Christ Alpha 2-4 LDplus, Alpha 1-4 LDplus, Alpha 1-2 LDplus, 101521 Operating Manual

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Translation of the original operating manual sb
Freeze-dryer
Rev. 2.2 of 17/10/2016 Alpha 1-4 LDplus;Freeze-dryer;Alpha 2-4 LDplus; ;
Version 11/2006
Alpha 1-4 LDplus
Part no. 101541
Alpha 2-4 LDplus
Part no. 101542
Freeze-dryer
Operating Manual
Please retain for later use!
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In case of inquiries, please state the following numbers:
Order number:
Serial number:
© Copyright by Martin Christ Gefriertrocknungsanlagen GmbH An der Unteren Söse 50 37520 Osterode am Harz Germany Tel.: +49 (0) 5522 / 5007-0 Fax: +49 (0) 5522 / 5007-12 Web: www.martinchrist.de E-mail: [email protected]
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1 General information ............................................................................................................. 9
1.1 Importance of the operating manual .................................................................................. 9
1.2 Intended use ..................................................................................................................... 9
1.3 Warranty and liability....................................................................................................... 10
1.4 Copyright ........................................................................................................................ 10
1.5 Explanation of symbols ................................................................ ................................... 10
1.6 Standards and regulations .............................................................................................. 10
1.7 Scope of supply .............................................................................................................. 10
2 Layout and mode of operation .......................................................................................... 11
2.1 Layout of the freeze-dryer ............................................................................................... 11
2.1.1 Functional and operating elements ............................................................................ 11
2.1.2 Name plate ................................................................................................................ 13
2.2 Mode of operation ........................................................................................................... 14
2.2.1 General information on freeze-drying ................................................................ ......... 14
2.2.2 Freeze-drying process ............................................................................................... 17
2.2.2.1 Preparation ........................................................................................................ 17
2.2.2.2 Freezing ............................................................................................................. 17
2.2.2.3 Main drying ........................................................................................................ 18
2.2.2.4 Final drying ........................................................................................................ 19
2.2.2.5 End of drying and aeration ................................................................................. 19
2.2.2.6 Defrosting .......................................................................................................... 20
3 Safety .................................................................................................................................. 21
3.1 Marking of the unit .......................................................................................................... 21
3.2 Explanation of the symbols and notes ............................................................................. 22
3.3 Responsibility of the operator .......................................................................................... 23
3.4 Operating personnel ....................................................................................................... 23
3.5 Informal safety instructions ............................................................................................. 24
3.6 Safety instructions .......................................................................................................... 24
3.6.1 Electrical safety ......................................................................................................... 25
3.6.2 Mechanical safety ...................................................................................................... 25
3.6.3 Fire prevention ................................ ................................................................ ........... 26
3.6.4 Thermal safety ........................................................................................................... 26
3.6.5 Chemical and biological safety .................................................................................. 26
3.7 Safety devices ................................ ................................................................................ 27
3.7.1 System check ............................................................................................................ 27
3.7.2 Earth conductor check ............................................................................................... 27
3.8 Procedures in the event of hazards and accidents .......................................................... 27
3.9 Remaining hazards ......................................................................................................... 28
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4 Storage and transport ....................................................................................................... 29
4.1 Dimensions and weight ................................................................................................... 29
4.2 Storage conditions .......................................................................................................... 29
4.3 Notes on transport .......................................................................................................... 30
4.4 Packaging ....................................................................................................................... 31
4.5 Transport safety device ................................................................................................... 31
5 Set-up and connection ...................................................................................................... 32
5.1 Installation site ................................................................................................................ 32
5.2 Power supply .................................................................................................................. 33
5.2.1 Connection ................................................................................................................ 33
5.2.2 Customer-provided fuses ........................................................................................... 33
5.3 Aeration and media drain valve ....................................................................................... 33
5.4 Vacuum sensor ............................................................................................................... 34
5.5 Vacuum pump................................................................................................................. 36
5.6 Pressure control valve .................................................................................................... 37
5.7 Rubber valves ................................................................................................................. 38
6 Operation ............................................................................................................................ 39
6.1 Initial start-up .................................................................................................................. 39
6.2 Installation of accessories ............................................................................................... 39
6.3 Preparation ..................................................................................................................... 39
6.4 Switching the freeze-dryer on ......................................................................................... 39
6.5 LDplus control system ..................................................................................................... 40
6.5.1 User interface ............................................................................................................ 40
6.5.2 Mode ......................................................................................................................... 43
6.5.3 Main menu ................................................................................................................. 45
6.5.3.1 Changing set values .......................................................................................... 45
6.5.3.2 Special functions ................................................................................................ 47
6.5.3.3 Process and equipment information ................................................................... 48
6.5.3.4 Options .............................................................................................................. 49
6.5.3.5 Tutorial ............................................................................................................... 51
6.6 Switching the freeze-dryer OFF ...................................................................................... 52
7 Malfunctions and error correction .................................................................................... 53
7.1 General malfunctions ...................................................................................................... 53
7.1.1 Power failure .............................................................................................................. 53
7.1.2 Insufficient vacuum .................................................................................................... 53
7.1.2.1 Small flange connections ................................................................................... 53
7.1.2.2 Aeration and media drain valve .......................................................................... 54
7.1.2.3 Pressure control valve ........................................................................................ 55
7.1.2.4 Rubber valves .................................................................................................... 55
7.1.2.5 Vacuum sensor ................................................................................................ .. 55
7.1.3 Insufficient ice condenser temperature ................................................................ ...... 55
7.2 Process and equipment messages ................................................................................. 56
7.3 Service contact ............................................................................................................... 58
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8 Maintenance and service ................................................................................................... 59
8.1 Maintenance ................................................................................................................... 59
8.1.1 General ...................................................................................................................... 59
8.1.1.1 Ice condenser chamber ...................................................................................... 60
8.1.1.2 Aeration valve, media drain valve ...................................................................... 60
8.1.1.3 Heat exchanger (only for air-cooled freeze-dryers) ............................................ 61
8.1.2 Vacuum pump ........................................................................................................... 61
8.1.3 Exhaust filter (oil mist separator) ................................................................................ 62
8.1.4 Vacuum sensor .......................................................................................................... 62
8.1.5 Accessories ............................................................................................................... 62
8.2 Disinfection of the drying chamber and accessories ....................................................... 63
8.3 Service ........................................................................................................................... 64
8.4 Return of defective parts ................................................................................................. 64
9 Disposal .............................................................................................................................. 66
9.1 Disposal of the freeze-dryer ............................................................................................ 66
9.2 Disposal of the packaging ............................................................................................... 66
10 Technical data .................................................................................................................... 67
10.1 Ambient conditions ......................................................................................................... 69
10.2 Technical documentation ................................................................................................ 69
11 Appendix ............................................................................................................................ 70
11.1 Brief operating instructions ............................................................................................. 70
11.2 EC declaration of conformity in accordance with the EC Machinery Directive ................. 75
11.3 Declaration of conformity – China RoHS 2 ...................................................................... 77
11.4 Resistance to stress cracking and chemical influences "Plexiglas" ................................. 79
12 Glossary ............................................................................................................................. 97
13 Index ................................................................................................................................... 99
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1 General information
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1.1 Importance of the operating manual
A fundamental requirement for the safe and trouble-free operation of the unit is to be familiar with the fundamental safety instructions and all possible hazards.
The operating manual includes important information concerning the safe operation of the freeze-dryer.
This operating manual, and in particular the notes on safety and hazards, must be observed by all persons operating the unit.
In addition, the local rules and regulations for the prevention of accidents
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must be complied with.
1.2 Intended use
CHRIST freeze-dryers have been solely designed for the freeze-drying of solid or liquid products in ampoules, vials or dishes. They are, therefore, solely intended for these applications.
The freeze-dryer is suitable
• for freeze-drying materials such as bacteria and virus cultures, blood plasma, serum fractions, antibodies, sera, vaccines, and pharmaceutical products
• for freeze-drying plant extracts, e.g. for biochemical tests
• for freeze-drying inorganic materials, e.g. nanoparticles
• for freeze-drying numerous other products (for further information
please contact our qualified personnel)
Any other use beyond this area of application is regarded as improper use. Martin Christ Gefriertrocknungsanlagen GmbH cannot be held liable for any damage resulting from such improper use.
The intended use also includes:
• observation of all the notes and instructions included in the operating manual
• compliance with the inspection and maintenance instruction
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• prohibition of any type of extensions to, or conversions of the unit.
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1.3 Warranty and liability
The warranty and liability are subject to our "General Terms and Conditions" that were distributed to the operator upon the conclusion of the contract.
Warranty and liability claims are excluded if they are due to one or several of the following reasons:
• improper use
• non-compliance with the safety instructions and hazard warnings in the
operating manual
• improper installation, start-up, operation, and maintenance of the
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freeze-dryer.
1.4 Copyright
The copyright concerning the operating manual remains with Martin Christ Gefriertrocknungsanlagen GmbH.
The operating manual is solely intended for the operator and their personnel. It includes instructions and information that may not be
• duplicated,
• distributed, or
• communicated in any other way neither in full nor in parts.
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Non-compliance may be prosecuted under criminal law.
1.5 Explanation of symbols
In this operating manual, specialist terms that are explained in the glossary (see chapter 12 - "Glossary") are marked by an arrow and printed in italics
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(e.g. sublimation).
1.6 Standards and regulations
EC declaration of conformity in accordance with the EC Machinery Directive (see chapter 11.2 - "EC declaration of conformity in accordance
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with the EC Machinery Directive")
1.7 Scope of supply
The scope of supply comprises:
• 1 tube of high-vacuum grease
• 1 litre of vacuum pump oil (only if a pump is included)
• 1 set of flange components and several small parts for service and
maintenance purposes
• 1 drain hose 0.5 m (silicone 8 x 12 mm)
• 1 operating manual
Accessories and commissioning
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According to your order, our order confirmation, and our delivery note.
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1 Ice condenser
chamber with an internal ice condenser
2 User interface (see
chapter 6.5.1 - "User interface")
3 Mains power switch
4 Pipe connection of the
vacuum pump (behind the cover plate)
5 Ice condenser
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2 Layout and mode of operation
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2.1 Layout of the freeze-dryer
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2.1.1 Functional and operating elements
Fig. 1: Total view of the freeze-dryer
Fig. 2: Ice condenser chamber
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6 Equipotential bonding
screw
7 Aeration and media
drain valve
8 Vacuum connection 9 Name plate (see
chapter 2.1.2 - "Name plate")
10 Heat exchanger of the
refrigeration unit
11 Electrical connection of
the vacuum sensor
12 Power supply of the
pressure control valve
13 Power supply of the
vacuum pump 14 Mains fuse 15 Mains cable
Fig. 3: Left side of the freeze-dryer
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Fig. 4: Rear view of the freeze-dryer
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1 Serial number 2 Type 3 Refrigerant data of
the 1st stage 4 Nominal voltage 5 Year of manufacture
(month/year) 6 Part number 7 Refrigerant data of
the 2nd stage 8 Rated current /
apparent power
Fig. 5: Example of a name plate (here: Alpha 2-4 LDplus)
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2.1.2 Name plate
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2.2 Mode of operation
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2.2.1 General information on freeze-drying
What is freeze-drying?
Freeze-drying or lyophilisation is a procedure for the gentle drying of high­quality products. The product is dried by sublimation without passing through the liquid phase.
What are typical applications for freeze-drying?
As far as their sheer quantity is concerned, foodstuffs are the major application for freeze-drying. One widely known example is the production of granulated instant coffee or the drying of fruit, e.g. for breakfast cereals. Other areas of application are the restoration of water-damaged documents or the drying of archaeological artefacts.
Another important area of application is the drying of biotechnological and pharmaceutical products, e.g. tissues and tissue extracts, bacteria, vaccines, and sera. Products that would not keep well when they are dissolved in water can be preserved by freeze-drying. During this process, the biological properties of these sensitive substances are preserved. The compounds remain unchanged from a qualitative and quantitative point of view. After the addition of water, the products will have the same characteristics as the original products.
How does freeze-drying work?
Freeze-drying is a very gentle procedure for the extraction of water from a product in the frozen state. The drying process takes place through sublimation, i.e. the direct transition of a product from the solid phase to the gas phase. This happens under vacuum.
The following section describes the process of sublimation based on the example of water, since most products that are processed by freeze-drying are aqueous solutions. Their behaviour is based on identical fundamental principles.
The vapour pressure curve above ice describes the phase transition as a function of the pressure and temperature. The higher the temperature is, the higher the vapour pressure.
• If the vapour pressure is higher than 6.11 mbar (A), water passes through all three phases: solid, liquid, and gas (see the illustration).
• If the vapour pressure is below 6.11 mbar (B) and energy is added, the ice will be directly converted into water vapour once the sublimation curve is reached. This transition is called “sublimation”. If thermal energy is added to pure ice with a temperature of less than –30°C at a pressure of 0.37 mbar, it will be converted into water vapour once it reaches –30°C (see figure).
The vacuum prevents the melting of ice when energy is added. If thermal energy is added to a frozen product under vacuum, thawing of the product will be prevented and the water that is contained within the product will be released in the form of water vapour.
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6.11 mbar
0.37 mbar
-30°C
B
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Triple point
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Fig. 6: Vapour pressure curve above ice
From a physical point of view, the freeze-drying process covers three phases (see figure below):
(1) Freezing: The product to be dried is frozen under atmospheric pressure. This can be done either directly in the freeze-dryer or in a separate deep­freeze. The freezing temperature should be approximately 10°C below the solidification point of the product.
(2) Evacuation: When the product is sufficiently frozen, the vacuum pump is activated. The pressure inside the drying chamber will be lowered to the value that corresponds to the freezing temperature in accordance with the vapour pressure curve above ice.
(3) Sublimation: Thermal energy is added to the product, thus starting the sublimation process. Due to the added energy, the water in the product is converted into water vapour. Since the ice condenser is much colder than the product that is to be dried, the vapour pressure in the ice condenser is considerably lower than above the product. As a result, the water vapour that is released by the product streams to the ice condenser, where it condenses on the condenser coils.
Once the free water has been extracted from the product during the main drying phase, the last traces of bound water will also be removed at a final pressure that is as low as possible and at higher temperatures. This takes place by way of desorption. This drying phase is also called final drying.
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NOTE
Please find further information about basic principles, optimum procedures and applications in the brochure "Smart freeze-drying", which can be downloaded at www.martinchrist.de [Applications].
1
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1 bar
20°C
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Fig. 7: Freeze-drying phases
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2.2.2 Freeze-drying process
The main components of a freeze-dryer are:
• vacuum drying chamber with a temperature control system for adding thermal energy
• vacuum pump for generating a vacuum inside the drying chamber
• ice condenser for binding the water vapour that is released by the
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2.2.2.1 Preparation
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2.2.2.2 Freezing
product.
The ice condenser chamber must be clean and dry. Any water residues from a preceding drying run must be removed.
The media drain valve and the aeration valve must be closed. In the case of units that are equipped with a pressure control valve
(standard on LSCplus units), the vacuum pump should be warmed up (“warm-up”) for at least 15 minutes prior to the start of the main drying phase. Do not subject the vacuum pump to condensable gases until the operating temperature is reached. In this way, the service life of the vacuum pump can be extended.
At the same time, the ice condenser is pre-cooled ("cool-down"). The ice condenser temperature does not have any influence on the product temperature. The sole purpose of the ice condenser is to bind the released water vapour.
First, the product that is to be dried is frozen. This can be carried out either directly in the freeze-dryer or in a separate deep-freeze. Especially in the case of small filling quantities, we recommend pre-cooling the shelves as well in order to prevent the product from thawing during the evacuation.
Two very different structures of the frozen material can be distinguished:
• crystalline structures with clearly distinguishable crystals
• amorphous structures with no crystal junctions at all (e.g. glass)
The majority of the freeze-drying products have a crystalline form. When freezing these kinds of products, one must take into consideration
that too deep and too quick freezing leads to smaller ice crystals, which has a negative effect on the duration of the drying process.
For every product to be dried, the solidification point must be determined as a first step. This is the point at which the water that is contained in the product has completely crystallised. In order to ensure an optimum freeze­drying process, the product temperature should be approximately 10°C below the solidification point.
A layer thickness of the product of 1-2 cm should not be exceeded, since otherwise the drying duration would be negatively affected. If liquids are to be dried in bottles with a layer thickness of more than 1 cm, we recommend freezing them in a cooling bath with the aid of a shell or spin freezing device (see figure). Due to the centrifugal force, the liquid to be frozen will rise on the inner wall of the bottle and freeze. This procedure reduces the layer thickness and, thereby, the total drying time will be shortened to a considerable extent (see figures on the right side).
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Fig. 8: Shell freezing
Fig. 9: Cooling bath with spin freezing device
Fig. 10: Spin freezing
NOTE
If the product that is to be dried contains solvents or high salt concentrations, it may start to thaw during the drying process, which is indicated by clearly visible foaming. In order to prevent this, the product must be frozen as deeply as possible, e.g. with the aid of liquid nitrogen, prior to putting it into the unit.
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2.2.2.3 Main drying
When the product is frozen to a sufficiently deep extent, the main drying phase commences. The vacuum pump is switched on. The pressure inside the drying chamber will be lowered to the value that corresponds to the freezing temperature in accordance with the vapour pressure curve above ice. At the same time, thermal energy will be added to the product. In the case of products in round-bottom flasks, wide-neck bottles, etc., this is realised through the environment that is considerably warmer (direct contact heat), in the case of unheated shelves by way of thermal radiation from the environment, and in the case of temperature-controlled shelves directly via the shelves. As a result, the sublimation process starts.
At the beginning of the drying process, the maximum drying rate will be reached. The more the sublimation area recedes into the product, the further the produced water vapour must pass through the layers that have already been dried.
Under certain conditions, it is possible that the vacuum inside the ice condenser chamber increases during the main drying phase (e.g. from 0.63 mbar to 0.47 mbar) although the valve towards the vacuum pump is closed. From a physical point of view, this is due to the pumping effect of the ice condenser ("cryo-pumping effect").
The required drying time depends strongly on the drying vacuum. At 1.0 mbar, one gram of ice takes up a volume of 1 m3 of vapour, at 0.1 mbar a volume of 10 m3 of vapour, and at 0.001 mbar a volume of 100 m3. The closer the vacuum is to the solidification point, the smaller is the resulting vapour volume. The drying rate increases and the drying time decreases.
The end of the main drying phase is reached, when the product temperature and the shelf temperature are nearly identical. The temperature difference between the shelf and the product should be
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approximately 3 K to 5 K.
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2.2.2.4 Final drying
Final drying is an option whenever one requires a product with minimal residual moisture. In the physical sense, this process is a desorption process, i.e. the removal of adsorptively bound water. Final drying is performed under the lowest possible final pressure that depends on the ice condenser temperature in accordance with the vapour pressure curve above ice as well as on the final vacuum of the vacuum pump that is used.
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The process is supported by a higher shelf temperature.
2.2.2.5 End of drying and aeration
The end of the drying process is reached when both the product and shelf temperature are clearly in the positive range (+15 to +20°C) and if their difference is not greater than 5 K.
Another indication of the end of the drying process is the behaviour of the vacuum and of the ice condenser temperature. The ice condenser is no longer subject to load and reaches the final temperature of approximately ­55°C or -85°C. The pressure in the drying chamber decreases in accordance with the ice condenser temperature.
The vacuum pump will be switched off and the drying chamber will be aerated via a rubber valve or via the aeration valve. The aeration valve can also be used to flood the unit with nitrogen or another inert gas instead of ambient air.
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Then, the product can be removed from the unit.
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1 Cover plate
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2.2.2.6 Defrosting
Defrosting of the ice condenser is carried out at room temperature or with warm water.
• At a maximum, the ice condenser chamber may be half filled with water.
• Ensure that no water gets into the pipe connection of the vacuum pump
and the vacuum sensor (behind the cover plate, see figure)
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Fig. 11: Eis condenser chamber
• Drain the condensate through the media drain valve at the left side of the freeze-dryer by attaching a hose on the nozzle (included in the scope of supply) and placing a vessel underneath.
In order to avoid damage, the condensate must be removed directly after the completion of the defrosting process. Then, any residual water must be removed from the ice condenser chamber by way of a cloth.
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Dangerous voltage
I
On (Power)
Hot surface
0
Off (Power)
Caution! Risk of bruising
Name plate (see chapter
2.1.2 - "Name plate")
Attention, consult the operating manual
CE mark in compliance with the directive 2006/42/EC
Protective earth (ground)
Unplug the mains plug
Earth (ground)
China RoHS 2 mark (only for China)
NOTE
Safety indications on the freeze-dryer must be kept readable at all times. If necessary, they must be replaced.
NOTE
Not all of the symbols/labels are used for this type of freeze-dryer.
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3 Safety
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3.1 Marking of the unit
The following symbols are used for CHRIST freeze-dryers:
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DANGER
This symbol stands for a direct hazard to the life and health of persons.
Non-observance of these symbols causes serious health problems up to life-endangering injuries.
DANGER
This symbol stands for a direct hazard to the life and health of persons due to electrical voltage.
Non-observance of these symbols causes serious health problems up to life-endangering injuries.
WARNING
This symbol stands for a potential hazard to the life and health of persons.
Non-observance of these symbols can cause serious health problems up to life-endangering injuries.
CAUTION
This symbol indicates a potentially hazardous situation
Non-observance of these notes can cause minor injuries or damage to property.
NOTE
This symbol indicates important information.
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3.2 Explanation of the symbols and notes
This operating manual uses the following names and symbols to indicate hazards:
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3.3 Responsibility of the operator
The operator is obliged to ensure that the persons working with the freeze­dryer
• are 18 years old or older,
• have been specifically ordered to operate the unit and made aware of
dangers originating from the freeze-dryer, supply media, starting and end products by the operator,
• are familiar with the fundamental regulations concerning workplace safety and accident prevention
• have read and understood this operating manual (and in particular the safety sections and warning notes) and confirmed this with their signature.
The areas of responsibility of the personnel concerning the operation, maintenance, and care of the unit must be clearly defined.
The safety-conscious work of the personnel in compliance with the operating manual and the relevant EC and national health and safety regulations as well as with the accident prevention regulations must be checked at regular intervals (e.g. every month).
The operator is responsible for performing a risk assessment in terms of disasters (e. g. fire) in the working area and, if necessary, for taking constructional measures.
The operator is responsible to check the chemical compatibility of all substances to be used inside the freeze-dryer (product to be processed, cleaning media, etc.) with the material of the chamber walls, shelves, pipes, and gaskets. Substances that may damage the material an degrade the mechanical strength must not be used.
The freeze-dryer has to be maintained regularly (see chapter 8 ­"Maintenance and service").
Components that are not in a perfect state must be replaced immediately.
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3.4 Operating personnel
It must be ensured that persons operating the unit
• are 18 years old or older,
• have been specifically ordered to operate the unit and made aware of
• be familiar with the fundamental regulations concerning workplace
• have read and understood this operating manual (and in particular the
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dangers originating from the freeze-dryer, supply media, starting and end products by the operator,
safety and accident prevention
safety sections and warning notes) and confirmed this with their signature.
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WARNING
• Ensure that the freeze-dryer was set up and connected properly (see chapter 5 - "Set-up and connection").
• Connections to customer-provided pipes must be force- and torque- free.
• Maintain a safety distance of at least 30 cm (12 inches) around the freeze-dryer.
• Do not store any dangerous goods in the safety area of the freeze- dryer.
• Do not stay in the safety area longer than what is absolutely necessary for the operation of the freeze-dryer.
• Only use accessories that have been approved by the manufacturer (except for commercial vessels made of glass or synthetic materials). We explicitly warn against the use of equipment of poor quality. Breaking glass or bursting vessels can cause dangerous situations.
• Observe the instructions on the installation of accessories (see the separate document).
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3.5 Informal safety instructions
This operating manual is a part of the product.
• The operating manual must be kept at the location of use of the freeze- dryer. Ensure that it is accessible at all times.
• The operating manual must be handed over to any subsequent owner or operator of the freeze-dryer.
• Any changes made must be added to the operating manual.
• In addition to the operating manual, the general and local rules and
regulations concerning the prevention of accidents and the protection of the environment must also be supplied.
• Safety and danger indications on the freeze-dryer must be kept
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readable at all times. If necessary, they must be replaced.
3.6 Safety instructions
The following instructions must be observed prior to every drying process:
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DANGER
• Ensure that the local mains voltage matches the nominal voltage that is stated on the name plate.
• Do not place any dangerous material, e.g. glass vessels containing liquid substances, within the safety area of 30 cm around the freeze­dryer. Spilled liquids may get into the freeze-dryer and damage the electrical or mechanical components.
• Work on the power supply system must only be performed by certified electricians.
• Inspect the electrical equipment of the unit regularly. Defects such as loose or burnt cables must be eliminated immediately.
WARNING
• Do not use the freeze-dryer if it was installed incorrectly.
• Do not use the freeze-dryer without panels.
• Do not use the freeze-dryer with accessories that shows signs of
damage.
• Only use the freeze-dryer with accessories that have been approved by the manufacturer. In case of doubt, contact the manufacturer (see chapter 7.3 - "Service contact").
• Do not hit or move the freeze-dryer during its operation.
• Do not lean against or rest on the freeze-dryer during its operation.
• Check the freeze-dryer and the accessories before every start-up for
any visible signs of damage.
• Do not dry any substances that could damage the material of the ice condenser chamber, drying chamber, lid, or accessories in any way, e.g. highly corrosive substances such as hydrogen chloride (HCl).
• Stop the freeze-dryer immediately in the event of a malfunction. Eliminate the malfunction (see chapter 7 - "Malfunctions and error correction") or contact the after-sales service of Firma Martin Christ Gefriertrocknungsanlagen GmbH (see chapter 7.3 - "Service contact").
• Ensure that all repairs are performed only by authorised and specialised personnel.
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3.6.1 Electrical safety
CHRIST freeze-dryers are units of safety class I. Please comply with the
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following points in order to preserve the safety features:
3.6.2 Mechanical safety
In order to ensure the safe operation of the freeze-dryer, please comply with the following points:
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DANGER
• Always use fuses of the same type and rating.
• Do not dry explosive or inflammable substances.
• Do not use the freeze-dryer within hazardous locations where there is a
risk of explosion.
DANGER
• Wear suitable protective gloves when installing or removing accessories. Do not reach into the ice condenser chamber without this protection – your limbs may freeze onto the chamber walls!
DANGER
• Infectious, toxic, pathogenic, and radioactive substances must be dried in suitable accessories. Take suitable precautions for your own safety!
• Do not dry products with a high solvent concentration or acidic products without special protective measures or device-based precautions (e.g. an additional cooling trap to protect the vacuum pump). It is absolutely necessary to consult the manufacturer in these cases (see chapter 7.3 - "Service contact").
• Special caution is necessary when handling azides, as a dangerous explosive develops in combination with copper or nonferrous metals! It is absolutely necessary to contact the manufacturer (see chapter 7.3 ­"Service contact").
WARNING
• Keep informed about local measures to avoid harmful emissions (depending on the substances to be dried).
• As personal protective equipment, safety gloves are required for the use of the freeze-dryer. The materials to be dried may, however, require additional special safety measures (e.g. drying of infectious, toxic, radioactive, or pathogenic substances)
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3.6.3 Fire prevention
Fuses protect certain electrical circuits within the freeze-dryer against over-
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current conditions.
3.6.4 Thermal safety
During the operation of the freeze-dryer, the ice condenser can reach
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surface temperatures of –85°C depending on the power.
3.6.5 Chemical and biological safety
If infectious, toxic, pathogenic, or radioactive substances are intended to be dried, it is in the responsibility of the user to ensure that all necessary safety regulations, guidelines, precautions, and practices are adhered to accordingly.
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3.7 Safety devices
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3.7.1 System check
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3.7.2 Earth conductor check
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An internal system check system monitors the data transfer and sensor signals with regard to plausibility. Errors are detected by continuous self­monitoring of the system. Error messages are displayed in the main window under "Process & equipment messages" ((see chapter 7.2 ­"Process and equipment messages")).
For the earth conductor check, there is an equipotential bonding screw on the rear panel of the freeze-dryer. An earth conductor check can be carried out with the aid of a suitable measuring instrument.
3.8 Procedures in the event of hazards and accidents
Hazardous electrical incident:
• Set the control switch to the "0" position in order to interrupt the power supply completely.
Fire:
• A fire in the electrical control system must be extinguished with a CO2 fire extinguisher!
• Burning oil must be extinguished with a CO2 fire extinguisher or powder fire extinguisher!
Electric shock:
• While ensuring your own safety, interrupt the circuit as quickly as possible (control switch). Keep the affected persons warm and calm. Get medical attention immediately! Check consciousness and breathing continuously. In the case of unconsciousness of lack of normal breathing, perform cardiopulmonary resuscitation (CPR).
Burns:
• Cool small-area burns (e.g. finger) immediately with cold water for approximately 2 minutes.
• Do not cool if larger areas of the body surface are burnt since there is a risk of hypothermia.
• Cover the burns loosely and in a sterile manner (e.g. with sterile dressing).
• Keep the affected persons warm and calm.
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IF IN DOUBT, CALL THE EMERGENCY PHYSICIAN (AMBULANCE)!
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3.9 Remaining hazards
All CHRIST freeze-dryers were built state-of-the-art and according to the accepted safety rules. Danger to life and limb of the operator, or of third parties, or impairments of the units or other material assets, however, cannot be completely excluded when the units are being used.
Use the freeze-dryer
• only for the purpose that it was originally intended for (see chapter 1.2 - "Intended use") and
• only if it is in a perfect running state.
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• Immediately eliminate any problems that can affect safety.
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Alpha 1-4 LDplus
Alpha 2-4 LDplus
Height:
415 mm
415 mm
Width:
390 mm
390 mm
Depth:
520 mm + 80 mm vacuum connection
520 mm + 80 mm vacuum connection
Weight:
approx. 42 kg
approx. 55 kg
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4 Storage and transport
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4.1 Dimensions and weight
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4.2 Storage conditions
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Values for the freeze-dryer without a vacuum pump:
In order to ensure the protection against mechanical and climatic influences, the guidelines of the German Federal Association for Wooden Packages, Pallets, and Export Packaging (Bundesverband Holzpackmittel, Paletten, Exportverpackung e.V.), the so-called HPE packaging guidelines, must be applied when packing and storing the freeze-dryer.
The storage must be:
• dust-free
• dry
• free from excessive temperature fluctuations
• free from a mechanical load.
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correct
incorrect
CAUTION
The freeze-dryer Alpha 1-4 LDplus weighs approx. 42 kg! The freeze-dryer Alpha 2-4 LDplus weighs approx. 55 kg!
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4.3 Notes on transport
• Use suitable packaging for the transport, and if at all possible, the original packaging.
• Install all transport safety devices (see chapter 4.5 - "Transport safety device").
• Over short distances, the freeze-dryer can be transported by a suitable number of persons who reach under it from the sides.
• When lifting the freeze dryer, always reach under the freeze-dryer from the side. Do not grab the unit at the plastic control panel (see figures below).
Fig. 12: Lifting the freeze-dryer
• When setting the unit down, ensure that the feet are upright (see figures
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below).
Fig. 13: Unit feet
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CAUTION
The freeze-dryer Alpha 1-4 LDplus weighs approx. 42 kg! The freeze-dryer Alpha 2-4 LDplus weighs approx. 55 kg!
NOTE
Prior to any transport, the vacuum sensor must be deinstalled.
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4.4 Packaging
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The freeze-dryer is packaged in a cardboard box or in a wooden crate, depending on the scope of supply.
• After opening the packaging, take out the box containing the accessories.
• Remove the packaging material.
• Lift the freeze-dryer upwards and out of the crate/cardboard box. When
lifting the unit, always reach under the freeze-dryer from the side.
• Retain the packaging for any possible future transport of the freeze- dryer.
4.5 Transport safety device
Prior to start-up, the vacuum sensor must be installed (see chapter 5.4 ­"Vacuum sensor").
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NOTE
Refrigeration problems of the freeze-dryer are often caused by insufficient conditions at the location of use. This is why compliance with the following conditions is absolutely mandatory!
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5 Set-up and connection
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5.1 Installation site
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Operate the freeze-dryer only in closed and dry rooms.
• The table must be stable and have a solid, even tabletop.
• Ensure sufficient ventilation. Do not place any paper, cloth, or similar
material behind or under the unit, since otherwise the air circulation will be impaired.
• Keep a safety distance of at least 30 cm around the freeze-dryer so that the vents in the unit remain fully effective.
• The ambient temperature must be in the range of +10°C to +25°C. A potential night-time setback of the air conditioning system must be taken into consideration.
• Prevent the room temperature from rising, for example due to closed doors at night.
• Do not subject the freeze-dryer to thermal stress, e.g. by positioning it near heat generators.
• Prevent thermal overload, e.g. caused by other equipment in the direct vicinity of the freeze-dryer.
• Do not set up the vacuum pump directly next to the heat exchanger (condenser).
• In the case of water-cooled systems, ensure that the water circuit provides a sufficient amount of cooling water.
• Avoid direct sunlight (UV radiation).
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DANGER
The operating voltage on the name plate must correspond to the local supply voltage
NOTE
The ice condenser chamber can be flooded with nitrogen via the hose nozzle of the aeration valve.
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5.2 Power supply
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5.2.1 Connection
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CHRIST freeze-dryers are units of safety class I. Alpha 1-4 LDplus and Alpha 2-4 LDplus units have a three-wire power cord with a fixed cable(see chapter 10 - "Technical data"). An equipotential bonding screw is located on the back below the mains
power input (see chapter 2.1.1 - "Functional and operating elements"). This equipotential bonding screw can be used to perform an earth conductor check.
5.2.2 Customer-provided fuses
Typically, the freeze-dryer must be protected with 16 Amp G fuses that are
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to be provided by the customer.
5.3 Aeration and media drain valve
The aeration and media drain valve is located on the left side of the unit (see chapter 2.1.1 - "Functional and operating elements").
After the end of a freeze-drying process, the unit will be aerated via the aeration valve.
Additionally, it is used to drain off the condensate and the defrosting water.
• Connect the drain hose (included in the scope of supply) to the hose connector.
• Place a collecting vessel under the unit.
The hose must be laid with a continuous slope and the end of the hose must always be above the liquid level in the collecting vessel. This prevents water and dirt residues from being sucked into the ice condenser chamber if there is negative pressure when the media drain valve is opened.
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NOTE
Please refer to the separate operating manual of the vacuum sensor!
1 Vacuum sensor 2 Clamping rings 3 Connection socket
NOTE
It is absolutely essential to comply with the manufacturer’s instructions in
the separate operating manual of the vacuum sensor!
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5.4 Vacuum sensor
In order to protect the vacuum sensor against transport damage, it comes supplied in its original packaging. Prior to commissioning the freeze-dryer, the sensor must be installed.
Fig. 14: Position of the vacuum sensor and the connection socket
• Switch the unit off by actuating the mains power switch.
• Take the vacuum sensor out of its original packaging and fasten it to the
connector with a bow-shaped connecting piece, two clamping rings (DIN16KF) and two centring rings (included in the scope of supply).
• Plug the connector to the connection socket and hand-tighten the screws on the connector.
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Thyracont VCP63
MKS 722B
NOTE
The vacuum sensor comes supplied in a calibrated state.
Fig. 15: Installed vacuum sensors of different manufacturers
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After the freeze-dryer has been switched on, the vacuum sensor needs several minutes until it is ready for operation.
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NOTE
It is absolutely essential to refer to the separate instruction manual of the vacuum pump and exhaust filter (if applicable)!
NOTE
The vacuum pump is supplied with power by the unit, but the maximum current for the vacuum pump is limited. It is absolutely essential to refer to the label of the electrical outlet for the vacuum pump (see the following picture)!
If the current requirement of the vacuum pump is higher than the value that is stated on the label, the pump must be supplied separately via an on-site power socket.
1 Label indicating the
maximum current
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5.4.6 Vakuumpumpe
5.5 Vacuum pump
The vacuum pump must be connected to the vacuum connection of the unit and to the electrical socket at the back of the unit, which is marked accordingly (see chapter 2.1.1 - "Functional and operating elements").
Fig. 16: Indication of the maximum current for the vacuum pump (example)
The oil mist that escapes from the pump during operation must be retained or discharged via an exhaust filter (oil mist separator).
• We strongly recommend using an oil mist separator. The filter prevents the contamination of the air with oil mist.
• For discharging the oil mist, connect a suitable hose (RZ-2.5 and RC-6: ½", DUO 5 or DUO 10 ¾") to the exhaust connector of the vacuum pump.
• The hose line must be laid in such a manner that any condensation water cannot flow back into the pump. In the case of a rising hose line,
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we recommend using a condensate trap (Woulff bottle or wash bottle).
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CAUTION
Observe the installation direction of the pressure control valve!
1Pressure control valve 2 Vacuum pump
connection
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5.6 Pressure control valve
The pressure control valve is integrated in the suction pipe between the vacuum pump and ice condenser chamber. During certain, specified process phases, it interrupts the volume flow to the vacuum pump (see chapter 2.2.1 - "General information on freeze-drying").
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Fig. 17: Installation of the pressure control valve
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1Locking handle 2Aeration connection 3Vessel connection 4Rubber plug 5Connection to freeze-
dryer (e.g. via a manifold)
NOTE
The rubber valves come supplied in an ungreased state. This is why a thin layer of vacuum grease must be applied to the connector of the freeze­dryer as well as to the vessel connector prior to start-up in order to ensure trouble-free operation.
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5.7 Rubber valves
The rubber valves (part no. 121860) enable the connection of round-bottom flasks, wide-neck filter bottles, or distributors for ampoules to a manifold or drying chamber. Depending on the connector of the components, the blue plug can be removed.
Fig. 18: Rubber valve
In position A (see figure below), the aeration connector is open and the vessel connector is closed. The accessory will be aerated while the vacuum inside the drying chamber is maintained. As a result, vessels can be exchanged without any interruption of the drying process.
In position B, the aeration connector is closed and the vessel connector is open. The connected accessory is connected to the freeze-dryer.
In position C, the aeration connector and the vessel connector are closed.
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Fig. 19: Possible positions of the locking handle
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WARNING
Before the initial start-up, please ensure that your freeze-dryer is properly set up and installed (see chapter 5 - "Set-up and connection")
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6 Operation
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6.1 Initial start-up
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6.2 Installation of accessories
The accessories must be completed in accordance with the drying method that is applied as well as in accordance with the scope of supply.
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Please contact our sales department if you have any queries.
6.3 Preparation
The ice condenser chamber must be clean and dry.
• Remove any water residues from the preceding run.
• Close the media drain valve and the aeration valve.
• Ensure that all of the valves of the accessories are closed.
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• Switch the vacuum pump on.
6.4 Switching the freeze-dryer on
• Actuate the mains switch.
The control unit performs a self-test and an initialisation. This may take several seconds.
• Follow the safety instructions and hazard warnings (see chapter 3 -
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"Safety")!
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1 Left function key 2 Right function key 3 "Up" key 4 "Down" key 5 Display
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6.5 LDplus control system
The control system LDplus ("Lyo Display plus") was specifically developed for the control of freeze-drying processes. The clear user interface enables the intuitive operation of the unit.
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6.5.1 User interface
Fig. 20: Start screen of the LDplus control system
Fig. 21: User interface of the LDplus control system
Function keys (1+2)
Function keys are keys whose function depends on the menu and operating state of the unit. The current function is displayed directly next to the key in the field with a black background.
Fig. 22: Indication of the current functions of the function keys; here, on the left, the "mode" function and on the right the "menu" function.
"Up" and "down" keys (3+4)
These keys are used to select the functions and values that are available in the menu or to change the selected parameters.
In addition, these keys also control the indication of the measurement value channels in the value windows. The "up" key is assigned to the left value window, whereas the "down" key controls the right value window.
• For a selection, press the "up" or "down" key repeatedly until the desired measurement value channel is indicated in the respective value window.
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6 Value window 7 Current function of the
function keys
8 Status line
9 Measurement value
channel
10 Set value (only in the
run mode)
11 Unit of the
measurement value
12 Actual value
Display (5)
The main window of the display is divided into the value windows, an area indicating the current function of the function keys, and a status line. The main window displays all of the relevant process data, such as set and actual values, menus, and process information (see the illustration).
Fig. 23: Layout of the LDplus control system display
Value windows (6) The value windows are displayed after the initialisation of the control
system. There are two value windows with an identical layout. The indication of the measurement value channels is controlled by way of the "up" and "down" keys (see above).
Fig. 24: Value windows
The available measurement values can be displayed in the left as well as in the right value window so that a combination of the following values can be selected:
• Total time (indicates the total runtime of the process)
• Section time (indicates the runtime of an individual phase, e.g. freezing,
warm-up of the vacuum pump, or main drying)
• Ice condenser temperature
• Vacuum in mbar (indicates the vacuum in the drying chamber; only
possible if a vacuum sensor is installed)
• Vacuum converted into °C (indicates the vacuum inside the drying chamber, converted based on the vapour pressure curve for ice and water, see chapter 2.2.1 - "General information on freeze-drying"; only possible if a vacuum sensor is installed)
Current function of the function keys (7) See function keys (1+2)
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13 Symbol of the
operating state 14 Active phase 15 Symbol of pending
information
The freeze-dryer is in the standby mode. All of the various units are switched off.
The freeze-dryer is in the run mode. The unit performs a continuous run.
The freeze-dryer is in the run mode. The timer is activated.
Freezing
The ice condenser is cooled.
Warm-up VP
The ice condenser is cooled and the vacuum pump is activated while the pressure control valve is closed. If no pressure control valve is integrated, the drying chamber must be separated from the vacuum pump by way of a manual valve or similar.
Main drying
The drying chamber is evacuated while the ice condenser is cooled. If a vacuum control system is included, the vacuum is controlled based on the corresponding set value for the main drying phase.
Final drying
The final drying phase is only available if a vacuum control system is included. It is possible to define different control parameters (set vacuum, timer) for the main drying and final drying phases.
The symbol flashes every second if there is pending information concerning the process or the freeze-dryer (error messages, process messages, or general information).
The information can be viewed under "Process & equipment info" (see chapter 6.5.3.3 - "Process and equipment information")
Status line (8) The status line at the bottom of the screen indicates the current operating
state, active phase, and any pending information. The status line is visible at all times.
Fig. 25: Status line
Operating state (13)
Active phases (14)
Pending information (15)
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6.5.2 Mode
The mode can be called up with the left function key if a value window is active. The individual phases can be selected as follows:
• Press the left function key "mode". The menu "Start with phase..." will be displayed (see the illustration).
• Select the desired menu item by way of the up/down keys.
• Confirm with the right function key "enter".
Fig. 26: Selecting a mode
Starting the freeze-drying process
The freeze-drying process comprises four phases:
• Freezing
• Warm-up vacuum pump
• Main drying
• Final drying
If "main drying" or "final drying" is selected, the system enquires as to whether the vacuum pump shall warm up beforehand.
Changing the phase
The freeze-dryer is in the run mode. In order to switch over to the next phase or to stop the process by way of "standby":
• Press the left function key "mode". The menu "Select mode" will be displayed (see the illustration).
Fig. 27: Selecting a mode
• Select the menu item "Continue with phase..." by way of the up/down
• Select the desired phase by way of the up/down keys and confirm the
Fig. 28: Continuing the freeze-drying process
keys and confirm the selection with the right function key "enter".
selection with the right function key "enter".
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Warm-up vacuum pump
Prior to a freeze-drying process, the vacuum pump usually needs to warm up in order to reach its operating temperature.
For this purpose, the warm-up phase can be started. The desired duration can be preselected (see chapter 6.5.3.4 - "Options").
The following processes take place during the warm-up phase.
• The ice condenser is cooled.
• The vacuum pump is activated while the pressure control valve is
closed. If no pressure control valve is integrated, the drying chamber must be separated from the vacuum pump by way of a manual valve or similar.
After the preset warm-up time, the following information will be displayed:
Fig. 29: Message at the end of the warm-up phase
• Confirm the message and continue the process with the desired phase.
Aborting the warm-up phase During the warm-up phase, the functions "Continue with phase" or
"Standby" can be selected by way of the left function key "mode".
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Selecting one of these functions will abort the warm-up phase.
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1 Menu bar 2 Menu title 3 Selection frame 4 Scroll bar 5 Function key "exit
menu"
6 Function key "open
menu item"
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6.5.3 Main menu
The main menu can be selected from the main window by way of the right function key "menu". It includes the following submenus:
• Change set values (see chapter 6.5.3.1 - "Changing set values")
• Special functions (see chapter 6.5.3.2 - "Special functions")
• Process & equipment info (see chapter 6.5.3.3 - "Process and
equipment information")
• Options (see chapter 6.5.3.4 - "Options")
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6.5.3.1 Changing set values
• Tutorial (see chapter 6.5.3.5 - "Tutorial")
Fig. 30: Layout of the main menu
• Select the "Change set values" function in the main menu.
Fig. 31: Menu "Change set values"
• Select the set value by way of the up/down keys. The selected value will be displayed in a selection frame.
Fig. 32: Manual mode – set value selection
• Confirm with the right function key "edit". The selected value will be displayed in inverted form.
Fig. 33: Inverted indication of the selected set value
• Change the set value by way of the up/down keys.
• Confirm with the right function key "ok".
The modification of the set value is now complete.
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NOTE
It is possible to specify an automatic phase change from "Freezing" to "Warm-up vacuum pump" (seechapter 6.5.3.4 - "Options" / Settings / Automatic phase change).
NOTE
The set values for the "Final Drying" phase are only available if the optional pressure control system is installed.
NOTE
It is possible to specify an automatic phase change from "Main drying" to "Final drying" (seechapter 6.5.3.4 - "Options" / Settings / Automatic phase change).
NOTE
For this set value, the optional vacuum control system must be installed.
Set values for the "freezing" phase
Timer The timer is used to define the duration of the phase. Settings between one
minute and 200 hours are possible. If, when starting at 00:00 h:m, the "down" key is pressed, the symbol will appear. It indicates that the timer is deactivated and that the freeze-dryer is in the continuous mode.
After the preselected time has elapsed, the system enquires as to whether the next phase is to be started.
Set values for the phases "Main drying" and "Final drying"
Timer The timer is used to define the duration of the phase. Settings between one
minute and 200 hours are possible. If, when starting at 00:00 h:m, the "down" key is pressed, the symbol will appear. It indicates that the timer is deactivated and that the freeze-dryer is in the continuous mode.
Vacuum
The range of possible values goes from 6.1 mbar to 0.0010 mbar, converted into steps of 1°C in accordance with the vapour pressure curve for ice and water (see chapter 2.2.1 - "General information on freeze-
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drying").
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NOTE
During the defrosting process, the chamber should not be covered in order to prevent the deactivation of the system due to overheating.
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6.5.3.2 Special functions
The freeze-dryer is equipped with one or several optional accessories. The components can be controlled by way of this function.
• Select the "Special functions" function in the main menu.
• Select the option by way of the up/down keys. The selected value will
be displayed in a selection frame.
Fig. 34: "Special functions" menu
• Confirm with the right function key "enter". The possible functions will be displayed.
• If an option is selected that is not installed, a corresponding message will be displayed:
Fig. 35: Message if an option is not available
Defrosting the ice condenser
As standard, the freeze-dryer is equipped with a defrosting system. The ice condenser chamber is supplied with heat that melts the ice off the ice condenser.
The freeze-dryer must be in the standby mode and completely aerated.
• The defrosting time and temperature can be set in the main menu under "Options" (see chapter 6.5.3.4 - "Options").
• Select the function "Defrosting ice condenser" under "Special functions" in the main menu (see above).
• Start the defrosting process by way of the right function key "start".
The progress of the defrosting process will be displayed in a dialogue box.
Fig. 36: Progress bar of the defrosting process
When the specified defrosting time has elapsed, the defrosting process will be stopped. The dialogue box disappears automatically.
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NOTE
The drying chamber cannot be moved in the "Main drying" and "Final drying" phases.
1 Message 2 Status of the
information
3 Number of active
messages
4 Function key "exit
menu"
5 Function key
"acknowledge message"
NOTE
The error messages are listed in detail under chapter 7 - "Malfunctions and error correction".
Option: Electrical lifting hoist
The freeze-dryer can be retrofitted with an electrical lifting hoist that facilitates the attachment and removal of drying chambers.
The freeze-dryer must be in the standby mode and completely aerated.
• Select the function "Lifting hoist" under "Special functions" in the main menu (see above).
• Move the drying chamber by way of the up/down keys.
Fig. 37: Operation of the electrical lifting hoist
• After the completion of the process, exit the menu via the left function
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key "back".
6.5.3.3 Process and equipment information
The menu "Process & equipment info" provides the user with information concerning error, process, and system messages.
In the event of a message, a sound signal will be issued, the symbol " " will appear on the status line, and the process and equipment information window will be displayed. If the user is currently in a menu, the window will not be displayed until the user exits the main menu.
Fig. 38: Structure of the "Process & equipment info" menu
Regardless of the presence of a message, the menu can be activated at all times in order to view any messages that are present.
• Select the "Process & equipment info" function in the main menu.
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Information present, not acknowledged
Information present, acknowledged
Cause of the message no longer present, information not acknowledged
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6.5.3.4 Options
Status of the information
All of the information that is displayed receives a certain status:
The sound signal is issued until all of the information has been acknowledged.
If the cause of the message is no longer present and if the information has been acknowledged it will be removed from the process and equipment information window.
The menu cannot be exited by way of the left function key "back" until all of the information has been acknowledged.
The following values can be adjusted in the "Options" menu:
• Display contrast
• Language
• Settings
• Service menu
Fig. 39: "Options" menu
Changing the display contrast
• Select the menu "Change display contrast".
• Adjust the contrast by way of the up/down keys.
• Confirm the entry with the right function key "ok".
Fig. 40: Menu for changing the display contrast
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Selecting a language
The LDplus control system can be used in various language versions.
• Select the menu "Select language".
• Select the desired language by way of the up/down keys.
• Confirm the entry with the right function key "enter".
Fig. 41: Menu for selecting a language
Settings
This menu can be used to adapt the operation and process control of the freeze-dryer's control system to your specific requirements.
• Select the desired menu.
• Change the value by way of the up/down keys.
• Confirm the entry with the right function key "ok".
Fig. 42: "Settings" menu
Warm-up vacuum pump This item is used to adjust the duration of the warm-up phase. Values
between 5 and 60 minutes are possible.
Automatic phase change If the "Change phase automatically" option is selected, the system will
automatically switch over to the next phase after a preset time (see chapter
6.5.3.1 - "Changing set values" / Timer).
Click at button push If this setting is active, a confirmatory sound signal will be issued whenever
a key/button is pressed.
High temperature resolution If this setting is active, temperatures will be displayed in the value window
with a resolution of 1/10°C (instead of 1°C).
Time defrosting Here, the time that is needed for defrosting the ice condenser can be
preselected. Settings between one minute and 200 hours are possible.
Temperature defrosting This value defines the maximum temperature of the ice condenser chamber
or ice condenser during the defrosting process. Values between 10 and 60°C are possible.
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NOTE
• Installed options must be activated with "yes".
• Options that are not installed must be deactivated with "no".
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6.5.3.5 Tutorial
Service menu
Fig. 43: Service menu
LDplus configuration Here, the following accessory components (options) can be configured:
• Vacuum sensor
• Vacuum control system
Load default settings This menu item is used to reset all of the set values and parameters to the
delivery state of the freeze-dryer. The system will issue a corresponding enquiry prior to performing this step.
Extended service menu The extended service menu is reserved for service technicians. This area is
protected by a password and is not accessible to the user.
The tutorial provides information concerning the most important functions of the LDplus control system.
The tutorial is available in German, English, and French.
Fig. 44: Tutorial
• Select the "Tutorial" function in the main menu.
• Browse the tutorial by way of the up/down keys.
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• Click the left function key repeatedly in order to exit the tutorial.
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6.6 Switching the freeze-dryer OFF
The freeze-dryer must be in the standby status.
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• Switch the freeze-dryer off by pressing the mains switch.
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NOTE
The vacuum checks must be carried out when the ice condenser is frozen.
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7 Malfunctions and error correction
Malfunctions are displayed in the dialog box "Process & equipment messages" (see chapter 6.5.3.3 - "Process and equipment information"). An acoustic signal sounds when an error message is generated.
• Eliminate the source of the problem (see the following chapter).
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7.1 General malfunctions
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7.1.1 Power failure
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• Acknowledge the error message.
The control system continues with the process after a power failure. The preselected conditions remain saved even during a process run.
In the event of a power failure in the drying phase, the batch may become unusable. Whether the batch can be saved or not depends on the drying phase in which the product was when the power failure occurred.
• In the final drying phase, the product has reached a residual moisture content of approx. 5%. Below this value, the product is generally not damaged even if the power failure lasts for a longer period of time.
• If the product is in the main drying phase, we recommend aerating the unit, removing the product, and storing it in a deep-freeze. The defrosted condensate must be drained off prior to the next start.
7.1.2 Insufficient vacuum
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7.1.2.1 Small flange connections
Leakages are often due to improper small flange connections between the various components and hose connections or to leakages in the valves.
• Loosen the connection and place the centring ring (with sealing ring inside) in a centred manner between the flange connections.
• Seal the connection with the clamping ring by tightening the wing nut.
• Ensure that the centring ring neither slips out of place nor gets jammed.
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Fig. 45: Small flange and centring ring
Fig. 46: Small flange with centring ring and small flange
Fig. 47: Attaching the clamping ring
Fig. 48: Tightened clamping ring
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7.1.2.2 Aeration and media drain valve
A malfunction of the aeration and media drain valve may have several causes. One potential source are contaminants such as product residues within the valve.
• Switch the freeze-dryer off and disconnect the mains plug.
• Clean the valve (see chapter 8.1.1.2 - "Aeration valve, media drain
valve").
• Put the freeze-dryer into operation again.
If there is still a leakage, the freeze-dryer must be checked by qualified
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specialist personnel (see chapter 7.3 - "Service contact").
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NOTE
The inspection of the valve must be carried out by qualified specialist personnel (see chapter 7.3 - "Service contact").
CAUTION
Ensure sufficient ventilation. Do not place any paper, cloth, or similar material behind or under the unit, since otherwise the air circulation will be impaired.
7.1.2.3 Pressure control valve
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A malfunction of the pressure control valve may have several causes.
7.1.2.4 Rubber valves
In order to identify a leaking rubber valve, the valves must be checked individually:
• Remove the rubber valve and seal the connection at the drying chamber with a rubber stopper.
• Check the tightness under vacuum until the leaking valve has been localised.
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• Clean the valve or replace it if necessary.
7.1.2.5 Vacuum sensor
Vacuum sensors have a limited service life and can be ordered as spare parts (e.g. VCP 63, order no. 312011).
Functional test:
• Connect the vacuum sensor directly to the suction side connector of the vacuum pump.
If a final pressure of at least 0.011 mbar is reached (with a vacuum pump that has reached its operating temperature), the sensor and the vacuum
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pump are OK.
7.1.3 Insufficient ice condenser temperature
The refrigeration unit is equipped with a protective device against overpressure in the refrigeration system and with a thermal motor protection switch.
The protective devices trip
• when the ambient temperature is too high
• when the air circulation of the heat exchanger of the refrigeration
system is insufficient
• when the refrigeration system is overloaded.
In these cases, the refrigeration unit will be switched off automatically. If the permissible operating conditions are re-established after a cool-down
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Error message
Possible cause
Remedy
Vacuum 6.11 mbar not reached
The value of 6.11 mbar is not reached within 15 minutes with an open pressure control valve. The pressure control valve will be closed and the vacuum pump will be switched off.
• The aeration and media drain valves are soiled.
• The small flange connections are not properly connected.
• A seal is soiled or damaged.
• The cover or drying chamber is
not properly attached.
• The ground-in stopper is not inserted correctly or it is missing.
• The vacuum pump is switched off or defective.
• Clean the valve (see chapter
8.1.1.2 - "Aeration valve, media drain valve") and replace it if necessary.
• Loosen the connection. Place the centring ring with the inner sealing ring in a centred manner between the flange connections and connect it with the clamping ring. Ensure that the centring ring neither slips out of place nor gets jammed.
• Clean the seal and replace it if necessary.
• Check the cover and drying chamber.
• Grease the ground-in stopper evenly and over the entire sealing surface with vacuum grease and install it.
• Switch the vacuum pump on. Refer to the separate instruction manual of the vacuum pump.
Defective vacuum sensor
The control system registers an invalid measurement value.
• The vacuum sensor is not connected correctly.
• The calibration is faulty.
• The vacuum sensor is soiled
(e.g. due to water residues).
• The vacuum sensor is defective.
• Check the vacuum sensor connectors.
• Calibrate the vacuum sensor (see the separate operating instructions of the vacuum sensor).
• Clean the vacuum sensor.
• Check the vacuum display with
the aid of a reference device (if available).
• See chapter 7.1.2.5 - "Vacuum sensor".
Overpressure of refrigeration unit 1
• The overpressure switch of the refrigeration unit has tripped.
• Let the freeze-dryer cool down.
• Ensure sufficient air circulation
(see chapter 7.1.3 - "Insufficient ice condenser temperature").
phase of several minutes, the refrigeration unit will be switched on again automatically.
The malfunctions are displayed in the process and equipment information window.
The minimum ice condenser temperature of approx. -55°C or approx. – 85°C (depending on the type of freeze-dryer) is reached when the ice condenser is not loaded and the ice condenser chamber is evacuated.
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7.2 Process and equipment messages
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Error message
Possible cause
Remedy
Overpressure of refrigeration unit 2
• The overpressure switch of the refrigeration unit has tripped.
• Let the freeze-dryer cool down.
• Ensure sufficient air circulation
(see chapter 7.1.3 - "Insufficient ice condenser temperature").
Ice condenser overtemperature
Ice condenser temperature > +65°C. All of the units will be switched off and the freeze-dryer will be automatically set to standby.
• The defrosting process has been performed with the cover closed.
• Remove the cover and let the freeze-dryer cool down.
Ice condenser temperature > 20°C
The ice condenser temperature rises to a non-permissible value during the freeze-drying process. The pressure control valve will close automatically in order to prevent the vacuum pump from being damaged.
• Insufficient cooling.
• Observe the behaviour of the
refrigeration system. If necessary, inform the service department (see chapter 7.3 ­"Service contact").
Defective ice condenser temperature sensor
• The temperature sensor is not connected or it is defective.
• Inform the service department (see chapter 7.3 - "Service contact").
Defective temperature sensor of the defrosting heater
• The temperature sensor is not connected or it is defective.
• Inform the service department (see chapter 7.3 - "Service contact").
Mains power failure (see chapter 7.1.1
- "Power failure")
• The power supply has been interrupted.
• The mains power connector is not connected.
• The fuses have tripped.
• The mains power switch has
been switched off.
• Check the mains fuse.
• Connect the mains power
connector firmly.
• Check the customer-provided fuses.
• Switch the mains power switch on.
Default settings loaded
All of the settings have been reset to the delivery state of the freeze-dryer.
• Error in the parameter memory.
• Manual execution in the service
menu.
• No measure required.
IO communication error (0x20)
• Error in the LDplus IO module.
• Inform the service department
(see chapter 7.3 - "Service contact").
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NOTE
If you would like to utilise our after-sales-service, please state the type of your freeze-dryer and its serial number.
7.3 Service contact
In the event of queries, malfunctions, or spare part enquiries:
From Germany:
Contact Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50 37520 Osterode (Germany) Tel. +49 (0) 55 22 / 50 07-44 44 E-mail: [email protected]
Outside Germany:
Contact our agency in your country. All agencies are listed at www.martinchrist.de [Sales Partners]
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CAUTION
If corrosion or other damage occurs due to improper care, the manufacturer cannot be held liable or subject to any warranty claims.
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8 Maintenance and service
The freeze-dryer and the accessories are subject to high mechanical stress. Thorough maintenance performed by the user extends the service
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life and prevents premature failure.
• Use soap water or other water-soluble, mild cleaning agents for cleaning the freeze-dryer and the accessories.
• Do not use corrosive and aggressive substances.
• Do not use solvents.
• Do not use agents with abrasive particles.
• Do not expose the freeze-dryer or its accessories to intensive UV
radiation (e.g. sunlight) or thermal stress (e.g. by heat generators).
• Do not turn the unit upside down in order to clean it.
8.1 Maintenance
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8.1.1 General
The general state of the freeze-dryer must be checked at regular intervals. Any defects must be eliminated immediately! The following points are of particular importance:
• dirt
• leaks
• corrosion
• bent system components
• loose screw and flange connections
• higher noise levels
• loose cables
• open cable ducts
• missing or illegible safety notes and hazard warnings
• missing or illegible inscriptions on components, pipes (direction of flow)
and cables
• etc.
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1Valve opening 2Valve core 3O-rings
Cleaning of the freeze-dryer
• Switch the freeze-dryer off by actuating the mains power switch and disconnect the power cord from the wall outlet before cleaning.
• If the freeze-dryer has been contaminated with toxic, radioactive, or pathogenic substances, clean the inside immediately with a suitable decontamination agent (depending on the type of contamination, see chapter 8.2 - "Disinfection of the drying chamber and accessories").
• Remove product residues thoroughly with a cloth.
• Open the lid/drying chamber when the freeze-dryer is not in use so
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8.1.1.1 Ice condenser chamber
moisture can evaporate.
Before each start-up, ensure that the ice condenser chamber is free from water residues.
• Open the media drain valve to drain off any liquid. Then, close the valve.
• If necessary, wipe the ice condenser chamber dry with a cloth.
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8.1.1.2 Aeration valve, media drain valve
Contaminants such as product residues may lead to an insufficient vacuum. In this case, the aeration valve and the media drain valve must be cleaned.
• Switch the freeze-dryer off and disconnect the mains plug.
• Remove the valve core.
• Clean the valve core and the opening with a moist cloth.
• Clean the O-rings and inspect them for any damage. Damaged O-rings
must be replaced.
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Fig. 49: Valve opening and valve core with O-rings (example, varies depending of the type of freeze-dryer)
• Reinsert the valve core.
• Put the freeze-dryer into operation again.
If the vacuum is still insufficient, the freeze-dryer must be checked by qualified specialist personnel (see chapter 7.3 - "Service contact").
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NOTE
Please refer to the separate operating manual of the vacuum pump!
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8.1.1.3 Heat exchanger (only for air-cooled freeze-dryers)
A lamellar heat exchanger is used for cooling the refrigerant that is compressed by the refrigeration unit. This air-cooled heat exchanger is located at the back of the unit (see chapter 2.1.1 - "Functional and operating elements").
Dust and dirt impair the cooling effect of the air flow. Dust on the lamellas prevents the exchange of heat and, thereby, impairs the performance and power of the refrigeration unit. Strong soiling may cause the unit to fail.
This is why the selected set-up location should be as clean as possible.
• Check the heat exchanger at least once per month for soiling and clean it if necessary.
• Please contact the Christ service department if you have any queries
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8.1.2 Vacuum pump
(see chapter 7.3 - "Service contact").
The stress of the vacuum pump in conjunction with a freeze-dryer is usually not very high. This is why the recommendations in this operating manual may differ from the information that is provided by the pump manufacturers.
Under normal operating conditions, the following maintenance tasks concerning the vacuum pump must be performed at regular intervals:
• Check the oil level of the vacuum pump once per week. If necessary, top it up with oil.
• Check the running pump for any unusual noise.
• Ensure that the pump has reached its operating temperature prior to
changing the oil.
• Perform the first oil change after approximately 100 operating hours.
• The other oil changes depend on the operating conditions. In general,
an interval of 500 to 1,000 operating hours is sufficient.
• Please contact the Christ service department if you have any queries
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(see chapter 7.3 - "Service contact").
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NOTE
Please refer to the separate operating manual of the vacuum pump and the exhaust filter!
NOTE
Please refer to the separate operating manual of the vacuum sensor!
CAUTION
For the care of the accessories, special safety measures must be considered as these are measures that will ensure operational safety at the same time.
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8.1.3 Exhaust filter (oil mist separator)
The oil mist that is emitted by the vacuum pump in quantities that depend on the working pressure must be led to the outside or to an exhaust hood or similar. If this is not possible, the pump must be equipped with an exhaust filter (oil mist separator).
• Observe the liquid level in the collecting vessel of the filter.
• Remove the condensate in time (please refer to the information
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8.1.4 Vacuum sensor
provided by the manufacturer in the separate operating manual).
The vacuum sensor has only a limited service life. Especially carbon­containing substances, e.g. alcoholic compounds, reduce the service life extremely.
• The vacuum sensor is maintenance-free.
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8.1.5 Accessories
• Remove any soiling on the outside with a cloth.
Chemical reactions as well as stress-corrosion (combination of oscillating pressure and chemical reaction) can affect or destroy the metal and plastic parts. Barely detectable cracks on the surface can expand and weaken the material without any visible signs.
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DANGER
If dangerous materials (e.g. infectious and pathogenic substances) are used, the freeze-dryer and accessories must be disinfected.
• Check the material regularly (at least once a month) for – cracks – visible damage of the surface – pressure marks – signs of corrosion – other changes.
• Replace any damaged components immediately for your own safety.
• Immediately rinse off the accessories if any liquids that may cause
corrosion come into contact with them.
• Clean the accessories outside the freeze-dryer once a week or
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preferably after each use.
8.2 Disinfection of the drying chamber and accessories
• Use commercially-available disinfectants such as, for example, Incidur, Meliseptol, Sagrotan, Buraton, or Terralin (available at specialised trade).
• The freeze-dryers and the accessories consist of various materials. A possible incompatibility must be considered.
• Before using cleaning or decontamination agents that were not recommended by us, contact the manufacturer to ensure that such a procedure will not damage the freeze-dryer.
• Please contact us if you have any queries (see chapter 7.3 - "Service contact").
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DANGER
In the event of service work that requires the removal of the panels, there is a risk of electric shock or mechanical injury. Only qualified specialist personnel is authorised to perform this service work.
NOTE
If you would like to utilise our after-sales-service, please state the type of your freeze-dryer and its serial number.
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8.3 Service
The freeze-dryer is subject to high mechanical stress. In order to be able to withstand this high level of stress, high-quality components were used during the production of the freeze-dryer. Nevertheless, wear cannot be excluded and it may not be visible from the outside.
This is why we recommend having the freeze-dryer checked by the manufacturer during an inspection once per year.
Information and appointments:
From Germany:
Contact Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50 37520 Osterode (Germany) Tel. +49 (0) 55 22 / 50 07-44 44 E-mail: [email protected]
Outside Germany:
Contact our agency in your country. All agencies are listed at www.martinchrist.de [Contacts] [Foreign agencies]
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8.4 Return of defective parts
Although we exercise great care during the production of our products, it may be necessary to return a unit or accessory to the manufacturer.
In order to ensure the quick and economical processing of returns of freeze-dryers, rotational vacuum concentrators, spare parts, or accessories, we require complete and extensive information concerning the process. Please fill in the following forms completely, sign them, enclose them with the return package, and send them together with the product to:
Martin Christ Gefriertrocknungsanlagen GmbH An der Unteren Söse 50 37520 Osterode (Germany)
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NOTE
We will return the part/unit if no declaration of decontamination is provided!
NOTE
The part/unit must be packaged in a transport-safe manner. Please use the original packaging for the unit, if at all possible.
If the product is dispatched to us in unsuitable packaging, you will be charged the cost for returning it to you in new packaging.
1.Declaration of decontamination As a certified company and due to the legal regulations for the protection of our employees and of the environment, we are obliged to certify the harmlessness of all incoming goods. For this purpose, we require a declaration of decontamination.
• The form must be filled in completely and signed by authorised and specialised personnel only.
• Affix the original form in a clearly visible manner to the outside of the packaging.
2. Form for the return of defective parts
This form is for the product-related data. They facilitate the assignment, and they enable the quick processing of the return. If several parts are returned together in one packaging, please enclose a separate problem description for every defective part.
• A detailed problem description is necessary in order to perform the repair quickly and economically.
• Upon request, we will prepare and submit to you a cost estimate prior to performing the repair. Please confirm such cost estimate within 14 days. If the cost estimate has still not been confirmed after 4 weeks, we will return the defective part/unit. Please note that you must bear the incurred costs.
The forms can be downloaded online from
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www.martinchrist.de [Service] [Overhaul and repair].
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9 Disposal
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9.1 Disposal of the freeze-dryer
Martin Christ Gefriertrocknungsanlagen GmbH is a registered manufacturer of electric and electronic devices that are solely intended for commercial use.
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• Comply with all local rules and regulations.
9.2 Disposal of the packaging
• Dispose of the packaging, after having separated the individual materials.
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• Comply with all local rules and regulations.
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Manufacturer:
Martin Christ Gefriertrocknungsanlagen GmbH An der Unteren Söse 50 37520 Osterode Germany
Type:
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Part number:
101541
101542
Performance data
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Ice condenser
- capacity:
- performance:
- temperature:
- chamber volume:
4 kg max 4 kg / 24 h max approx. –55°C approx. 6.5 l
4 kg max 4 kg / 24 h max approx. –85°C approx. 6.5 l
Possible shelf temperatures ( single chamber method): freezing and drying inside the ice condenser chamber
approx. –20°C to +60°C
approx. –35°C to +60°C
Possible shelf temperatures ( double chamber method): drying outside the ice condenser chamber
Room temperature to +60°C
Room temperature to +60°C
Max. shelf surface area ( double chamber method): drying outside the ice condenser chamber
drying in injection vials with sealing under vacuum or nitrogen atmosphere outside the ice condenser chamber
drying in round bottom flasks
5 shelves, Ø 265 mm each A
total
=0.28m2 distance 79 mm with accessory no. 120902 or 5 shelves, 360 mm each A
total
=0.51 m
2
distance 70 mm with accessory no. 120916
4 shelves, 250 mm each A
total
=0.18 m
2
distance 50 mm with accessory no. 121011
12 pieces or 24 pieces
10 shelves, Ø 200 mm each A
total
=0.31m2 distance 79 mm with accessory no. 120902 or 5 shelves, 360 mm each A
total
=0.51 m
2
distance 70 mm with accessory no. 120916
4 shelves, 250 mm each A
total
=0.18 m
2
distance 50 mm with accessory no. 121011
12 pieces or 24 pieces
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10 Technical data
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Connection requirements (without vacuum pump and accessories)
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Electrical connection:
1 x 230V / 50-60 Hz
1 x 230V / 50-60 Hz
Protection class:
I
I
IP protection category according to DIN 60529:
11
11 Apparent power:
0.85 kVA
1.6 kVA
Nominal current:
4.0 A
7.0 A
Mains fuse:
10 A F
12 A F
Vacuum pump connection:
230 V, 50/60 Hz, 6.0 A max.
230 V, 50/60 Hz, 5.0 A max.
Filling quantity
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Refrigerant: filling quantity / CO2 equivalent
- R290:
- R404A:
- R508A:
-­160 g / 0.60 t 22 g / 0.26 t
12 g / < 0.01 t 130 g / 0.49 t 26 g / 0.31 t
Physical data (without vacuum pump and accessories)
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Dimensions
- height:
- width:
- depth:
415 mm 390 mm 520 mm + 80 mm vacuum
connection
415 mm 390 mm 520 mm + 80 mm vacuum
connection
Weight:
approx. 42 kg
approx. 55 kg
Noise level according to DIN 45635:
54 dB(A)
54 dB(A)
EMC according to EN 55011:
Class B
Class B
Heat emission:
0.6 kW min.
1.1 kW max.
1.1 kW min.
1.6 kW max.
Equipment connections
Alpha 1-4 LDplus
Alpha 2-4 LDplus
Vacuum connection:
Small flange connection DN25KF (ISO 28403, DIN 2861)
Small flange connection DN25KF (ISO 28403, DIN 2861)
Aeration and media drain valve:
Hose nozzle DN10 (outside diameter 12 mm)
Hose nozzle DN10 (outside diameter 12 mm)
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10.1 Ambient conditions
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• The figures are valid for an ambient temperature of +20°C.
• Allowable ambient temperature +10 °C to +25 °C.
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• Max. humidity 85% (non-condensing) at +25°C.
10.2 Technical documentation
The technical documentation of this freeze-dryer (e.g. circuit diagram, cooling system ) and the safety data sheets of the manufacturers of refrigerant and heat transfer medium is not attached to this operating manual.
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You can order these documents from our service department.
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1Ice condenser
chamber with an
internal ice condenser 2User interface (see
chapter 6.5.1 - "User
interface") 3Mains power switch
4Pipe connection of the
vacuum pump (behind
the cover plate) 5Ice condenser
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11.1 Brief operating instructions
Functional and operating elements
Fig. 50: Total view of the freeze-dryer
Fig. 51: Ice condenser chamber
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6Equipotential bonding
screw 7Aeration and media
drain valve
8Vacuum connection 9Name plate (see
chapter 2.1.2 - "Name
plate") 10 Heat exchanger of the
refrigeration unit 11 Electrical connection of
the vacuum sensor 12 Power supply of the
pressure control valve 13 Power supply of the
vacuum pump 14 Mains fuse 15 Mains cable
Fig. 52: Left side of the freeze-dryer
Fig. 53: Rear view of the freeze-dryer
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1 Left function key 2 Right function key 3 "Up" key 4 "Down" key 5 Display
NOTE
Ensure that the layer thickness of 1 to 2 cm is not exceeded, since otherwise the drying time needs to be extended.
NOTE
Recommendation: Store the product vessels on the aluminium shelves or, if possible, the entire rack with the shelves in the deep- freeze. The advantage is that due to the higher cold storage capacity of the aluminium material, the product will remain frozen for a longer period of time so that the sample will not thaw.
Fig. 54: LDplus user interface
Step-by-step instructions – shelf drying
1Freeze the sample separately, e.g. in a deep-freeze.
2Check the ice condenser chamber and ensure that it is completely free
from water residues. 3Close the media drain valve and install the base plate. 4Switch the unit on 20 to 30 minutes prior to the start of the drying
process in order to let the vacuum pump warm up. 5Place the plate rack on the base plate. 6Transport the frozen samples as quickly as possible from the deep-
freeze to the freeze-dryer and place them on the shelves.
7 nstall the drying chamber. Prior to doing so, check whether the O-ring
is completely free of dirt particles. The ground-in stopper of the acrylic
glass bell must be greased with high-vacuum grease. 8Ensure that all of the valves of the acrylic glass bell are closed. 9Ensure that the aeration valve is closed. 10 Ensure that the media drain valve is closed. 11 Start the main drying process either by opening the manual shut-off
valve or by waiting for the electromagnetic valve to open. Vacuum is
applied to the chamber and the freeze-drying process commences.
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NOTE
The vacuum pump always runs with maximum power. With this type of freeze-dryer, the power of the vacuum pump cannot be controlled.
CAUTION
Ensure that no water gets into the pipe connection of the vacuum pump or vacuum sensor.
NOTE
Ensure that the layer thickness of 1 to 2 cm is not exceeded, since otherwise the drying time needs to be extended.
12 The operating panel displays the vacuum, the ice condenser
temperature, and the current operating mode. 13 The end of the process is reached when the ice condenser is no longer
loaded and when it again reaches a final temperature of approximately -
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature. 14 Switch the vacuum pump off and aerate the drying chamber via the
media drain valve or via a rubber valve. 15 Switch the unit off by actuating the mains power switch and take the
product out of the freeze-dryer. 16 Switch the unit on again and start the defrosting process (button
"Operating mode: select/start" – "Defrosting”).
17 Drain the defrosting water via the media drain valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel. 18 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
service life of the vacuum sensor.
Step-by-step instructions – drying in a flask
1Freeze the sample separately, e.g. in a deep-freeze.
2Check the ice condenser chamber and ensure that is completely free
from water residues. 3Install the drying chamber. Prior to doing so, check whether the O-ring
is completely free of dirt particles. The ground-in stopper of the acrylic
glass bell must be greased with high-vacuum grease. 4Ensure that all of the valves are closed. 5Let the vacuum pump warm up 20 to 30 minutes before the freeze-
drying processes commences. 6Connect a frozen sample to a valve.
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CAUTION
After the pressure has fallen below 1.030 mbar, a frozen sample can be connected to a valve. The next frozen sample cannot be connected to another valve until the pressure is again lower than 1.030 bar.
NOTE
The vacuum pump always runs with maximum power. With this type of freeze-dryer, the power of the vacuum pump cannot be
controlled.
NOTE
The drying time depends on the layer thickness of the sample, the solids content of the sample, and the amount of heat that is supplied during the drying process. In the case of a layer thickness of 1 cm, the freeze-drying process usually takes 24 hours.
CAUTION
Ensure that no water gets into the pipe connection of the vacuum pump or vacuum sensor.
7The operating panel displays the vacuum, the ice condenser
temperature, and the current operating mode. 8The end of the process is reached when the ice condenser is no longer
loaded and when it again reaches a final temperature of approximately -
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature.
9Switch the vacuum pump off and aerate the drying chamber via the
media drain valve or via a rubber valve. 10 Switch the unit off by actuating the mains power switch and take the
product out of the freeze-dryer. 11Switch the unit on again and start the defrosting process (button
"Operating mode: select/start" – "Defrosting").
12 Drain the defrosting water via the defrosting water valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel. 13 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
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service life of the vacuum sensor.
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11.2 EC declaration of conformity in accordance with the EC Machinery Directive
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11.3 Declaration of conformity – China RoHS 2
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11.4 Resistance to stress cracking and chemical influences "Plexiglas"
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12 Glossary
Desorption
Desorption (from Latin de-sorbere, sorbere = sup up, suck in) describes a phenomenon whereby molecules are released from the surface of a solid. In order to be able to desorb, the particle must have, or be provided with, a sufficient amount of energy in order to overcome the binding energy.
Eutectic point
The eutectic point is the point at which a homogenous mixture (e.g. a eutectic alloy) passes directly from the liquid to the solid phase without the formation of a crystal mixture that consists of different phases.
Single-chamber method
At the single-chamber method, the freezing as well as the subsequent drying of the product are both performed in the ice condenser chamber. The sample is frozen as a result of the low temperature of the ice condenser (–55°C in the case of one-stage systems or –85°C in the case of two-stage systems). The inside of the chamber can be cooled to approximately –20°C or –40°C. The moderate supply of the frozen sample with energy, which is necessary during the main drying phase, is ensured by heatable shelves on which the product is placed.
Double-chamber method
Drying on shelves outside the ice condenser chamber is referred to as a double-chamber system. The advantage compared to the single- chamber method is the considerably higher product capacity. In addition, the product chamber can be isolated from the ice condenser chamber by an intermediate valve in order to perform a so-called pressure increase test for determining the end of the drying process. In freeze-dryers without an active shelf cooling, the samples need to be pre-frozen externally, e.g. in a deep-freeze or freezer cabinet. After the transfer of the product into the freeze-dryer, the actual sublimation is started.
Reference designator
During the service life of industrial systems, a standardised reference designation system is required for the planning, design, realisation, maintenance, and disassembly stages in order to be able at all times to identify every single component within the system in an unambiguous manner. The reference designators) are affixed to the components and entered into the technical documentation (e.g. circuit diagrams).
Sublimation
Sublimation (from Latin "sublimis" = high up in the air, raised), is a thermodynamic process of the direct transition of a substance from the
=== Ende der Liste für Textmarke Inhalt ===
solid phase to the gas phase.
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13 Index
A
Aborting the warm-up phase ...................... 44
Accessories ................................... 10, 25, 62
Accident prevention ................................... 23
Active phases ............................................ 42
Aeration valve .......................... 12, 33, 68, 71
Aeration valve, cleaning and care .............. 60
Aeration valve, malfunction ........................ 54
Ambient conditions ..................................... 69
Ambient temperature ........................... 32, 69
Apparent power ................................... 13, 68
Automatic phase change ............................ 50
B
Brief operating instructions ......................... 70
C
CE mark in compliance with the directive
2006/42/EC ............................................ 21
Changing set values .................................. 45
Changing the display contrast .................... 49
Changing the phase ................................... 43
Chemical and biological safety ................... 26
Chemical reactions .................................... 62
China RoHS 2 – Declaration of conformity . 77
Circuit diagram ........................................... 69
Cleaning agents ................................... 59, 63
Cleaning of the freeze-dryer ....................... 60
Cleaning the freeze-dryer and the
accessories ............................................ 59
Click at button push ................................... 50
Commissioning .......................................... 10
Connection................................................. 33
Connection requirements ........................... 68
Cooling system .......................................... 69
Copyright ................................................... 10
Corrosion ............................................. 59, 62
Cost estimate ............................................. 65
Cracks ....................................................... 62
Current function of the function keys .......... 41
Customer-provided fuses ........................... 33
D
Dangerous goods....................................... 24
Dangerous materials .................................. 63
Declaration of conformity – China RoHS 2 . 77 Declaration of conformity (Machinery
Directive) .......................................... 10, 76
Declaration of decontamination .................. 65
Decontamination agents ............................ 63
Defrosting the ice condenser ..................... 47
Desorption ................................................. 97
Dimensions .......................................... 29, 68
Direct hazard to the life and health ............. 22
Disinfectants .............................................. 63
Disinfection of the drying chamber and
accessories ............................................ 63
Display ....................................................... 41
Disposal of the freeze-dryer ....................... 66
Disposal of the packaging .......................... 66
Double-chamber method ............................ 97
E
Earth conductor check ............................... 27
EC declaration of conformity (Machinery
Directive) .......................................... 10, 76
Electrical connection .................................. 68
Electrical connection of the vacuum sensor
......................................................... 12, 71
Electrical lifting hoist .................................. 48
Electrical safety .......................................... 25
EMC according to EN 55011 ...................... 68
Emissions .................................................. 26
End of drying and aeration ......................... 19
Equipment connections .............................. 68
Equipotential bonding screw .......... 12, 27, 71
Error correction .......................................... 53
Error messages ................................... 27, 56
Eutectic point ............................................. 97
Exhaust filter ........................................ 36, 62
Explanation of symbols .............................. 10
Explanation of the symbols and notes ........ 22
Extended service menu.............................. 51
F
Filling quantity ............................................ 68
Final drying ................................................ 19
Fire prevention ........................................... 26
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Form for the return of defective parts ......... 65
Freeze-dryer, cleaning and care ................ 60
Freeze-drying phases ................................ 16
Freeze-drying process ............................... 17
Freezing ..................................................... 17
Function keys ............................................. 40
Functional and operating elements ............ 11
Fuses ......................................................... 26
G
General conditions ................................ ..... 10
General information on freeze-drying ......... 14
General work (maintenance) ...................... 59
H
Hazard warnings .................................... 9, 10
Heat emission ............................................ 68
Heat exchanger ......................................... 61
Heat exchanger of the refrigeration unit 12, 71
High temperature resolution ....................... 50
Highly corrosive substances ...................... 25
I
Ice condenser ............................................ 67
Ice condenser chamber........................ 11, 70
Ice condenser chamber, cleaning and care 60
Importance of the operating manual ............. 9
Important information ................................. 22
Infectious substances .......................... 26, 63
Inflammable substances ............................ 26
Informal safety instructions ........................ 24
Initial start-up ............................................. 39
Inspection by the manufacturer .................. 64
Installation of accessories .......................... 39
Installation site ........................................... 32
Insufficient ice condenser temperature ....... 55
Insufficient vacuum .................................... 53
Intended use ................................................ 9
IP protection category according to DIN
60529 ..................................................... 68
K
Lifting hoist, electrical ................................. 48
Load default settings .................................. 51
M
Main drying ................................................ 18
Main menu ................................ ................. 45
Mains cable .......................................... 12, 71
Mains fuse ..................................... 12, 68, 71
Mains power switch .............................. 11, 70
Maintenance (general work) ....................... 59
Maintenance (vacuum sensor) ................... 62
Maintenance and service ........................... 59
Malfunctions ............................................... 53
Manufacturer ................. 24, 26, 59, 63, 66, 67
Marking of the unit ..................................... 21
Max. humidity ............................................. 69
Maximum current for the vacuum pump ..... 36
Mechanical safety ...................................... 25
Media drain valve ..................... 12, 33, 68, 71
Media drain valve, cleaning and care ......... 60
Media drain valve, malfunction ................... 54
Mode .......................................................... 43
Mode of operation ...................................... 14
N
Name plate .........................12, 13, 25, 33, 71
Noise level ................................................. 68
Nominal current ......................................... 68
Nominal voltage ................................... 13, 25
Notes on safety and hazards ....................... 9
Notes on transport ..................................... 30
O
Oil mist separator ................................. 36, 62
Operating elements .................................... 11
Operating personnel .................................. 23
Operating state .......................................... 42
Operating voltage....................................... 33
Operational safety ...................................... 62
Option: electrical lifting hoist ...................... 48
Options ...................................................... 49
Keys "up" and "down" ................................ 40
L
Layout of the freeze-dryer .......................... 11
LDplus configuration .................................. 51
LDplus control system ................................ 40
P
Packaging ............................................ 31, 66
Part number ............................................... 67
Pathogenic substances .................. 26, 60, 63
Pending information ................................... 42
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