
view.
[Cancel] Cancels an operation.
[Add to favourites] Adds the selected item to the
[[Favourites]] menu.
[Remove from
favourites]
[Confirm] Confirms an entry.
[Edit] Allows the selected item to be
[Menu] Allows selection of a menu from the
[Save] Saves the setting.
Process control function buttons
Symbol Description Meaning
[Defrost] Defrosts the ice condenser.
[Aerate] Vents the system.
[Shut down] The instrument shuts down.
[[Start]] Starts the freeze-drying process.
Removes the selected item from the
[Favourites] menu.
edited.
menu bar using the navigation control.
[Start conditioning] Starts the conditioning phase.
[Skip] Skips vacuum pump warm-up
phase.
The other conditioning phase pro-
cesses are carried out.
[Open] Opens the selected valve.
[Close] Closes the selected valve.
6.3 Menu bar
The menus are represented by symbols on the menu bar. Navigation through the
menus is by input controls.
The following menus are available:
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Menu symbol
6.3.1 Start menu
On the [Start] menu, parameters can be set manually.
Changing parameters
u Select a parameter by turning the navigation control.
ð The control panel highlights the selected parameter in green.
Meaning Submenu/Action
[Start] menu Process control parameters
[Favourites] menu Bookmarks for individual entry points
[Configuration] menu Process settings
Settings
Servicing
Service
System information
[Messages] menu Notifications
Logbook
u Tap the function [Edit] on the function bar.
ð The control panel highlights the selected parameter in black.
u To increase or decrease the figure, turn the navigation control clockwise or anti-
clockwise.
u Tap the function [Save] on the function bar.
ð The setting is saved.
6.3.2 Favourites menu
The [Favourites] menu allows you to define submenus and actions as bookmarks.
Adding a favourite
u Navigate to a submenu or action.
u Tap the function [Add to favourites] on the function bar.
ð The user interface switches to the [Favourites] menu and displays the
favourite created.
Removing a favourite
u On the [Favourites] menu, navigate to the favourite you wish to remove.
u Tap the function [Remove from favourites] on the function bar.
ð The favourite is removed.
6.3.3 Configuration menu
On the [Configuration] menu, you can enter a variety of settings and retrieve information.
Process settings submenu
The submenu [[Process settings]] contains functions for automatic process control.
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Action Option Explanation
[Vacuum test after
conditioning]
Off/On Automatic vacuum test after the con-
ditioning phase
[[Defrost before
conditioning]]
[[Defrost Mode]] Choice of which ice
Off/On Automatic condenser defrosting be-
fore the conditioning phase
The action is only available if the
condenser chamber is
defrosted.
status bar shows the status
Standby.
The following options are available:
None/One chamber/Both chambers
Settings submenu
The submenu [[Settings]] contains system settings for the instrument.
Action Option Explanation
[Mobile connection
password]
[Mobile connection
QR code]
View The control panel shows a password
for entry in the BUCHI Monitor app.
View The control unit shows a QR code
for reading by the BUCHI Monitor
app.
[Language] Choice of display lan-
guage on the control
panel
The following languages are avail-
able:
English/German/French/Italian/
Spanish/Russian/Portuguese/Japa-
nese/Chinese/Indonesian/Korean
[Temperature unit] Choice of unit for indi-
cation of temperatures
The following units are available:
°C (Celsius)/°F (Fahrenheit)/K
(Kelvin)
[Pressure unit] Choice of unit for indi-
cation of the vacuum
The following units are available:
HPa (hectopascals), mbar (mil-
libars), torr (= torr), mTorr (= milli-
torr), mmHg (millimetres of mercury)
[Date] Date input Enter in sequence: Day, month,
year. Apply the settings by pressing
[Save].
[Time] Time input Enter in sequence: Minutes, hours.
Apply the settings by pressing
[Save].
[[Vacuum Sensor
1]]
Pressure sensor selection
The following pressure sensors are
available:
None, Inficon Porter CDG020D, Infi-
con PSG 550
[[Vacuum Sensor
2]]
Pressure sensor selection
The following pressure sensors are
available:
None, Inficon Porter CDG020D, Infi-
con PSG 550
[Vacuum pump oil
change]
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Enter value Enter the oil change interval recom-
mended by the manufacturer.
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BÜCHI Labortechnik AG Operating the control panel | 6
Action Option Explanation
[Button tone] Off/On Setting for audible signal in re-
sponse to input controls.
[Display brightness] Enter setting Display illumination level in %: 0 -
100
[Network] Enter value The following parameters can be
edited:
Device name/MAC address/DHCP/
System IP address/Subnet mask/
Gateway/DNS server/BUCHI Cloud/
Server IP address
[Delete app connection]
Confirmation question Resets external connections to the
instrument.
Submenu Maintenance
The submenu [[Maintenance]] contains tests for maintaining the instrument.
Action Option Explanation
[[Leak test]] Perform leak test See section Chapter9.3 "Performing
a leak test", page90
[Vacuum test] Perform vacuum test See Chapter9.2 "Performing a vac-
uum test", page89
Submenu Service
NOTE
While freeze-drying is in progress, no settings can be changed on the Service submenu.
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6 | Operating the control panel BÜCHI Labortechnik AG
Action Option Explanation
[Refrigerant circuit] View The following information on the re-
frigerant circuit is available:
Duty hours
Compressor high temperature
Compressor low temperature
Inlet temperature, ice condenser 1
Outlet temperature, ice condenser
1
Inlet temperature, ice condenser 2
Outlet temperature, ice condenser
2
Expansion valve 1
Expansion valve 2
Bypass valve
Safety switch for low pressure/low
temp
Safety switch for high pressure/
low temp
Intermediate heat exchanger tem-
perature
Safety switch for low pressure/
high temp
Safety switch for high pressure/
high temp
Ambient temperature
Evaporation pressure, low tem-
perature
Evaporation pressure, high tem-
perature
Condensation pressure, low tem-
perature
Condensation pressure, high tem-
perature
Suction gas temperature, low tem-
perature
Discharge line temperature, low
temperature
Discharge line temperature, high
temperature
EEV bypass, low temperature
EEV, high temperature
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Action Option Explanation
[Vacuum system] View The following information on the vac-
uum system is available:
Pump hours of duty
Pump oil hours of duty
Pressure, ice condenser 1
Pressure, ice condenser 2
Main valve 1
Main valve 2
Vacuum Pump
Venting valve 1
Venting valve 2
Regulating valve 1
Regulating valve 2
Vacuum sensor 1
Vacuum sensor 2
[[Ice condenser]] View The following information on the ice
condenser is available:
Steam generator valve
Defrost valve, ice condenser 1
Defrost valve, ice condenser 2
Intermediate valve 1
Intermediate valve 2
Active ice condenser
[Defrosting system] View The following information on the de-
frosting system is available:
Duty hours
Steam generator
Water pump
Drain valve 1
Drain valve 2
Safety valve, vacuum sensor 1
Safety valve, vacuum sensor 2
Steam generator excess pressure
Steam generator excess tempera-
ture
Steam generator water level OK
Water tank fill level low
Drain tank full
Water pump
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Action Option Explanation
[[Stoppering System]]
View The following information on the
stoppering system is available:
Number of uses
Start
On
Off
Oil pressure
Submenu System Information
The submenu [[System information]] contains details of the connected components
and information on network connection diagnosis.
Action Option Explanation
[Control panel] View The following information on the
control panel is available:
Serial number
Firmware version
Hours of duty
Status
PCB Temperature
24V power supply
5V power supply
[[Instrument]] View The following information on the
[Network diagnostics]
6.3.4 Messages menu
The [Messages] menu shows the current instrument messages and the instrument's
message history.
The following message types are possible:
I = Information
W = Warning
E = Error
L-300 is available:
Serial number
Firmware version
Hours of duty
Status
PCB Temperature
48V power supply
24V power supply
5V power supply
3.3V power supply
View/Enter settings The following network diagnosis in-
formation is available:
Network interruptions
Event list
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Submenu Notifications
The submenu [Notifications] shows a list of unacknowledged and unresolved notifications together with date and time in each case.
Submenu Logbook
The submenu [Logbook] shows the instrument's message history.
Logbook:
List of the last 100 messages.
Every occurrence is shown with date and time.
The following status types are possible:
Symbol Description Meaning
x Acknowledged The message has been be processed
and acknowledged.
< Sent The message initiator is no longer
present.
> Received The display shows a message.
6.4 Status bar
The status bar shows the status of the instrument.
The following statuses are possible:
Indication on status bar
View Status
Unload / Load Before the freeze-drying process:
Aerating The system is venting.
Shutting down The instrument is shutting down.
Defrosting The instrument is defrosting.
Standby The instrument is in energy-saving mode.
Conditioning The instrument is starting up.
Load the top-mount drying rack with a frozen
sample.
After the freeze-drying process:
Remove the dried sample from the top-mount
drying rack.
The status bar shows the remaining time.
The status bar shows the remaining time.
Reconditioning The instrument is restarting after a temporary
power failure.
Warming up pump The vacuum pump is being brought up to operat-
ing temperature.
Vacuum Test The instrument is performing a vacuum test.
Leak Test The instrument is performing a leak test.
Manual Drying The instrument is in the course of a manual
freeze-drying process.
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View Status
Recovering The system is in the process of recovering from a
power failure.
The current parameters of the freeze-drying
process are being re-established.
Symbols on the status bar
Symbol Status
The instrument is connected to the BUCHI Cloud.
The instrument is defrosting.
The instrument is starting up.
The instrument is in energy-saving mode.
Before the freeze-drying process:
Load the top-mount drying rack with a frozen
sample.
6.5 Carrying out freeze-drying
6.5.1 Preparing the instrument
Time
required:
Navigation path
➔ Start
Precondition:
R All commissioning operations have been completed. See Chapter5.2 "Putting the
approx.
30min
instrument in operation", page24
After the freeze-drying process:
Remove the dried sample from the top-mount
drying rack.
The system evacuates to the set pressure.
The instrument is performing a vacuum test or a
leak test.
u Navigate to the [Start] menu via the navigation path.
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u Tap the function [[Start conditioning]] on the function bar.
ð The temperature in the ice condenser cools down to operating temperature.
ð The vacuum pump is being brought up to operating temperature.
ð After completion of the conditioning phase, the status bar shows the status
Unload / Load.
6.5.2 Starting freeze-drying
CAUTION
Risk of skin burns from touching parts of the ice condenser after completion of conditioning.
u Wear protective gloves when working on the instrument after the conditioning
phase.
Navigation path
➔ Start
Precondition:
R The instrument has been prepared.
u Fit a top-mount drying rack. See Chapter8 "Operating top-mount drying racks",
page73.
u Load the top-mount drying rack with frozen samples.
u Navigate to the [Start] menu via the navigation path.
u Enter the required settings for the process parameters.
u Tap the function [Start] on the function bar.
ð The freeze-drying process starts.
ð The control panel shows the S tar t menu with a black background.
ð The status bar shows a clock counting up and the status Manual Drying.
ð The system evacuates to the set pressure.
6.5.3 Editing parameters while the process is running
Navigation path
➔ Start
Precondition:
R The freeze-drying process has been started.
u Navigate to the [Start] menu via the navigation path.
u Navigate to the desired parameter using the navigation control.
u Tap the function [Edit] on the function bar.
ð The control panel highlights the selected parameter in white.
u Turn the navigation control to increase or decrease the parameter setting.
u Tap the function [Save] on the function bar.
ð The setting is saved.
6.5.4 Ending freeze-drying
Navigation path
➔ Start
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Precondition:
R The sample is dry.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Aerate] on the function bar.
u Answer YES to the confirmation question.
ð The system is vented.
ð The status bar shows the status Aerating.
u As soon as the status bar shows the status Unload / Load, remove the dried sam-
ple from the drying rack.
6.5.5 Shutting down the instrument
NOTICE
Not completed shut down of the instrument.
An interruption while shutting down the instrument can damage the instrument.
u Shut down the instrument completely.
u If the shutdown was interrupted, tap the function [Defrost] on the function bar.
Time
80 min
required:
Navigation path
➔ Start
Precondition:
R The freeze-drying process has ended.
R The gas balast on the vacuum pump is open.
R Make sure that there is sufficient distilled water available.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Shut down] on the function bar.
ð The instrument is shutting down.
ð The status bar shows the remaining time and the status Shutting down.
ð After the instrument has shut down, the status bar shows the remaining time
and the status Defrosting.
ð After the defrosting, the status bar shows the status Standby.
6.5.6 Switching off the instrument
Precondition:
R The instrument has been shut down. See Chapter6.5.5 "Shutting down the instru-
ment", page46
u Switch the On/Off master switch to Off.
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5
4
3
2
1
7 Operating Pro control panel
This section describes the operation of the instrument using the Pro control panel.
CAUTION
Risk of injury from glass splinters
Sharp objects can damage the display.
u Keep sharp objects away from the display.
7.1 Layout of Pro control panel
Fig.23: Layout of Pro control panel
No. Description Function
1 Status bar Shows the current status of the instrument.
2 Menu bar Shows symbols representing the menus.
3 Content area Shows current settings, submenus or actions
4 Function bar Shows functions that can be performed ac-
5 Navigation control Used for navigating the user interface. Press-
7.2 Function bar
The function bar shows functions that can be performed according to the current operation.
The functions on the function bar are executed by tapping the relevant function buttons or pressing the navigation control.
General function buttons
depending on the current operation.
cording to the current operation
ing the control performs the assigned function on the function bar.
Symbol Description Meaning
[Back] The display reverts to the previous
view.
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E S C
O K
E D I T
M E N U
S AV E
OFF
S TAR T
DELETE
Symbol Description Meaning
[Cancel] Cancels an operation.
[Add to favourites] Adds the selected item to the
[[Favourites]] menu.
[Remove from
favourites]
[Confirm] Confirms an entry.
[Edit] Allows the selected item to be
[Menu] Allows selection of a menu from the
[Save] Saves the setting.
Process control function buttons
Symbol Description Meaning
[Defrost] Defrosts the ice condenser.
[Aerate] Vents the system.
[Shut down] The instrument shuts down.
[[Start]] Starts the freeze-drying process.
Removes the selected item from the
[Favourites] menu.
edited.
menu bar using the navigation control.
[Start conditioning] Starts the conditioning phase.
[Manual] Switches to manual freeze-drying.
[Method] Switches to freeze-drying with pro-
grammable parameters.
[New] Creates a new method
[Right] Moves the selection to the right.
[Left] Moves the selection to the left.
[Progression] Graphical display of method pro-
gression showing pressure and temperature details.
[Activate] Confirms selection of a method.
[Delete] Deletes the selected method or step.
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SKIP
C O P Y
OPEN
CLOSE
Symbol Description Meaning
[Skip] Skips vacuum pump warm-up
phase.
The other conditioning phase pro-
cesses are carried out.
[[Deactivate sample
protection]]
[Copy] Copies the selected method.
[Open] Opens the selected valve.
[Close] Closes the selected valve.
7.3 Other symbols on the control panel
Symbol Description Meaning
[Closed] The assigned method is active and
7.4 Menu bar
The menus are represented by symbols on the menu bar. Navigation through the
menus is by the input controls.
The following menus are available:
Menu symbol
Meaning Submenu/Action
Start menu Process control parameters
Manually deactivates sample protection.
cannot be changed.
7.4.1 Start menu
On the [Start] menu, parameters can be set manually.
Favourites menu Bookmarks for individual entry points
Method menu For saving freeze-drying methods
Editing and activating freeze-drying
method
Configuration menu Process settings
Settings
End point determination
Maintenance
Service
System information
Messages menu Notifications
Logbook
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Setting parameters using the navigation control
u Select a parameter by turning the navigation control.
ð The control panel highlights the selected parameter in green.
u Tap the function [Edit] on the function bar.
ð The control panel highlights the selected parameter in black.
u To increase or decrease the figure, turn the navigation control clockwise or anti-
clockwise.
u Press the navigation control.
ð The setting is saved.
ð The control panel highlights the new setting in green.
Setting parameters using the touch-screen
u Select the parameter by tapping the control panel screen.
ð The control panel shows a dialog box with a numeric input box.
ð The control panel highlights the selected parameter in black.
u Enter the value in the numeric input box.
u Tap the function [Save] on the function bar.
ð The setting is saved.
ð The dialog box closes.
ð The control panel highlights the new setting in green.
7.4.2 Favourites menu
The [Favourites] menu allows you to define submenus and actions as favourites.
Adding a favourite
u Navigate to a submenu or action.
u Tap the function [Add to favourites] on the function bar.
ð The user interface switches to the [Favourites] menu and displays the
favourite created.
Removing a favourite
u On the [Favourites] menu, navigate to the favourite you wish to remove.
u Tap the function [Remove from favourites] on the function bar.
ð The favourite is removed.
7.4.3 Method menu
The [Method] menu allows freeze-drying processes with multiple phases and steps to
be saved. See Chapter7.6 "Editing a method", page57
7.4.4 Configuration menu
On the [Configuration] menu, you can enter a variety of settings and retrieve information.
Process settings submenu
The submenu [[Process settings]] contains actions for automatic process control.
Action Option Explanation
[Vacuum test after
conditioning]
[Leak test after
conditioning]
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Off/On Automatic leak test after the condi-
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Action Option Explanation
[[Defrost before
conditioning]]
Off/On Automatic condenser defrosting be-
fore the conditioning phase
[[Defrost Mode]] Choice of which ice
condenser chamber is
defrosted.
The action is only available if the
status bar shows the status
Standby.
The following options are available:
None/One chamber/Both chambers
Settings submenu
The submenu [[Settings]] contains system settings for the instrument.
Action Option Explanation
[Mobile connection
password]
[Mobile connection
QR code]
View The control panel shows a password
for entry in the BUCHI Monitor app.
View The control unit shows a QR code
for reading by the BUCHI Monitor
app.
[Language] Choice of display lan-
guage on the control
panel
The following languages are available:
English/German/French/Italian/
Spanish/Russian/Portuguese/Japanese/Chinese/Indonesian/Korean
[Temperature unit] Choice of unit for indi-
cation of temperatures
The following units are available:
°C (Celsius)/°F (Fahrenheit)/K
(Kelvin)
[Pressure unit] Choice of unit for indi-
cation of the vacuum
The following units are available:
HPa (hectopascals), mbar (mil-
libars), torr (= torr), mTorr (= millitorr), mmHg (millimetres of mercury)
[[Vacuum Sensor
1]]
Pressure sensor selection
The following pressure sensors are
available:
None, Inficon Porter CDG020D, Inficon PSG 550
[[Vacuum Sensor
2]]
Pressure sensor selection
The following pressure sensors are
available:
None, Inficon Porter CDG020D, Inficon PSG 550
[Vacuum pump oil
change]
Enter value Enter the oil change interval recom-
mended by the manufacturer.
[Date] Date input Enter in sequence: Day, month,
year. Apply the settings by pressing
[Save].
[Time] Time input Enter in sequence: Minutes, hours.
Apply the settings by pressing
[Save].
[Button tone] Off/On Setting for audible signal in re-
sponse to input controls.
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Action Option Explanation
[Display brightness] Enter setting Display illumination level in %: 0 -
100
[Network] Enter value The following parameters can be
edited:
Device name/MAC address/DHCP/
System IP address/Subnet mask/
Gateway/DNS server/BUCHI Cloud/
Server IP address
[Delete app connection]
Confirmation question Resets external connections to the
instrument.
Submenu End point determination
Action Option Explanation
[[Pressure rise
test]]
[Pressure difference test]
[Temperature difference test]
View Shows the current settings for the
pressure rise test.
View Actual and specified settings
Result
View Actual and specified settings
Result
Submenu Maintenance
The submenu [[Maintenance]] contains tests for maintaining the instrument.
Action Option Explanation
[[Leak test]] Perform leak test See section Chapter9.3 "Performing
a leak test", page90
[Vacuum test] Perform vacuum test See Chapter9.2 "Performing a vac-
uum test", page89
Submenu Service
NOTE
While freeze-drying is in progress, no settings can be changed on the Service submenu.
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Action Option Explanation
[Refrigerant circuit] View The following information on the re-
frigerant circuit is available:
Duty hours
Compressor high temperature
Compressor low temperature
Inlet temperature, ice condenser 1
Outlet temperature, ice condenser
1
Inlet temperature, ice condenser 2
Outlet temperature, ice condenser
2
Expansion valve 1
Expansion valve 2
Bypass valve
Safety switch for low pressure/low
temp
Safety switch for high pressure/
low temp
Intermediate heat exchanger tem-
perature
Safety switch for low pressure/
high temp
Safety switch for high pressure/
high temp
Ambient temperature
Evaporation pressure, low tem-
perature
Evaporation pressure, high tem-
perature
Condensation pressure, low tem-
perature
Condensation pressure, high tem-
perature
Suction gas temperature, low tem-
perature
Discharge line temperature, low
temperature
Discharge line temperature, high
temperature
EEV bypass, low temperature
EEV, high temperature
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Action Option Explanation
[Vacuum system] View The following information on the vac-
uum pump is available:
Pump hours of duty
Pump oil hours of duty
Pressure in the ice condenser
Main valve
Vacuum pump
Venting valve
Regulating valve
[[Ice condenser]] View The following information on the ice
condenser is available:
Steam generator valve
Defrost valve, ice condenser 1
Defrost valve, ice condenser 2
Intermediate valve 1
Intermediate valve 2
Active ice condenser
[Defrosting system] View The following information on the de-
frosting system is available:
Duty hours
Steam generator
Water pump
Drain valve 1
Drain valve 2
Safety valve, vacuum sensor 1
Safety valve, vacuum sensor 2
Steam generator excess pressure
Steam generator excess tempera-
ture
Steam generator water level OK
Water tank fill level low
Drain tank full
Water pump
[[Stoppering System]]
View The following information on the
stoppering system is available:
Number of uses
Start
On
Off
Oil pressure
[Drying shelves] View Switches heating for the individual
shelves on and off (where available).
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Submenu System Information
The submenu [[System information]] contains details of the connected devices and information on network connection diagnosis.
Action Option Explanation
[Control panel] View The following information on the
control panel is available:
Serial number
Firmware version
Hours of duty
Status
PCB Temperature
24V power supply
5V power supply
[[Instrument]] View The following information on the
L-300 is available:
Serial number
Firmware version
Hours of duty
Status
PCB Temperature
48V power supply
24V power supply
5V power supply
3.3V power supply
[Network diagnostics]
7.4.5 Messages menu
The [Messages] menu shows the current instrument messages and the instrument's
message history.
The following message types are possible:
I = Information
W = Warning
E = Error
Submenu Notifications
The submenu [Notifications] shows a list of unacknowledged and unresolved notifications together with date and time in each case.
Submenu Logbook
The submenu [Logbook] shows the instrument's message history.
Logbook:
List of the last 100 messages.
Every occurrence is shown with date and time.
View/Enter settings The following network diagnosis in-
formation is available:
Network interruptions
Event list
The following status types are possible:
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Symbol Description Meaning
x Acknowledged The message has been be processed
and acknowledged.
< Sent The message initiator is no longer
present.
> Received The display shows a message.
7.5 Status bar
The status bar shows the status of the instrument.
The following statuses are possible:
Indication on status bar
View Status
Unload / Load Before the freeze-drying process:
Load the top-mount drying rack with a frozen
sample.
After the freeze-drying process:
Remove the dried sample from the top-mount
drying rack.
Aerating The system is venting.
Shutting down The instrument is shutting down.
The status bar shows the remaining time.
Defrosting The instrument is defrosting.
The status bar shows the remaining time.
Standby The instrument is in energy-saving mode.
Conditioning The instrument is starting up.
Reconditioning The instrument is restarting after a temporary
power failure.
Warming up pump The vacuum pump is being brought up to operat-
ing temperature.
Vacuum Test The instrument is performing a vacuum test.
Leak Test The instrument is performing a leak test.
Manual Drying The instrument is in the course of a manual
freeze-drying process.
Recovering The system is in the process of recovering from a
power failure.
The current parameters of the freeze-drying
process are being re-established.
Hold The instrument is in the holding phase.
Primary drying The instrument is in the primary drying phase.
Secondary drying The instrument is in the secondary drying phase.
Tempering shelves The instrument is modulating the heatable
shelves to the set temperature.
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Symbols on the status bar
Symbol Status
The instrument is defrosting.
The instrument is in energy-saving mode.
The instrument is in the course of a freeze-drying
process using a method.
The instrument is starting up.
The instrument is in the course of a manual
freeze-drying process.
The instrument is connected to the BUCHI Cloud.
Sample protection is active.
Reason: the pressure is outside the pressure lim-
its.
Sample protection is active.
Reason: the temperature is outside the safe tem-
perature range.
7.6 Editing a method
The Pro control panel can save up to 35 methods. The methods enable the freezedrying process to be automated.
Sample protection is active.
Reason: the pressure is outside the pressure lim-
its.
the temperature is outside the safe temperature
range.
Before the freeze-drying process:
Load the top-mount drying rack with a frozen
sample.
After the freeze-drying process:
Remove the dried sample from the top-mount
drying rack.
The vacuum pump is being brought up to operating temperature.
The instrument is performing a vacuum test or a
leak test.
The memory card has been inserted.
7.6.1 Creating a new method
There are two possible ways of creating a new method:
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Creating a new method
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the function [New] on the function bar.
ð The new method is created.
Creating a new method by copying an existing method
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to copy.
u Tap the function [Copy] on the function bar.
ð The new method is created.
7.6.2 Changing the name of a method
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [Information].
ð The control panel shows the action Information.
u Tap the setting [Name].
ð The control panel shows a blank box with an alphanumeric input box.
u Enter a name for the method.
u Tap the function [Save] on the function bar.
ð The new name is saved.
ð The dialog box closes.
7.6.3 Setting the sample collapse temperature
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [General].
ð The control panel shows the action [General].
u Tap the setting [Sample collapse temperature].
ð The control panel shows a dialog box with a numeric input box.
u Enter the value in the numeric input box.
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u Tap the function [Save] on the function bar.
ð The setting is saved.
ð The dialog box closes.
7.6.4 Setting the gas type
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [General].
ð The control panel shows the action [General].
u Tap the setting [Gas type].
ð The control panel shows a dialog box with an alphanumeric input box.
u Enter the gas type.
u Tap the function [Save] on the function bar.
ð The setting is saved.
ð The dialog box closes.
7.6.5 Setting the shelf loading temperature
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [General].
ð The control panel shows the action [General].
u Tap the action [Shelf load temp.]
ð The control panel shows a dialog box with a numeric input box.
u Enter the value in the numeric input box.
u Tap the function [Save] on the function bar.
ð The setting is saved.
ð The dialog box closes.
7.6.6 Setting the steps of a method
The Pro control panel can save up to 30 steps for each method.
NOTE
The maximum heating rate is 3 °C/min.
NOTE
The settings for the action Steps affect a single step in each case.
Navigation path
➔ Method
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u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [Steps].
ð The control panel shows the action Steps.
The following settings are available for each step:
Setting Option Meaning
[Step phase] Primary drying/Sec-
Sets the type of step phase.
ondary drying
[Term] Enter value Sets the duration of the step in
minutes.
[Shelf temperature] Enter value Set the temperature of the heat-
able shelves in one step.
[Pressure zone] Regulated/Minimum Regulated: the settings for pres-
sure and pressure limits are applied.
Minimum: The maximum vacuum is applied to reach the lowest possible pressure.
[Pressure] Enter value Sets a target value for the regu-
lated pressure.
[Pressure limit] Enter value Absolute value for divergence
from the set pressure before the
sample protection function is activated.
[Pressure duration] Enter value Sets the period of time that the
pressure is allowed to exceed
the pressure limit before the
sample protection function is activated.
Editing a step
u Use the function [Right] or [Left] on the function bar to navigate to the step that
you wish to edit.
u Using the navigation control, navigate to the setting that you wish to change.
u Tap the function [Edit] on the function bar.
u Edit the setting as required.
u Tap the function [Save] on the function bar.
ð The setting is changed.
Add step
u Use the function [Right] or [Left] on the function bar to navigate to the position at
which you wish to add a step.
u Tap the function [New] on the function bar.
ð The new step is created.
Delete step
u Use the function [Right] or [Left] on the function bar to navigate to the step that
you wish to delete.
u Tap the function [Delete] on the function bar.
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u When asked to confirm, press [OK].
ð The step is deleted.
7.6.7 Setting the phases of a method
NOTE
The settings in the Phase view affect all steps of a phase.
Navigation path
➔ Method
u Navigate to the [[Method]] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [[Phase]].
ð The control panel shows the Phase view.
The following phases of a method are available:
Phase Setting Option Meaning
[[Primary
drying]]
[[Pressure action]]
None/Sample
protection/
Message
None: no action is carried out.
Sample protection: if the pressure is
too high, heating of the shelves is
paused.
[[Temp. action]]
[[Safety temperature]]
[[Safety temp
time]]
[[End point definition]]
Message: if the pressure is too high,
the control panel displays a message.
None/Sample
protection/
Message
None: no action is carried out.
Sample protection: if the temperature is too high, heating of the
shelves is paused.
Message: if the temperature is too
high, the control panel displays a
message.
Enter value Maximum divergence below the set
sample collapse temperature before
the sample protection function is activated.
Enter value Time as of which sample protection
in inactive. The value relates to the
time before completion of primary
drying.
More settings See Setting end point definitions
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Phase Setting Option Meaning
[[Secondary
drying]]
[[Pressure action]]
None/Sample
protection/
Message
None: no action is carried out.
Sample protection: if the pressure is
too high, heating of the shelves is
paused.
Message: if the pressure is too high,
the control panel displays a message.
[[Stoppering]]
[[Temp. action]]
None/Sample
protection/
Message
None: no action is carried out.
Sample protection: if the temperature is too high, heating of the
shelves is paused.
Message: if the temperature is too
high, the control panel displays a
message.
[[Safety temperature]]
Enter value Maximum lower divergence from the
set shelf temperature before the
sample protection function is activated.
[[End point def-
More settings See Setting end point definitions
inition]]
[[Pressure
range]]
Regulated/Minimum
Regulated: the settings for pressure
and pressure limits are applied.
Minimum: the lowest possible vacuum pressure is applied.
[[Pressure]] Enter value Sets a target value for the regulated
pressure.
[[Mode]] None/Manual None: no action is carried out.
Manual: sealing is performed manually.
[[Hold]] [[Pressure
range]]
Regulated/Minimum
Regulated: the settings for pressure
are applied.
Minimum: the lowest possible vacuum pressure is applied.
[[Pressure]] Enter value Sets a level for the regulated pres-
sure.
[[Drying shelf
temperature]]
Enter value Specifies a temperature for the dry-
ing shelves.
Editing the settings for a phase
u Tap the phase that you wish to edit.
ð The control panel highlights the selected phase in green.
u Tap the setting that you wish to edit.
u Edit the setting as required.
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u Tap the function [Save] on the function bar.
ð The setting is changed.
7.7 Deleting a method
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the function [Delete] on the function bar.
u Select [Confirm] to confirm the action in response to the confirmation question.
ð The method is deleted.
7.8 Setting end point definitions
The end of each phase can be automated by setting the end point definition.
The end point can be defined by means of the temperature difference test, the pressure difference test or the pressure rise test.
7.8.1 Pressure difference test
The pressure difference test establishes the difference between the readings from
two pressure sensors in the drying chamber. If the difference between the two sensor
readings is below a threshold, the freeze-drying phase can be ended.
Navigation path
➔ Method
Precondition:
R A capacitive pressure sensor (Inficon Porter CDG020D) is connected to the con-
nection Vacuum Sensor 1. See Chapter5.2.8 "Fitting pressure sensors (option)",
page28
R A Pirani pressure sensor (Inficon PSG55x) is connected to the connection Vac-
uum Sensor 2. See Chapter5.2.8 "Fitting pressure sensors (option)", page28
u Perform vacuum test. See Chapter9.2 "Performing a vacuum test", page89
u Navigate to the [Method] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [[Phase]].
ð The control panel shows the action Phase.
u Tap the setting [[End point definition]].
ð The control panel shows the setting End point definition.
u Tap [[Pressure difference test]].
ð The control panel shows the pressure difference test.
The following settings are available:
Setting Option Explanation
[[Pressure difference test]]
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Yes/No Switches the pressure differ-
ence test on or off.
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Setting Option Explanation
[[Start time]] Enter value Sets the time from which the
pressure difference test is to be
performed. The value relates to
the time before completion of
the primary drying phase or the
secondary drying phase.
[[Pressure dif-
Enter value Specifies the difference between
ference limit]]
[[Duration]] Enter value The period of time during which
[[Continue]] Yes/No Yes : the method switches to the
[[Message]] Yes/No The control panel shows or does
7.8.2 Temperature difference test
NOTE
The temperature test is successfully completed if all drying shelves are below the
threshold.
the two sensor readings below
which the end point is reached.
the difference is not to be exceeded. If the threshold is not
exceeded for the full period of
time, the pressure difference
test is passed.
next phase.
No: the phase is ended when
the set levels are reached.
not show a message as soon as
the pressure difference test is
passed.
The samples on a drying shelf have different drying times. Take account of the different drying times in the [Duration] setting.
The temperature difference test establishes the difference between the readings from
the temperature sensor for the heatable shelf and the temperature sensor in the sample. If the difference between the two sensor readings is below a threshold, the
freeze-drying phase can be ended.
Navigation path
➔ Method
Precondition:
R The heatable shelves are fitted in the rack. See Chapter8 "Operating top-mount
drying racks", page73
R The optional temperature sensor has been installed. See Chapter8 "Operating
top-mount drying racks", page73
u Place the optional temperature sensor in the sample.
u Navigate to the [Method] menu via the navigation path.
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u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [Phase].
ð The control panel shows the action Phase.
u Tap the setting [End point definition].
ð The control panel shows the setting End point definition.
u Tap [Temperature difference test].
ð The control panel shows the temperature difference test.
The following settings are available:
Setting Option Explanation
[Temperature
difference test]
Yes/No Switches the temperature differ-
ence test on or off.
[Start time] Enter value Sets the time from which the
temperature difference test is to
be performed. The value relates
to the time before completion of
the primary drying phase.
[Temperature
difference limit]
[Term] Enter value The period of time during which
[Continue] Yes/No Yes : the method switches to the
[Message] Yes/No The control panel shows or does
7.8.3 Pressure rise test
NOTE
Take account of the [result] of the leak test in settings for [[Pressure limit]] and [[Duration]].
Enter value Specifies the difference between
the two sensor readings below
which the end point is reached.
the difference is not to be exceeded. If the threshold is not
exceeded for the full period of
time, the temperature difference
test is passed.
next phase.
No: the phase is ended when
the set levels are reached.
not show a message as soon as
the temperature difference test
is passed.
Navigation path
➔ Method
Precondition:
R The Inficon PSG550 or Inficon porter CDG020D pressure sensor is fitted.See
Chapter5.2.8 "Fitting pressure sensors (option)", page28
R A leak test has been successfully completed before the pressure rise test. See
Chapter9.3 "Performing a leak test", page90.
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u Navigate to the [[Method]] menu via the navigation path.
u Tap the name of the method that you wish to edit.
ð The control panel highlights the selected method in green.
u Tap the action [[Phase]].
ð The control panel shows the action Phase.
u Tap the setting [[End point definition]].
ð The control panel shows the setting End point definition.
u Tap [[Pressure rise test]].
ð The control panel shows the pressure rise test.
The following settings are available:
Setting Option Explanation
[[Pressure rise
test]]
Yes/No Switches the pressure rise test
on or off.
[[Duration]] Enter value Specifies the length of time for
which the pressure rise test is to
be carried out.
[[Start time]] Enter value Sets the time from which the
pressure difference test is to be
performed. The value relates to
the time before completion of
the primary drying phase or the
secondary drying phase.
[[Pressure
limit]]
Enter value The threshold that the pressure
must be below.
[[Interval]] Enter value Time between repetitions of the
test.
[[Start condition]]
Time/Pressure difference test/
Temp difference test/Both
Time:The pressure rise test is
carried out when the specified
time has elapsed.
Pressure difference test: The
pressure rise test is only carried
out if a pressure difference test
is passed.
Temperature difference test:The
pressure rise test is only carried
out if a temperature difference
test is passed.
Both: The pressure rise test is
only carried out if the temperature difference test and the pressure difference test are both
passed.
[[Continue]] Yes/No Yes : the method switches to the
next phase.
No: the phase is ended when
the set levels are reached.
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Setting Option Explanation
[[Message]] Yes/No The control panel shows or does
not show a message as soon as
the temperature difference test
is passed.
7.9 Performing freeze-drying using a method [Pro control panel]
7.9.1 Preparing the instrument
Time
re-
approx.
30min
quired:
Navigation path
➔ Start
Precondition:
R All commissioning operations have been completed. See Chapter5.2 "Putting the
instrument in operation", page24
u Navigate to the [Start] menu via the navigation path.
u Tap the function [[Start conditioning]] on the function bar.
ð The temperature in the ice condenser cools down to operating temperature.
ð The vacuum pump is being brought up to operating temperature.
ð After completion of the conditioning phase, the status bar shows the status
Unload / Load.
7.9.2 Selecting a method
Navigation path
➔ Method
u Navigate to the [Method] menu via the navigation path.
u Tap the function [Method] on the function bar.
u Tap the method that you wish to use.
u Tap the function [Activate] on the function bar.
ð The status bar shows the method activated.
7.9.3 Starting freeze-drying
CAUTION
Risk of skin burns from touching parts of the ice condenser after completion of conditioning.
u Wear protective gloves when working on the instrument after the conditioning
phase.
NOTE
The freeze-drying process can be cancelled by tapping the functions [Manual] and
[Aerate] on the [Start] menu.
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Navigation path
➔ Start
If a gas is being used
Precondition:
R The instrument has been prepared.
R A method is selected.
u Fit a top-mount drying rack. See Chapter8 "Operating top-mount drying racks",
page73.
u Load the top-mount drying rack with frozen samples.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Start] on the function bar.
u Make sure that the specified gas is being used.
u Answer YES to the confirmation question.
ð The freeze-drying process starts.
ð The control panel shows the S tar t menu with a black background.
ð The system carries out the selected method.
If a gas is not being used
Precondition:
R The instrument has been prepared.
R A method is selected.
u Fit a top-mount drying rack. See Chapter8 "Operating top-mount drying racks",
page73.
u Load the top-mount drying rack with frozen samples.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Start] on the function bar.
ð The freeze-drying process starts.
ð The control panel shows the S tar t menu with a black background.
ð The system carries out the selected method.
7.9.4 Changing parameters while the process is running
NOTE
The method parameters can be adjusted while the freeze-drying process is in
progress. See Chapter7.6 "Editing a method", page57.
7.9.5 Ending freeze-drying
Navigation path
➔ Start
Precondition:
R The status bar is showing the status Hold.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Aerate] on the function bar.
u Answer YES to the confirmation question.
ð The system is vented.
ð The status bar shows the status Aerating.
u Wait until the status bar shows the status Unload / Load.
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u Remove the dried preparation from the top-mount drying rack.
7.9.6 Shutting down the instrument
NOTICE
Not completed shut down of the instrument.
An interruption while shutting down the instrument can damage the instrument.
u Shut down the instrument completely.
u If the shutdown was interrupted, tap the function [Defrost] on the function bar.
Time
80 min
required:
Navigation path
➔ Start
Precondition:
R The freeze-drying process has ended.
R The gas balast on the vacuum pump is open.
R Make sure that there is sufficient distilled water available.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Shut down] on the function bar.
ð The instrument is shutting down.
ð The status bar shows the remaining time and the status Shutting down.
ð After the instrument has shut down, the status bar shows the remaining time
and the status Defrosting.
ð After the defrosting, the status bar shows the status Standby.
7.9.7 Switching off the instrument
Precondition:
R The instrument has been shut down. See Chapter7.9.6 "Shutting down the instru-
ment", page69
u Switch the On/Off master switch to Off.
7.10 Performing freeze-drying manually [Pro control panel]
7.10.1 Preparing the instrument
Time
required:
Navigation path
➔ Start
Precondition:
R All commissioning operations have been completed. See Chapter5.2 "Putting the
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approx.
30min
instrument in operation", page24
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u Navigate to the [Start] menu via the navigation path.
u Tap the function [[Start conditioning]] on the function bar.
ð The temperature in the ice condenser cools down to operating temperature.
ð The vacuum pump is being brought up to operating temperature.
ð After completion of the conditioning phase, the status bar shows the status
Unload / Load.
7.10.2 Starting freeze-drying
CAUTION
Risk of skin burns from touching parts of the ice condenser after completion of conditioning.
u Wear protective gloves when working on the instrument after the conditioning
phase.
Navigation path
➔ Start
Precondition:
R The instrument has been prepared.
u Fit a top-mount drying rack. See Chapter8 "Operating top-mount drying racks",
page73.
u Load the top-mount drying rack with frozen samples.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Manual] on the function bar.
u Enter the required settings for the process parameters.
u Tap the function [Start] on the function bar.
ð The freeze-drying process starts.
ð The background color of the S tar t menu changes from white to black.
ð The status bar shows a clock counting up and the status Manual Drying.
ð The system evacuates to the set pressure.
Shutting down The instrument is shutting down.
The aeration valve and the drain valve
are closed.
The status bar shows the remaining
time.
7.10.3 Editing parameters while the process is running
Navigation path
➔ Start
Precondition:
R The process has been started.
u Navigate to the [Start] menu via the navigation path.
u Using the navigation control, navigate to the parameter that you wish to change.
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u Tap the function [Edit] on the function bar.
ð The control panel shows a dialog box with a numeric input box.
ð The control panel highlights the selected parameter in white.
u Enter the value in the numeric input box.
u Tap the function [Save] on the function bar.
ð The setting is saved.
ð The dialog box closes.
7.10.4 End point definition
To determine the end point of the freeze-drying process, a pressure rise test can be
carried out manually while freeze-drying is in progress.
Navigation path
➔ Configuration ➔ End point determination ➔ Pressure rise test
Precondition:
R The process has been started.
u Navigate to the action [[Pressure rise test]] via the navigation path.
u On the line [[Pressure limit]] enter the threshold that the pressure must be below.
u On the line [[Test duration]] set the length of time for which the pressure rise test is
to be carried out.
u Tap the function [[Start]] on the function bar.
ð The pressure rise test starts.
ð After completion of the pressure rise test, the [[Pressure rise test]] line shows
whether the pressure rise test has been passed or not.
7.10.5 Ending freeze-drying
Navigation path
➔ Start
Precondition:
R The sample is dry.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Aerate] on the function bar.
u Answer YES to the confirmation question.
ð The system is vented.
ð The status bar shows the status Aerating.
u As soon as the status bar shows the status Unload / Load, remove the dried sam-
ple from the drying rack.
7.10.6 Shutting down the instrument
NOTICE
Not completed shut down of the instrument.
An interruption while shutting down the instrument can damage the instrument.
u Shut down the instrument completely.
u If the shutdown was interrupted, tap the function [Defrost] on the function bar.
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Time
80 min
required:
Navigation path
➔ Start
Precondition:
R The freeze-drying process has ended.
R The gas balast on the vacuum pump is open.
R Make sure that there is sufficient distilled water available.
u Navigate to the [Start] menu via the navigation path.
u Tap the function [Shut down] on the function bar.
ð The instrument is shutting down.
ð The status bar shows the remaining time and the status Shutting down.
ð After the instrument has shut down, the status bar shows the remaining time
and the status Defrosting.
ð After the defrosting, the status bar shows the status Standby.
7.10.7 Switching off the instrument
Precondition:
R The instrument has been shut down. See Chapter7.10.6 "Shutting down the in-
strument", page71
u Switch the On/Off master switch to Off.
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8 Operating top-mount drying racks
8.1 Operating stoppering acrylic drying chamber
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Locate the springs in the holes on the main
plate.
u Place the intermediate plate on the main plate.
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u Loosen all fixing screws.
u Align the slots for the shelves.
u Tighten the fixing screws.
u Place the rack on the intermediate plate.
u Slide the shelves into the rack.
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u Press the plug onto the shelf connection and
turn the ring counterclockwise at the same
time.
(option)
u Turn the temperature sensor electrical con-
nector so that the marks on the connector and
the heatable shelf are parallel
u Press the temperature sensor electrical con-
nector onto the connection.
u Locate the cylinder in the groove above the
main plate.
u Check the O-ring for damage and grease it
with vacuum grease.
u Screw the hand wheel upwards until the plate
inside the lid has pressed the hooks all the
way in.
u Place the O-ring into the groove of the cover.
u Place the cover on the cylinder.
u Make sure that the hooks on the rack are en-
gaged.
u Carry out freeze-drying.
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Precondition:
R The status bar shows the status Stoppering.
u Turn the hand wheel, until all samples are
sealed.
u Confirm the verification question on the control
panel.
8.2 Operating manifold acrylic drying chamber (heatable shelves)
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Place the intermediate plate on the main plate.
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u Loosen all fixing screws.
u Align the slots for the shelves.
u Tighten the fixing screws.
u Place the rack on the intermediate plate.
u Slide the shelves into the rack.
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u Press the plug onto the shelf connection and
turn the ring counterclockwise at the same
time.
(option)
u Turn the temperature sensor electrical con-
nector so that the marks on the connector and
the heatable shelf are parallel
u Press the temperature sensor electrical con-
nector onto the connection.
u Locate the cylinder in the groove above the
main plate.
u Fit manifold valve onto the connection on the
top-mount drying rack.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove of the cover.
u Place the manifold cover on the cylinder.
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u Carry out freeze-drying.
8.3 Operating manifold acrylic drying chamber (non-heatable shelf)
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Place the intermediate plate on the main plate.
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u Place the rack on the intermediate plate.
u Locate the cylinder in the groove above the
main plate.
u Fit manifold valve onto the connection on the
top-mount drying rack.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove of the cover.
u Place the manifold cover on the cylinder.
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u Carry out freeze-drying.
8.4 Operating acrylic drying chamber (heatable shelf)
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Place the intermediate plate on the main plate.
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u Loosen all fixing screws.
u Align the slots for the shelves.
u Tighten the fixing screws.
u Place the rack on the intermediate plate.
u Slide the shelves into the rack.
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u Press the plug onto the shelf connection and
turn the ring counterclockwise at the same
time.
(option)
u Turn the temperature sensor electrical con-
nector so that the marks on the connector and
the heatable shelf are parallel
u Press the temperature sensor electrical con-
nector onto the connection.
u Locate the cylinder in the groove above the
main plate.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove of the cover.
u Place the cover on the cylinder.
u Carry out freeze-drying.
8.5 Operating acrylic drying chamber (non-heatable shelf)
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
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u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Place the intermediate plate on the main plate.
u Place the rack on the intermediate plate.
u Locate the cylinder in the groove above the
main plate.
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u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove of the cover.
u Place the cover on the cylinder.
u Carry out freeze-drying.
8.6 Operating manifold drying rack
u Make sure that the groove above the ice con-
denser is clean, free of dust and not
scratched.
u Check the O-ring for damage and grease it
with vacuum grease.
u Place the O-ring into the groove on the ice
condenser.
u Place the main plate on the ice condenser.
u Make sure that the groove on the ice con-
denser is clean, free of dust and not
scratched.
u Check the 300mm dia. O-ring for damage and
grease it with vacuum grease.
u Place the 300mm dia. O-ring in the groove in
the main plate.
u Fit manifold valve onto the connection on the
top-mount drying rack.
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u Place the base plate on the main plate.
u Place the seal on the connection.
u Fit the manifold drying rack onto the seal and
fix it with the clamp.
u Carry out freeze-drying.
8.7 Determining the number of flasks
NOTE
Do not overfill flasks
Maximum volume of the samples ≤ half of the flask volume
NOTE
The number of flasks used should be determined individually for every process.
The number of flasks used is dependent on the following factors:
The volume of the flask
The method of freezing
The concentration of the sample
The composition of the solvent
Number of flasks using water as an example
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1
2
A
B
Flask volume 1000 mL Flask volume 500 mL
Rotating freezing Max. 22 flasks Max. 22 flasks
Static freezing Max. 36 flasks Max. 36 flasks
8.8 Operating manifold valves
The lever on a manifold valve can be set to the following positions:
Position Function
A: Lever pointing up The connected vessel is evacuated.
B: Lever pointing down The connected vessel is vented.
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9 | Cleaning and servicing BÜCHI Labortechnik AG
9 Cleaning and servicing
NOTE
Users may only carry out the servicing and cleaning operations described in this section.
Any servicing and repair work which involves opening up the casing may only be carried out by BUCHI service technicians.
9.1 Regular maintenance work
Component Action Interval
Vacuum Pump u Carry out maintenance according to
the manufacturer's instructions. See
relevant documentation.
See manufacturer's
instructions
Top-mount drying
racks
O-ring, dia.
300mm
u Wipe down the top-mount drying
racks with a damp cloth.
u If heavily soiled, use a mild detergent.
u Wipe down the 300mm O-rings with
a damp cloth.
u Check for scratches and other dam-
age.
u Replace the 300mm O-ring if it is
damaged.
u Grease with vacuum grease if neces-
sary.
u Replace the 300mm O-ring. Annually
Seals
ISO-KF 16
Seals
ISO-KF 25
u Wipe down the seals with a damp
cloth.
u Check for scratches and other dam-
age.
u Replace seals if they are damaged.
Vacuum tubing u Wipe down the vacuum tube with a
damp cloth.
u Check for damage.
u Replace the vacuum tube if it is dam-
aged.
Daily
Daily
Annually
Annually
Space above ice
condensers
u Wipe down the space between the ice
condensers with a damp cloth.
u If heavily soiled, use ethanol or a mild
Daily
detergent.
Casing u Wipe down the casing with a damp
Weekly
cloth.
u If heavily soiled, use ethanol or a mild
detergent.
Warning symbols u Check that the warning symbols on
Weekly
the instrument are legible.
u If they are dirty, clean them.
Heat exchanger
Heater
u Remove dust and foreign objects
from the ventilation slots using com-
Monthly
pressed air or a vacuum cleaner.
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Component Action Interval
View u Wipe down the display with a damp
Monthly
cloth.
Ice condenser u Clean the ice condenser. See Chap-
ter9.4 "Cleaning the ice condenser",
page93
9.2 Performing a vacuum test
The vacuum test checks the performance capacity of the vacuum system.
Time
required:
Navigation path
➜ Configuration ➜ Servicing ➜ Vacuum test
Precondition:
R Conditioning of the instrument has been completed.
R A top-mount drying rack is fitted.
R The top-mount drying rack does not contain sample.
u Navigate to the action [Vacuum Test] via the navigation path.
u Specify a required setting for the vacuum to be achieved.
u Specify a required time within which the vacuum is to be reached.
u Tap the function [Start] on the function bar.
max. 10 min
ð The vacuum test starts.
Annually
ð The status bar shows the status Vacuum Test.
ð If the vacuum pressure is not below 500 mbar after 30 s, the vacuum test au-
tomatically aborts.
ð After completion of the vacuum test, the [Vacuum test] line shows whether the
vacuum test has been passed or not.
Troubleshooting after failed vacuum test
Possible cause Action
Top-mount drying rack not correctly fitted Fit the top-mount drying rack correctly.
Top-mount drying rack is damaged Check function of PMMA parts, replace
manifold valves, clean drain valve.
O-rings dirty Wipe down the O-rings with a damp
cloth.
O-rings damaged Check O-rings and replace if necessary.
Groove of O-rings dirty Wipe groove of O-rings with a damp
cloth.
KF clamps not closed Close the KF clamps.
KF seals dirty Wipe down the KF seals with a damp
cloth.
KF seals damaged Inspect KF seals and replace as neces-
sary.
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9 | Cleaning and servicing BÜCHI Labortechnik AG
111
Possible cause Action
The pump connected is not delivering
sufficient performance
Carry out vacuum test with a different
vacuum pump.
9.3 Performing a leak test
9.3.1 Performing a leak test with a drying chamber
The leak test checks the vacuum system for possible leaks.
Time
45 min
required:
NOTE
The leak test can be aborted by tapping [Stop] on the function bar.
Navigation path
➜ Configuration ➜ Servicing ➜ Leak test
Precondition:
R Conditioning of the instrument has been completed.
R A top-mount drying rack is fitted.
R The top-mount drying rack does not contain sample.
u Navigate to the action [Leak test] via the navigation path.
u On the [Ice Condenser] line, enter a required setting for the vacuum.
u On the [Shelf temperature] line enter the required shelf temperature.
u On the [Test scope] line select the component to be tested.
u On the [Drying shelf heating] line switch the drying shelf heating on or off.
u On the [Volume] line enter the actual volume of the components to be tested.
The following options are available:
Ice condenser 1
24.4L 47.2L
Acrylic drying chamber
(with 4 drying shelves)
54.1L
Acrylic drying chamber
(with 6 drying shelves)
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BÜCHI Labortechnik AG Cleaning and servicing | 9
222
1 2
1 2
1 2
Ice condenser 2
24.4L 47.2L
Acrylic drying chamber
(with 4 drying shelves)
Both ice condensers
33.5L 56.3L
Acrylic drying chamber
(with 4 drying shelves)
u Tap the function [Start] on the function bar.
ð The leak test starts.
ð The status bar shows the status Leak Test.
54.1L
Acrylic drying chamber
(with 6 drying shelves)
63.2L
Acrylic drying chamber
(with 6 drying shelves)
ð When the leak test is completed, the [Leak test] tab indicates whether the leak test
was successful.
ð The leak test is passed if the measured leakage rate is less than the pre-set rate
of 10.10mbar*L/h.
Troubleshooting after failed leak test
Possible cause Action
Top-mount drying rack not correctly fitted Fit the top-mount drying rack correctly.
O-rings dirty Wipe down the O-ring with a damp cloth.
O-rings damaged Check O-rings and replace if necessary.
Groove of O-rings dirty Wipe groove of O-rings with a damp
cloth.
KF clamps not closed Close the KF clamps.
KF seals dirty Wipe down the KF seals with a damp
cloth.
KF seals damaged Inspect KF seals and replace as neces-
sary.
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9 | Cleaning and servicing BÜCHI Labortechnik AG
121 2
Possible cause Action
Pump oil dirty Service according to manufacturer's in-
structions.
Leaking manifold valves
(manifold acrylic drying chamber only)
Replace leaking manifold valve.
Locate leaking manifold valve. See
Chapter10.3 "Locating leaking manifold
valve", page96
9.3.2 Performing leak test with a manifold drying rack
The leak test checks the vacuum system for possible leaks.
Time
45 min
required:
NOTE
The leak test can be aborted by tapping [Stop] on the function bar.
Navigation path
➜ Configuration ➜ Servicing ➜ Leak test
Precondition:
R Conditioning of the instrument has been completed.
u Fit the base plate with a KF 40 blind flange, an ISO-KF 40 seal and an ISO-KF 4
clamp.
u Navigate to the action [Leak test] via the navigation path.
u On the [Ice Condenser] line, enter a required setting for the vacuum.
u On the [Shelf temperature] line enter the required shelf temperature.
u On the [Test scope] line select the component to be tested.
u On the [Drying shelf heating] line switch the drying shelf heating on or off.
u On the [Volume] line enter the actual volume of the components to be tested.
The following options are available:
24.4L 24.4L 33.5L
u Tap the function [Start] on the function bar.
ð The leak test starts.
ð The status bar shows the status Leak Test.
ð When the leak test is completed, the [Leak test] tab indicates whether the leak test
was successful.
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BÜCHI Labortechnik AG Cleaning and servicing | 9
ð The leak test is passed if the measured leakage rate is less than the pre-set rate
of 10.10mbar*L/h.
NOTE
To test the leak-tightness of the manifold drying rack, carry out another leak test with
the manifold drying rack installed.
Troubleshooting after failed leak test
Possible cause Action
Top-mount drying rack not correctly fitted Fit the top-mount drying rack correctly.
O-rings dirty Wipe down the O-ring with a damp cloth.
O-rings damaged Check O-rings and replace if necessary.
Groove of O-rings dirty Wipe groove of O-rings with a damp
cloth.
KF clamps not closed Close the KF clamps.
KF seals dirty Wipe down the KF seals with a damp
cloth.
KF seals damaged Inspect KF seals and replace as neces-
sary.
Pump oil dirty Service according to manufacturer's in-
Leaking manifold valves
(only if manifold drying rack installed)
9.4 Cleaning the ice condenser
Opening intermediate valve
Navigation path
➔ Configuration ➔ Service ➔ Ice condenser
Precondition:
R The instrument is in standby mode. See Chapter7.9.6 "Shutting down the instru-
ment", page69
u Navigate to the Ice co ndenser view via the navigation path.
u Open the intermediate valve of the ice condensers.
Cleaning the ice condenser
Navigation path
structions.
Replace leaking manifold valve.
Locate leaking manifold valve. See
Chapter10.3 "Locating leaking manifold
valve", page96
➔ Configuration ➔ Service ➔ Defrosting system
Precondition:
R A receiving vessel is installed. See Chapter5.2.5 "Fitting the drain tubes", page26
u Pour approx. 5 L of warm water into the ice condenser through the open interme-
diate valve.
u Leave it to take effect for five minutes.
u Navigate to the Def ros ting sy ste m view via the navigation path.
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9 | Cleaning and servicing BÜCHI Labortechnik AG
u Tap the action [Drain valve 1].
ð The control panel shows the drain valve highlighted in green.
u Tap the function [Open] on the function bar.
u Tap the action [Drain valve 2].
ð The control panel shows the drain valve highlighted in green.
u Tap the function [Open] on the function bar.
u Wait until the water has run off.
u Tap the action [Drain valve 1].
ð The control panel shows the drain valve highlighted in green.
u Tap the function [Close] on the function bar.
u Tap the action [Drain valve 2].
ð The control panel shows the drain valve highlighted in green.
u Tap the function [Close] on the function bar.
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BÜCHI Labortechnik AG Help with faults | 10
10 Help with faults
10.1 Troubleshooting
Problem Possible cause Action
Compressor fails to
start or switches off
No power supply to compressor
u Check the power supply
and switch on the device.
Compressor overheated u Allow the compressor to
cool down.
u Check ambient conditions.
Cooling tempera-
Wrong ambient conditions Adjust ambient conditions.
ture is not achieved
Too much ice in the ice condenser
10.2 Faults, possible causes and remedies
Malfunction Possible cause Remedy
Instrument does
not work
Vacuum is not
achieved
Instrument is not connected to
the power supply.
Vacuum system is leaking. u Carry out a leak test (see
Vacuum pump is too weak. u Use a vacuum pump with a
See Installation site
Defrost the ice condenser.
u Make sure that the power
supply is connected and
switched on.
Performing a leak test).
u Carry out a vacuum test
(see Chapter9.2 "Performing a vacuum test",
page89).
u If necessary, replace tub-
ing and/or seals.
performance of at least 9
m3/h.
u Carry out maintenance
work according to the vacuum pump manufacturer's
documentation.
Drain valve is leaking. u Check whether closed
drain tube contracts. If it
does, contact BUCHI Service.
Instrument is not
vented
The connection for the gas
supply is blocked.
u Make sure that gas is able
to flow into the instrument
through the gas supply
connection.
u Clean the air filter (option).
One of the ice condensers is overfilled with ice
Operation Manual Lyovapor™ L-300/L-300 Pro 95/106
The instrument only uses one
ice condenser.
u See Chapter10.4 "Manu-
ally defrosting ice condenser", page96
Page 96
10 | Help with faults BÜCHI Labortechnik AG
10.3 Locating leaking manifold valve
Navigation path
➔ Start
Precondition:
R The system does not evacuate to less than 0.1 mbar.
u Navigate to the Sta rt view via the navigation path.
u Set the vacuum to 0.5 mbar.
u Tap the function [Start] on the function bar.
u Turn each manifold valve individually while checking the display to see if the ac-
tual pressure changes.
u If the vacuum decreases in the case of one of the manifold valves, then that valve
is the one that is leaking.
u Tap the function [Aerate] on the function bar.
u Replace the manifold valve concerned.
10.4 Manually defrosting ice condenser
Opening intermediate valve
Navigation path
➔ Configuration ➔ Service ➔ Ice condenser
Precondition:
R The instrument is in standby mode. See Chapter7.9.6 "Shutting down the instru-
ment", page69
u Navigate to the Ice co ndenser view via the navigation path.
u Open the intermediate valve of the ice condenser concerned.
Defrosting the ice condenser
Navigation path
➔ Configuration ➔ Service ➔ Defrosting system
Precondition:
R A receiving vessel is installed. See Chapter5.2.5 "Fitting the drain tubes", page26
u Pour approx. 5 L of warm water into the ice condenser through the open interme-
diate valve.
u Leave it to take effect for five minutes.
u Navigate to the Def ros ting sy ste m view via the navigation path.
u Tap the drain valve that is to be opened.
ð The control panel shows the drain valve highlighted in green.
u Tap the function [Open] on the function bar.
u Wait until the water has run off.
u Tap the function [Close] on the function bar.
u Repeat the instructions for defrosting the ice condenser until the temperature of
the defrosting water matches the ambient temperature.
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BÜCHI Labortechnik AG Taking out of service and disposal | 11
11 Taking out of service and disposal
11.1 Disposal
The operator is responsible for proper disposal of the Lyovapor™.
CAUTION
Potential environmental hazard
The refrigerants R507 and R1150 are used in the instrument. Those refrigerants are
toxic and must not be allowed to enter the soil or groundwater.
u Dispose of the appliance properly, if necessary using a professional disposal ser-
vice.
u When disposing of equipment observe the local regulations and statutory require-
ments regarding waste disposal.
11.2 Returning the instrument
Before returning the instrument, contact the BÜCHI Labortechnik AG Service Department.
https://www.buchi.com/contact
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12 | Appendix BÜCHI Labortechnik AG
12 Appendix
12.1 Spare parts and accessories
Use only genuine BUCHI consumables and spare parts in order to ensure correct,
safe and reliable operation of the system.
NOTE
Any modifications of spare parts or assemblies are only allowed with the prior written
permission of BUCHI.
12.1.1 Accessories
Description Order no. Image
Pirani pressure sensor Inficon PSG 550 11062229
Capacitive pressure sensor Inficon CDG
020 D
PT1000 sample temperature sensor 11064031
Level sensor capacitive, for water canister
12.1.2 Further accessories
Description Order no. Image
Set for defrost and waste water
incl. canisters, level sensors, tubing
11062230
11069608
11067317
Canister 20 L, for waste and defrosting
water
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BÜCHI Labortechnik AG Appendix | 12
Description Order no. Image
Air filter 11057925
SD-Card 1 GB 11064730
Connection cable, for vacuum pump 11064934
12.1.3 Spare parts
Description Order no. Image
User interface 11063580
User interface Pro 11063581
O-Ring Ø 300 mm 11065367
O-Ring Ø 430 mm 11065343
Vacuum hose, KF 25, L 1000 mm 11066031
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12 | Appendix BÜCHI Labortechnik AG
Description Order no. Image
Vacuum clamp KF 16 11064939
Vacuum clamp KF 25 11063662
Vacuum clamp, KF 40 11063663
Vacuum seal KF 16 11063455
Vacuum seal KF 25 11063457
Vacuum seal KF 40 11063659
O-Ring, Silicone, 94.61 x 6.99 mm 11062420
O-Ring, Silicone, 161.3 x 5.33 mm 11062421
Vacuum flange adapter, stainless steel,
11064870
KF 16 to KF 25
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