Christ Alpha 3-4 LSCbasic Operating Manual

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Rev. 1.2 of 05/03/2019 Alpha 3-4 LSCbasic; ;
Version 11/2018
Alpha 3-4 LSCbasic
Part no. 102394, 102395
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: info@martinchrist.de
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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 .............................................................................................................. 11
2 Layout and mode of operation .......................................................................................... 12
2.1 Layout of the freeze-dryer ............................................................................................... 12
2.1.1 Functional and operating elements ............................................................................ 12
2.1.2 Name plate ................................................................................................................ 14
2.2 Mode of operation ........................................................................................................... 15
2.2.1 General information on freeze-drying ......................................................................... 15
2.2.2 Freeze-drying process ............................................................................................... 18
2.2.2.1 Preparation ........................................................................................................ 18
2.2.2.2 Freezing ............................................................................................................. 18
2.2.2.3 Main drying ........................................................................................................ 19
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 ....................................................................................................... 24
3.5 Informal safety notes....................................................................................................... 24
3.6 Safety notes concerning the transport, set-up and connection and initial start-up
of the freeze-dryer .......................................................................................................... 25
3.6.1 General hazards ........................................................................................................ 25
3.6.2 Hazards caused by improper transport ...................................................................... 25
3.6.3 Hazards caused by improper set-up .......................................................................... 25
3.6.4 Hazards caused by improper connection ................................................................... 26
3.7 Safety notes concerning the operation ............................................................................ 26
3.7.1 Hazards caused by electricity .................................................................................... 26
3.7.2 Hazards caused by the refrigeration system (natural, flammable refrigerants) ........... 27
3.7.3 Hazards caused by harmful products ......................................................................... 27
3.7.4 Hazards caused by acids in the products ................................................................... 27
3.7.5 Hazards caused by contaminated condensate (defrosting water) .............................. 28
3.7.6 Hazards caused by hot surfaces ................................................................................ 28
3.7.7 Hazards caused by cold surfaces .............................................................................. 28
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3.8 Safety devices ................................................................................................................ 28
3.8.1 System check ............................................................................................................ 28
3.8.2 Earth conductor check ............................................................................................... 28
3.9 Procedures in the event of hazards and accidents .......................................................... 29
3.10 Maintenance and cleaning of the freeze-dryer ................................................................ 29
3.11 Measures to be taken to ensure safe operation of the freeze-dryer ................................. 30
3.12 Remaining hazards ......................................................................................................... 31
4 Storage and transport ....................................................................................................... 32
4.1 Dimensions and weight ................................................................................................... 32
4.2 Storage conditions .......................................................................................................... 32
4.3 Notes on transport .......................................................................................................... 33
4.4 Packaging ....................................................................................................................... 34
4.5 Transport locking devices ............................................................................................... 34
5 Set-up and connection ...................................................................................................... 35
5.1 Location of use ............................................................................................................... 35
5.2 Power supply .................................................................................................................. 36
5.2.1 Connection ................................................................................................................ 36
5.2.2 Customer-provided fuses ........................................................................................... 36
5.3 Aeration valve ................................................................................................................. 36
5.4 Media drain valve ............................................................................................................ 37
5.5 Vacuum sensor ............................................................................................................... 37
5.6 Vacuum pump................................................................................................................. 39
5.7 Pressure control valve .................................................................................................... 40
5.8 Installation of the accessories ......................................................................................... 41
5.8.1 Rubber valves ............................................................................................................ 42
6 Operation ............................................................................................................................ 44
6.1 Initial start-up .................................................................................................................. 44
6.2 Preparation ..................................................................................................................... 44
6.3 Switching the freeze-dryer on ......................................................................................... 44
6.4 LSCbasic control system ................................................................................................ 45
6.4.1 User interface ............................................................................................................ 45
6.4.1.1 Main window "Process" ...................................................................................... 46
6.4.1.2 Main window "Options" ...................................................................................... 55
6.4.1.3 Main window "?" ................................................................................................. 65
6.4.2 Starting a freeze-drying process ................................................................................ 65
6.4.2.1 Entering set values ............................................................................................ 66
6.5 Optional extensions ................................................................ ........................................ 68
6.6 Switching the freeze-dryer OFF ...................................................................................... 68
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7 Malfunctions and error correction .................................................................................... 69
7.1 General malfunctions ...................................................................................................... 69
7.1.1 Power failure ................................................................................................ .............. 70
7.1.2 Insufficient vacuum .................................................................................................... 71
7.1.2.1 Small flange connections ................................................................................... 71
7.1.2.2 Aeration valve, media drain valve ...................................................................... 72
7.1.2.3 Pressure control valve ........................................................................................ 72
7.1.2.4 Rubber valves .................................................................................................... 72
7.1.2.5 Vacuum sensor ................................................................................................ .. 72
7.1.3 Insufficient ice condenser temperature ...................................................................... 73
7.2 Process and error messages .......................................................................................... 73
7.3 Service contact ............................................................................................................... 74
8 Maintenance and service ................................................................................................... 75
8.1 Maintenance ................................................................................................................... 75
8.1.1 General ...................................................................................................................... 75
8.1.2 Ice condenser chamber ............................................................................................. 76
8.1.3 Aeration valve, media drain valve .............................................................................. 76
8.1.4 Heat exchanger (only for air-cooled freeze-dryers) .................................................... 77
8.1.5 Vacuum pump ........................................................................................................... 78
8.1.6 Exhaust filter (oil mist separator) ................................................................................ 78
8.1.7 Vacuum sensor .......................................................................................................... 79
8.1.8 Accessories ................................................................................................ ............... 79
8.2 Disinfection of the drying chamber and accessories ....................................................... 80
8.3 Service ........................................................................................................................... 80
8.4 Return of defective parts ................................................................................................. 81
9 Disposal .............................................................................................................................. 82
9.1 Disposal of the freeze-dryer ............................................................................................ 82
9.2 Disposal of the packaging ............................................................................................... 82
10 Technical data .................................................................................................................... 83
10.1 Ambient conditions ......................................................................................................... 84
10.2 Technical documentation ................................................................................................ 84
11 Appendix ............................................................................................................................ 85
11.1 EC declaration of conformity in accordance with the EC Machinery Directive ................. 85
11.2 Declaration of conformity – China RoHS 2 ...................................................................... 87
11.3 EC declaration of conformity in accordance with the Pressure Equipment Directive ....... 89
12 Glossary ............................................................................................................................. 91
13 Index ................................................................................................................................... 93
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1 General information
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
must be complied with.
1.2 Intended use
The freeze-dryer has been exclusively designed for the freeze-drying of solid or liquid products. It is, therefore, solely intended for this application. The freeze-dryer must correspond to the solvent package for flask drying (part number: 102394) or to the solvent package "universal system" (part number: 102395). The freeze-dryer may only be used with the specified accessories made by Martin Christ Gefriertrocknungsanlagen GmbH.
The freeze-dryer is suitable for freeze-drying solid substances and liquid solutions (e.g. bacteria and virus cultures, blood plasma, serum fractions, antibodies, sera, vaccines and pharmaceutical products such as chloramphenicol, streptomycin, vitamins, ferments and plant extracts for biochemical tests).
The solvents that are used must be of the temperature classes T1 to T4 as per DIN EN-60079-0:2014-06. We recommend performing a workplace evaluation in terms of the handling of flammable solutions in accordance with the local labour legislation.
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 following operations are regarded as NOT PERMISSIBLE:
operation of the freeze-dryer if it is not properly installed
use of the freeze-dryer if it is not in a perfect technical state
use of the freeze-dryer within hazardous locations where there is a risk
of explosions
use of the freeze-dryer within locations with insufficient ventilation
use of the freeze-dryer with unauthorised additions or conversions
without the written approval by Martin Christ Gefriertrocknungsanlagen GmbH
use of the freeze-dryer with accessories that have not been approved by Martin Christ Gefriertrocknungsanlagen GmbH
freeze-drying of products that may react during the freeze-drying process following the supply of high amounts of energy
freeze-drying of azide-containing products
use of substances that damage the material (stainless steel 1.4404 and
1.4435, borosilicate glass, EPDM, PVDF, ceramic AI2O3 and PTFE) or decrease the mechanical strength
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The intended use also includes:
observation of all of the notes and instructions that are included in the operating manual
compliance with the inspection and maintenance instructions
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
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.
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
(e.g. sublimation).
1.6 Standards and regulations
EC declaration of conformity in accordance with the EC Machinery Directive (see chapter 11.1 - "EC declaration of conformity in accordance with the EC Machinery Directive")
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Name
Part number
Freeze-dryer Alpha 3-4 LSCbasic
102372
Capacitive vacuum sensor
125491
Vacuum pump RC6
125295
Corrugated hose, stainless steel
510075
Reducing adapter DN 25/DN 16
141717
Pressure control valve
125908
Manifold with 12 rubber valves, including a glass cover
121212
Name
Part number
Freeze-dryer Alpha 3-4 LSCbasic
102372
Capacitive vacuum sensor
125491
Vacuum pump RC6
125295
Corrugated hose, stainless steel
510075
Reducing adapter DN 25/DN 16
141717
Pressure control valve
125908
Base plate, stainless steel
120921
Guide tube
122036
3 shelves
120903
Adapter ring
113412
Drying chamber made of real glass
122300
Connecting ring with 12 rubber valves
113398
Glass cover
121448
1.7 Scope of supply
Solvent package for round bottles (part no. 102394) includes:
Solvent package universal (part no. 102395) includes:
In addition, every package includes:
1 tube of high vacuum grease
1 litre of vacuum pump oil
1 set of small parts
1 drain hose 0.4 m (silicone 8 x 12 mm)
1 operating manual
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1 Ice condenser
chamber
2 LSCbasic user (see
chapter 6.4.1 - "User interface")
3 Mains power switch
4 Pipe connection of the
vacuum sensor
5 Pipe connection of the
vacuum pump (behind the cover plate)
6 Ice condenser
2 Layout and mode of operation
2.1 Layout of the freeze-dryer
2.1.1 Functional and operating elements
Fig. 1: Total view of the freeze-dryer
Fig. 2: Ice condenser chamber
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7 Aeration valve 8 Media drain valve
9 Touchpanel
Fig. 3: Left side of the freeze-dryer
Fig. 4: User interface with touchpanel
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10 Heat exchanger of the
refrigeration unit
11 Name plate (see
chapter 2.1.2 - "Name
plate") 12 Vacuum connection 13 Serial interface 14Electrical connection of
the vacuum sensor 15Connection of the
vacuum sensor 16Power supply of the
pressure control valve 17Power supply of the
vacuum pump 18 Mains fuse 19 Mains cable 20Equipotential bonding
screw
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. 6: Example of a name plate
Fig. 5: Rear view of the freeze-dryer
2.1.2 Name plate
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2.2 Mode of operation
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?
An 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 for ice and water (sublimation pressure curve) 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).
At 6.11 mbar and 0.0098°C, the melting pressure curve, vapor pressure curve, and sublimation pressure curve meet in one point, the so-called triple point. In this point, all three phases coexist (simultaneously).
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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Fig. 7: Vapour pressure curve for ice and water (Sublimationsdruckkurve
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 for ice and water.
(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] [Lyophilisation].
Fig. 8: Freeze-drying phases
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NOTE
In the case of a solvent-containing product or of a product with a high salt concentration, the product may thaw during the freeze-drying process. This is indicated by easily visible foaming. To prevent this, the product must be frozen down to a very deep temperature, e.g. in liquid nitrogen, prior to placing it in the freeze-dryer.
2.2.2 Freeze-drying process
The main components of a freeze-dryer are:
vacuum drying chamber or drying manifold,
vacuum pump for generating a vacuum inside the drying chamber,
ice condenser for binding the water vapour that is released by the
2.2.2.1 Preparation
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 and LSCbasic 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. 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.
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2.2.2.3 Main drying
When the product is frozen, 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 for ice and water (sublimation pressure curve). 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.
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 for ice and water as well as on the final vacuum of the vacuum pump that is
used. The process is supported by a higher shelf temperature.
2.2.2.5 End of drying and aeration
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
-105°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.
Then, the product can be removed from the unit.
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2.2.2.6 Defrosting Defrosting with hot gas
As standard, the freeze-dryer is equipped with a hot-gas defrosting system. In order to defrost the ice condenser, heated refrigerant is fed through the heating coil. In addition, the bottom of the ice condenser chamber is heated by way of a heating collar.
In order to avoid damage, the condensate must be drained off through the media drain valve 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
Filled with natural inflammable refrigerants
Protective earth (ground)
CE mark in compliance with the directive 2006/42/EC
Earth (ground)
China RoHS 2 mark (only for China)
Unplug the mains plug
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.
3 Safety
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.
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 on/with the freeze-dryer
are 18 years old or older,
have been specifically ordered to do so by the operator/owner and that
they have been duly informed about the specific hazards associated with the system, supply media and starting/final products as well as about the correct conduct and necessary measures to take in the event of accidents or malfunctions,
are familiar with the fundamental health, safety and accident prevention
regulations
have been trained in terms of the operation of this system,
have read and understood this operating manual (in particular the safety
sections and warning notes) and confirmed this with their signature.
The operator must observe the system limits defined by the
manufacturer in which a risk assessment for explosive atmospheres has been performed. The defined system limits include
– the drying chamber up to the aeration valve, drain valve and
pressure control valve,
the glass cover with/without a manifold and the chamber made of real glass.
The freeze-dryer must correspond to the solvent package for flask
drying (part number: 102394) or to the solvent package "universal system" (part number: 102395).
Freeze-drying products with a high solvent concentration may lead to
the formation of potentially explosive gas mixtures. This is why the operator must provide standard operating procedures (SOPs) for the freeze-drying of the various products, including specifications concerning the chamber pressure. The solvents that are used must be of the temperature classes T1 to T4 as per DIN EN-60079-0:2014-06.
The operator must comply with the specifications of DIN EN 378-
1:2018-04 and DIN EN 378-2:2018-04 for refrigeration systems and heat pumps.
The operator must comply with the specifications of DIN EN 378-
3:2017-03 and DIN EN 378-4:2017-03 for refrigeration systems and heat pumps.
The safety-conscious work of the personnel in compliance with the
instructions for use/operating instructions, SOPs and with the relevant EC directives and the national laws concerning health and safety and the prevention of accidents must be checked at regular intervals (e.g. every month).
The areas of responsibility of the personnel concerning the operation,
maintenance and care of the unit must be clearly defined.
The operator must perform a risk assessment concerning potential
accidents in connection with the freeze-dryer and take appropriate countermeasures, if necessary, for example the use of a safety cabinet.
The operator must perform a compatibility test of all the substances that
are used in the freeze-dryer (products to be dried as well as cleaning agents, etc.) and that come into contact with the chamber walls, shelves, pipes/hoses and seals. The use of substances that damage
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the material (stainless steel 1.4404 and 1.4435, borosilicate glass, EPDM, PVDF, ceramic AI2O3 and PTFE) or decrease the mechanical strength is prohibited.
The system must be maintained at regular intervals (see chapter 8 -
"Maintenance and service").
Any parts or components that are not in perfect working order must be
replaced without delay.
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
dangers originating from the freeze-dryer, supply media, starting and end products by the operator,
be familiar with the fundamental regulations concerning workplace
safety and accident prevention
have been trained in terms of the operation of this unit, and
have read and understood this operating manual (and in particular the
safety sections and warning notes) and confirmed this with their
signature.
3.5 Informal safety notes
This operating manual is part of the product.
This 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 every subsequent owner
or user of the freeze-dryer.
Any changes, additions or updates received must be added to the
operating manual.
In addition to the operating manual, the general and operational rules
and regulations for the prevention of accidents and the protection of the environment must be provided.
All of the safety and hazards notes on the freeze-dryer must be kept
readable at all times. If necessary, they must be replaced.
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WARNING
General risk of injury
Among the general hazards during the transport, set-up and connection and start-up of the freeze-dryer are impact hazards, crushing hazards, grazing hazards, cutting hazards, etc.
This may lead to severe injuries.
Comply with the fundamental health and safety rules and regulations as well as with the rules and regulations for the prevention of accidents!
Wear personal protective equipment (safety shoes, work gloves, and hardhat)!
DANGER
Risk of injury caused by the uncontrolled movement of loads
Units that are not properly fastened or secured may shift, or fall over.
Prior to transporting or setting-up the freeze-dryer, read the chapter 4 - "Storage and transport" thoroughly!
WARNING
Risk of injury caused by poor accessibility of the freeze-dryer
In cramped spaces or locations with poor accessibility, sharp edges and corners may protrude into the work area.
This may lead to injuries caused by impact hazards or grazing hazards.
Ensure that the freeze-dryer is set up freely accessible!
Comply with the fundamental health and safety rules and regulations
as well as with the rules and regulations for the prevention of accidents!
3.6 Safety notes concerning the transport, set-up and connection and initial start-up of the freeze-dryer
The following notes and instructions must be observed in order to protect
3.6.1 General hazards
all persons and property.
3.6.2 Hazards caused by improper transport
3.6.3 Hazards caused by improper set-up
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WARNING
Risk of injury caused by consequences of improper connection
Improper connection may lead to a hazardous electrical incident at a later time during the operation of the freeze-dryer.
This may lead to severe damage to health or even life-threatening injuries.
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.
DANGER
Danger of life caused by electric shock
There is a risk of electric shock when touching current-carrying components.
This may lead to ventricular fibrillation, cardiac arrest, or respiratory paralysis.
Only qualified electritians are authorised to perform work on the electrical system of the freeze-dryer!
The electrical equipment of the freeze-dryer must be checked at regular intervals by a qualified electrician! Defects such as loose connections or burnt cables must be eliminated immediately.
3.6.4 Hazards caused by improper connection
3.7 Safety notes concerning the operation
The following notes and instructions concerning the operation of the freeze­dryer must be observed in order to protect all persons and property.
3.7.1 Hazards caused by electricity
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DANGER
Risk of explosion due to refrigerants
The refrigerants used are highly flammable and can form an explosive mixture if their concentration in the ambient air is sufficiently high.
There is an explosion hazard.
Work on the refrigeration system of the freeze-dryer must only be carried out by qualified specialist personnel who have been trained to handle flammable refrigerants!
Ensure good ventilation and make sure that no ignition sources (e.g. soldering iron, welding equipment) are present!
DANGER
Risk of poisoning/infection caused by the products
Operating personnel: When loading and unloading the drying chamber, the personnel are
exposed to the product. Maintenance personnel: When performing maintenance work on parts coming into contact with the
product (e.g. all parts inside the chamber), the personnel may be exposed to product residues.
Skin contact or the inhalation of particles may cause severe damage to health depending on the product in question.
Operating personnel:
Wear suitable protective clothes, gloves, and respiratory protection!
Maintenance personnel:
Take suitable decontamination measures prior to commencing the maintenance!
Wear suitable protective clothes and gloves!
DANGER
Risk of injury caused by acids in the products
Products containing acids may damage the material of the components of the freeze-dryer and affect the mechanical strength.
This may lead to severe injuries. Freeze-drying of products containing acids is only permissible if special
protective measures and equipment-related precautions are taken! Consultation of Martin Christ Gefriertrocknungsanlagen GmbH is abso­lutely mandatory in order to define the measures that need to be taken!
Refer to the safety data sheets of the products that are used!
3.7.2 Hazards caused by the refrigeration system (natural, flammable refrigerants)
3.7.3 Hazards caused by harmful products
3.7.4 Hazards caused by acids in the products
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WARNING
Risk of poisoning/infection caused by contaminated condensate (defrosting water)
The condensate may contain harmful substances originating from the product.
Contact with the condensate may cause severe damage to health.
Ensure the environmentally sound disposal of the condensate in compliance with the local rules and regulations!
Wear suitable protective clothes, gloves, and respiratory protection!
WARNING
Risk of burns on hot surfaces
After a drying process, some or all of the surfaces inside the chamber may still be hot.
There is a risk of burns when touching the surfaces.
Wear suitable protective clothes and gloves!
Do not touch the surfaces on purpose!
WARNING
Risk of freezing to cold surfaces
The ice condenser coils can already be cold during the loading phase. There is a risk of freezing to the ice condenser coils when touching the
surfaces.
Wear suitable protective clothes and gloves!
Do not touch the surfaces on purpose!
3.7.5 Hazards caused by contaminated condensate (defrosting water)
3.7.6 Hazards caused by hot surfaces
3.7.7 Hazards caused by cold surfaces
3.8 Safety devices
3.8.1 System check
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" (chapter 6.4.1.1 - "Main window "Process"", chapter 7.2 - "Process and error messages").
3.8.2 Earth conductor check
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.
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3.9 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.
IF IN DOUBT, CALL THE EMERGENCY PHYSICIAN (AMBULANCE)!
3.10 Maintenance and cleaning of the freeze-dryer
The substances and materials that are used must be properly handled and disposed of (Please refer to the safety data sheets!). This applies particularly to
the handling of solvents, lyes, and acids,
the changing and topping-up of operating supplies.
Compliance with the national rules and regulations must be ensured.
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3.11 Measures to be taken to ensure safe operation of the freeze-dryer
In order to ensure the safe operation of the freeze-dryer, please comply
with the following points prior to every freeze-drying process:
Set-up, connection and operation
Ensure that the freeze-dryer was set up and connected properly (see chapter 5 - "Set-up and connection").
Check the freeze-dryer and the accessories before every start-up for any visible signs of damage.
Do not hit or move the freeze-dryer during its operation.
Do not lean against or rest on the freeze-dryer during its operation.
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.
Fire prevention
Fuses protect certain electrical circuits within the freeze-dryer against over-current conditions. Always use fuses of the same type and rating.
Safety area
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 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.
Do not stay in the safety area longer than what is absolutely necessary for the operation of the freeze-dryer.
Accessories
Do not use the freeze-dryer with accessories that shows signs of damage.
Only use accessories that have been approved by Martin Christ Gefriertrocknungsanlagen GmbH. This does not apply to commercially available freeze-drying vessels made of glass. We explicitly warn against the use of equipment of poor quality! Breaking glass or bursting vessels can cause dangerous situations during the freeze-drying
process.
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3.12 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.
Immediately eliminate any problems that can affect safety.
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Alpha 3-4 LSCbasic
Height:
415 mm
Width:
780 mm
Depth:
555 mm + 80 mm vacuum connection
Weight:
approx. 86 kg
4 Storage and transport
4.1 Dimensions and weight
4.2 Storage conditions
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 3-4 LSCbasic weighs approx. 86 kg!
CAUTION
The centre of gravity of the freeze-dryer is off-centre!
correct
incorrect
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 locking devices").
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. 9: Lifting the freeze-dryer
When setting the unit down, ensure that the feet are upright (see figures below).
Fig. 10: Unit feet
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CAUTION
The freeze-dryer Alpha 3-4 LSCbasic weighs approx. 86 kg!
CAUTION
The centre of gravity of the freeze-dryer is off-centre!
NOTE
Reinstall the transport locking devices prior to any transport.
4.4 Packaging
The freeze-dryer is packaged in a wooden crate.
After opening the packaging, take out the accessories.
Remove the packaging material.
Remove the side walls of the crate.
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 locking devices
Prior to commissioning, the following transport locking devices must be removed:
Install the vacuum sensor that had been removed for transport(see chapter 5.5 - "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!
5 Set-up and connection
5.1 Location of use
Use the freeze-dryer solely in closed and dry spaces.
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 in the area of the heat exchanger ventilation grid (see chapter 2.1.1 - "Functional and operating elements").
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.
5.2 Power supply
5.2.1 Connection
Christ freeze-dryers are units of protection class I. The freeze-dryers of the type Alpha 3-4 LSCbasic have a three-wire power cord with an IEC C13 connector (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
to be provided by the customer.
5.3 Aeration valve
The aeration valve is located on top of 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.
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NOTE
Please refer to the separate operating manual of the vacuum sensor!
1 Vacuum sensor 2 Connection socket
5.4 Media drain valve
The media drain valve is located at the bottom of the left side of the unit (see chapter 2.1.1 - "Functional and operating elements"). 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
5.5 Vacuum sensor
if there is negative pressure when the media drain valve is opened.
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. 11: 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 (DIN25KF) 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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NOTE
It is absolutely essential to comply with the manufacturer’s instructions in
the separate operating manual of the vacuum sensor!
Pfeiffer CMR 363 (capacitive)
NOTE
The vacuum sensor comes supplied in a calibrated state.
Fig. 12: Vacuum sensor
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
5.4.6 Vacuum pump
5.6 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. 13: 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 air pollution by the oil mist that is emitted more or less strongly by the pump depending on the working pressure.
The exhaust gases must be discharged in a proper manner.
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,
The hose line must be laid in such a mann er that any condensation water cannot flo w back into the pump. In the case of a rising hos e line, we recommend using a condensate trap ( Woulff bottle or wash bottle).
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.
1 Pressure control valve 2 Connection to the
vacuum pump
5.7 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")
Fig. 14: Installation of the pressure control valve
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1 Freeze-dryer 2 Vacuum pump 3Reducing adapter
DN 25/ DN 16
4 Corrugated hose
(stainless steel) 5 Glass cover 6Vacuum sensor 7Manifold 8Rubber valve
5.8 Installation of the accessories
The accessories of the respective packages (see chapter 1.7 - "Scope of supply") must be installed as shown in the illustrations below:
Solvent package for round bottles (part no. 102394)
Fig. 15: Freeze-dryer Alpha 3-4 LSCbasic with solvent package for round bottles
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1 Freeze-dryer 2 Vacuum pump 3Reducing adapter
DN 25/ DN 16 4 Corrugated hose
(stainless steel) 5 Adapter ring 6Vacuum sensor 7Base plate (stainless
steel) 8Guide tube 9Drying chamber made
of real glass, with
three shelves inside 10 Connecting ring with
rubber valves 11 Glass cover
1Locking handle 2Aeration connection 3Vessel connection 4Rubber plug 5Connection to freeze-
dryer (e.g. via a
manifold)
Solvent package universal (part no. 102395)
5.8.1 Rubber valves
Fig. 16: Freeze-dryer Alpha 3-4 LSCbasic with solvent package
The rubber valves 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. 17: Rubber valve
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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.
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.
Fig. 18: 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")
6 Operation
6.1 Initial start-up
6.2 Preparation
The ice condenser chamber must be clean and dry.
Remove any water residues from the preceding run.
Close the aeration valve and the media drain valve.
Ensure that all of the valves of the accessories are closed.
Switch the vacuum pump on.
6.3 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 ­"Safety")!
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6.4 LSCbasic control system
The control system LSCbasic (Lyo Screen Control basic) was specifically developed for the control of freeze-drying processes. The clear user interface enables the intuitive operation of the unit.
Fig. 19: Start screen of the LSCbasic control unit (example)
6.4.1 User interface
The system is operated via a touch panel, i.e. by touching the buttons on the display. Every button is marked by a frame. Pressing the button activates the associated function. Depending on the function, a dialogue box opens, a value can be changed, or a transaction can be confirmed.
Fig. 20: User interface LSCbasic
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1 Status line 2 Schematic system
diagram
3 Value windows 4 Button "Tools" 5Button "Set" (set
values)
6 Button "Process
and equipment messages"
7 Button "Operating
mode: select/start"
8 Button "Stop"
The user interface is divided into three main windows that can be called up by touching the corresponding buttons:
Process
This window is also the standard user interface. It is used to control the freeze-drying process manually.
Options
This window is used for personalised settings that enable the users to adapt the system as far as possible to their respective area of activity.
?
In this window, the users can find all of the relevant information concerning the control system at a glance. In the event of enquiries at the factory, these data facilitate the assignment and expediting of the processing of the enquiries.
6.4.1.1 Main window "Process"
This main window shows all of the relevant process data. Here, the individual phases of a freeze-drying process can be controlled manually.
...
Fig. 21: Overview of the main window "Process"
Status line (1)
This line shows the operating status of the freeze-dryer as well as the active phase.
The status line also shows the current date and time. The clock is battery­buffered and must be reset after a failure (chapter 6.4.1.2 - "Main window "Options"", section "Administration").
In addition, the drive symbol provides information concerning the status of the external data storage device or of the network drive. The following symbols are possible:
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No
symbol
No USB storage device or LAN network connected
USB storage device connected
Active process recording on a USB storage device
Network available, but no network drive connected
Network drive connected (e.g. LyoLogplus)
Network drive connected and active process recording
Button "Schematic system diagram" (2)
The left side of the user interface shows a schematic view of the system including all of its components. Active components are displayed in green. Touching a component calls up its name and reference designation.
Fig. 22: Schematic system diagram with the name and reference designation of the component
Value windows (3)
This area shows the current process data. The three value windows can be configured as desired.
Select the button of the value window that is to be adapted. A dialogue box with the possible parameters opens:
– Total time (duration of the entire freeze-drying process up to this
moment)
Section time (duration of the current section up to this moment) Ice condenser (temperature of the ice condenser) Vacuum (value of the vacuum inside the ice condenser chamber) Temperature vacuum (conversion of a vacuum value into a
temperature value based on the vapour pressure curve for ice and water)
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Fig. 23: Dialogue box "Select actual value"
Select the desired configuration or exit the dialogue box by pressing the "return" button.
In this way, it is possible to configure a personalised overview of the actual values.
Dialogue box "Tools" (4)
This dialogue box is used to call up various aids and resources.
Vapour pressure curve for ice and water A diagram shows the relationship between the pressure and sample
temperature. The pressure and temperature values can be changed by way of the buttons or by moving the arrows (see item 1 in the screenshot). The other value will be adapted automatically.
Fig. 24: Dialogue box “Vapour pressure curve for ice and water”
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1
Option: USB process recording (see chapter 6.5 - "Optional extensions")
Select the "USB process recording" function in the dialogue box "Tools".
Select the input fields ("Batch data"). A keyboard for the data input will
be displayed.
If necessary, select the "Options" tab, choose between manual or automatic recording, and define a recording interval.
Press the "return" button in order to close the dialogue box.
The process recording will now run in the background.
Fig. 25: Dialogue box "USB process recording"
Option: Lifting hoist1 (see chapter 6.5 - "Optional extensions") This function is described in the separate operating manual of the lifting
hoist.
Button "Set" (5)
This button is used to enter the set values for the individual phases of the freeze-drying process prior to the start of the process. Value ranges have been saved for the various phases. These value ranges can be displayed in the input window with the aid of the buttons "min" or "max" (see chapter
6.4.2.1 - "Entering set values").
Dialogue box "Process and equipment messages" (6)
This dialogue box is used to view and save all of the error messages and
other messages. In the event of an error or message, the window “Process
and equipment messages” will open automatically. In addition, a sound
signal is emitted until the error is acknowledged.
Not available for Alpha 3-4 LSCbasic
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1 The fault has been
eliminated, but the message has not been acknowledged yet
2 The fault has not be
eliminated and the message has not been acknowledged yet
3 The fault has not
been eliminated yet, but the message has been acknowledged
There are three categories of faults:
Red: error messages
Orange: process messages
Yellow: general messages
The representation of the message provides information about its current status. A double frame around a message means that the error has not been eliminated yet. The colour of the button "quit" changes from blue to grey once the message has been acknowledged.
Fig. 26: Representation of an error message
The advantage of this system is that faults that occurred during the night can be discovered the next day even if the cause of the fault has already been eliminated.
The dialogue box cannot be quit until all of the messages have been acknowledged.
If a message has been acknowledged even though the fault has not been eliminated, the button "Process and equipment messages" will be displayed in the respective colour of the fault in the main window.
Fig. 27: Dialogue box "Process and equipment messages
Details Tapping the message displays details concerning the error message:
Cause of the message
Effects of the message
Measures to eliminate the error
Reference designation
Error counter (indicates how often this error has occurred) and the time
stamp of the last error message.
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NOTE
The error message text is always followed by an error code. Always indicate the error code in the event of enquiries or service requests!
4Error message 5Error code 6Detailed information 7Error counter and
time stamp of the last error
8Arrow buttons
NOTE
The texts of the process and error messages are not included in this operating manual.
The associated documents can be requested from our service department.
Use the arrow buttons to open the individual windows.
Fig. 28: Details concerning an error message
Dialogue box "Operating mode: select/start" (7)
After the set values have been entered for the process, the process can be started with this function (see chapter 6.4.2 - "Starting a freeze-drying process").
Fig. 29: Dialogue box "Operating mode: select/start" (The version of the dialogue box that is displayed depends on the equipment of the freeze-dryer.)
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NOTE
Prior to performing a test, ensure that the chamber is dry and unloaded and that the ice condenser is defrosted!
Button "Standard unit test" Apart from the process phases of the freeze-drying process ("Freezing",
"Warm-up", "Main drying" and "Final drying") and the operating mode "Defrosting", the button "Standard unit test" is also available. This button opens a selection of tests with fixed parameters. After consultation with the manufacturer, these tests can be performed in order to check the functionality and processes of the freeze-dryer.
Fig. 30: Dialogue box "Standard unit test"
Performance test (1)
This test is used to determine the following performance parameters of a freeze-dryer:
vacuum decrease rate
final vacuum
minimum ice condenser temperature
Procedure:
In the main window "Process", select the button "Standard unit test" under "Operating mode: select/start".
Select "Performance test" and start the test via the "Run" button.
The test will be performed. The parameters will be measured at defined points of time, evaluated, and displayed in a dialog box (see the following illustration).
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Fig. 31: Results of the performance tests
Evaluation: Please contact Martin Christ Gefriertrocknungsanlagen GmbH for an
assessment of the results.
Option: Leakage test (2)
The leakage test is used to test the chamber of the freeze-dryer for tightness in view of any gaseous or liquid media. Since absolutely tight components simply do not exist, a leak rate is determined.
Procedure:
In the main window "Process", select the "Set" button to open the dialogue box "Set values: view/edit". Then, select the button "Leakage test".
Enter the test time (value between 10 min and 18 h) and chamber volume (see the technical data), accept the entries and return to the main window.
In the main window "Process", select the button "Standard unit test" under "Operating mode: select/start".
Select "Leakage test" and start the test via the "Run" button.
The parameters for the leakage test have been developed by Martin Christ Gefriertrocknungsanlagen specifically for the freeze-dryers. In a first step, these parameters (vacuum, ice condenser temperature) must be reached. It is not until the conditions are fulfilled that the pressure control valve closes. Then, the actual leakage test is performed in a second step. The result will be indicated by way of a dialogue box.
Evaluation: The leak rate that is calculated after the test provides information
concerning the tightness of the system. If the threshold value is not reached, the test has been passed. If it is exceeded, the test has been failed.
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Button "Stop" (8)
Pressing this button stops the current process. The freeze-dryer switches to standby.
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"General" options:
1"Language" 2"Scale unit" 3"Freeze-drying
process"
6.4.1.2 Main window "Options"
The main window "Options" is where the basic configuration of the control system is defined. It enables the optimum adaptation of the freeze-dryer to its specific area of application.
General
Fig. 32: Overview of the main window "Options/General"
Language (1) The control system can be used in several languages which can be
selected via the dialogue box.
Fig. 33: Dialogue box "Change language"
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NOTE
This function depends on the type of freeze-dryer and is not available for all types.
2 3
Scale unit (2) This dialogue box is used to change the unit of measurement for the
temperature and vacuum values.
Fig. 34: Dialogue box "Change scale unit"
Freeze-drying process (3)
Prior to the start of the process, the correct process must be selected. The following processes are available:
Cold trap operation2: Use of the freeze-dryer as a cold trap
Double-chamber method (outside): Drying outside the ice condenser
chamber
Double-chamber method LyoCube3: Drying outside the ice condenser chamber, but with the CHRIST LyoCube (a rectangular drying chamber that can be loaded from the front)
Not available for Alpha 3-4 LSCbasic. Not available for Alpha 3-4 LSCbasic.
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"Administration" options:
1"Date/Time" 2 "Network" 3 "System
properties"
4 "Access
protection"
5 "Device options"
Fig. 35: Dialogue box "Freeze-drying process"
Administration
Fig. 36: Dialogue box "Options" / "Administration"
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NOTE
The changes will not become effective until after a restart of the freeze­dryer.
Date/Time (1) The control system is equipped with an integrated, battery-buffered clock.
After a failure of the buffer battery, the date and time must be reset.
Fig. 37: Dialogue box “Change date/time
Network (2) This dialogue box is used to change the network settings.
Fig. 38: Dialogue box "Change network settings"
System properties (3) This dialogue box is used to change the system settings.
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Fig. 39: Dialogue box "System properties"
Beeper: The beeper sounds in the event of a malfunction, for example.
If the setting is "On", the beeper sounds at intervals of a few seconds until the message is acknowledged.
If the setting is "Silent", the beeper sounds once when the malfunction occurs.
If the setting is "Off", the beeper will not sound at all.
Click on touch: If this function is active, a clicking sound can be heard whenever the system registers that a button has been touched.
Behaviour of the pressure control valve in the case of insufficient ice condenser cooling: If this function is active (button "closed"), the pressure
control valve will close at an ice condenser temperature of ≥ 20°C during the drying process in order to avoid damage to the vacuum pump caused by the withdrawal of condensable gases. Selecting the button again deactivates the function (button "controlled").
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NOTE
The other buttons cannot be activated unless the access protection is active.
Access protection (4) In this dialogue box, the access rights can be managed on several levels
and they can be protected with a password. In the factory setting with activated access protection, data can be viewed
but not edited.
Fig. 40: Dialogue box "Access protection"
Password timer runtime: In order to prevent unauthorised access, the
system will automatically switch back to the default setting after a pre­defined period of time.
In this case, there is a small lock symbol in the status line and below this symbol the remaining time until the lock will be active is counted down. At the same time, a button with a big lock symbol will be displayed under the status line.
Fig. 41: Countdown of the password timer and the button with the lock symbol
The button with the lock symbol blocks any access immediately and the system switches to the default setting.
Fig. 42: Access blocked, data editing not possible
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Action
Operator
Service
Administrator
Editing of the data of the current process run (e.g. selection of the operating mode, changing of set values)
Editing of maintenance functions (e.g. oil change of the vacuum pump)
--
Editing of the default settings (e.g. editing of the access protection configuration, creating and editing of programs, editing of system settings)
--
--
NOTE
The changes will not become effective until after a restart of the freeze­dryer.
Operator/maintenance/administrator password: For each of these access levels, certain editing rights have been defined. They can be enabled with the corresponding password.
The rights of the various access levels are detailed in the following table.
Device options (5) This dialogue box lists all of the device options that are available for the
freeze-dryer in question. A list of all the possible options can be found at chapter 6.5 - "Optional extensions". Options that require a series-number­specific release code are marked with the symbol " ".
Fig. 43: Dialogue box "Device options" (example)
If the freeze-dryer is to be extended by an option, this option must be enabled via this dialogue box.
Select the button "Add option". An input window opens.
Enter the six-digit CHRIST activation code that was supplied for this
option. Note that the code is case-sensitive.
Options can be removed in the same way.
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"Service" options:
1"Operating hours" 2 "Failure memory" 3 "Vacuum pump
oil change"
4 "Maintenance" 5 "Sensor
adjustment"
Service
Fig. 44: Dialogue box "Service" (varies depending on the type of freeze-dryer)
Operating hours (1) This dialogue box is used to view the number of operating hours of the
various components of the freeze-dryer, e.g. the refrigeration unit, vacuum pump or pressure control valve. In addition to the name, the respective reference designation is also displayed.
These data are provided for informational purposes only. They cannot be edited.
Fig. 45: Dialogue box "Operating hours" (here: refrigeration unit 1.1)
Failure memory (2) The failure memory stores the most recent messages of the process and
equipment information system. The messages can be viewed in this dialogue box. The failure memory includes the last 32 messages. If this number is exceeded, the oldest message will be overwritten.
Use the arrow keys to select the individual messages. The error message text is always followed by an error code.
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NOTE
Always indicate the error code in the event of enquiries or service requests!
Fig. 46: Dialogue box "Failure memory"
Vacuum pump oil change (3) The system monitors the oil change interval of the vacuum pump. The
interval can be adapted to the vacuum pump model and utilisation. When the end of an oil change interval is reached, a corresponding
message will be displayed.
Acknowledge the message.
Change the oil of the vacuum pump.
Reset the operating hour counter in the dialogue box "Vacuum pump oil
change" by way of the "reset" button.
Fig. 47: Dialogue box "Vacuum pump oil change"
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CAUTION
Sensors that are not properly adjusted will lead to incorrect measurements which, in turn, will have a negative effect on the process control.
NOTE
Only specialised personnel are authorised to perform the sensor adjustment.
Maintenance (4) The maintenance interval of the freeze-dryer is set at 3,000 operating hours
or at least one maintenance per year. When the end of a maintenance interval is reached, a corresponding
message will be displayed.
Acknowledge the message.
Make an appointment for the maintenance of your freeze-dryer.
After the maintenance, our service engineer will reset the operating
hour counter in the dialogue box "Maintenance".
Fig. 48: Dialogue box "Maintenance"
Sensor adjustment (5) In this dialogue box, the sensors are adjusted based on a predefined
reference value.
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1 Freeze-dryer type 2 Control system type 3 Serial number 4 Manufacturer contact
data
5 Details concerning the
software version
NOTE
In the event of enquiries at the manufacturer, please state the data that is stated here.
NOTE
Prior to any freeze-drying process, the correct method must be selected (chapter 6.4.1.2 - "Main window "Options"", "Freeze-drying process (3)").
NOTE
If the freeze-drying process is to be started directly with the "Main drying" phase, the vacuum pump must be warmed up approximately 15 minutes prior to the process start. Failure to do so will result in a corresponding warning message when the process starts.
6.4.1.3 Main window "?"
This main window includes the most important information concerning your freeze-dryer:
Fig. 49: Freeze-dryer system information (example)
6.4.2 Starting a freeze-drying process
Freeze-drying processes are started in the main window "Process".
The set values for the individual process phases ("Freezing", "Warm-up", "Main drying" and "Final drying") are defined prior to the start of the process (see chapter 6.4.2.1 - "Entering set values"). Then, the freeze­drying process can be started via the dialogue box "Operating mode: select/start".
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NOTE
If the value "∞" (infinite) is selected for a process phase, the next phase
must be started manually via the button "Operating mode: select/start".
The set values of the active phase can be changed during the process run. In this case, the control system adapts the freeze-dryer to the new set values as quickly as possible.
After the completion of a phase, the freeze-dryer switches to the next phase without switching to standby. The transition from "Freezing" to "Warm-up" takes place automatically. After the completion of the "Warm­up" phase, a dialogue box opens:
Fig. 50: Dialogue box after the completion of the warm-up phase
The freeze-dryer will remain in the "Warm-up" phase until a confirmation is issued.
Normally, the transition from "Main drying" to "Final drying" takes place automatically.
After the completion of the "Final drying" phase, there will be another enquiry with which the freeze-drying process will be completed. The freeze­dryer remains in the "Run" mode until the enquiry is confirmed.
The process can be stopped any time by way of the "Stop" button. In this case, the freeze-dryer will be switched to standby.
6.4.2.1 Entering set values
The system has stored set values for every phase, and for every value there are pre-defined value ranges that can be determined in the various dialogue boxes by pressing the buttons "min" and "max".
In order to protect the product, a safety pressure value can be entered in every drying section.
Viewing or editing the set values:
Press the button "Set" (see chapter 6.4.1.1 - "Main window "Process""). The following dialogue box will be displayed:
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1 "Defrosting" button 2"Leakage test" button
(option)
1Set value display 2Button for changing the
sign (e.g. when entering
temperature values) 3"" (infinite) 4Button for editing the
value in pre-defined
steps 5Selection of a possible
maximum or minimum
value 6Input of a value via the
numerical keypad 7Button for deleting the
displayed value
NOTE
If the dialogue box is closed by the button "return", the changes will be discarded.
Fig. 51: Dialogue box "Set values: view/edit"
Fields that are displayed in the form of buttons can be edited.
Defrosting (1) This button is used to pre-define the defrosting time and temperature.
Leakage test (2) This button displays the parameters that are used for the leakage test. In addition, the test time and the chamber volume must be stated (depending on the accessories that are used).
Numerical values can be edited with the aid of a numerical keypad:
Fig. 52: Editing set values
Confirm the new value and quit the numerical keypad by pressing the button "Accept".
Confirm the input and quit the dialogue box via the button "Accept".
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6.5 Optional extensions
The basic unit is extendable with the following optional functions:
Leakage test
see also chapter 6.4.2.1 - "Entering set values" and chapter 6.4.1.1 - "Main window "Process"", dialogue box "Operating mode: select/start" (7), button "Standard unit test"
The leakage test enables the chamber of the freeze-dryer to be tested for tightness in view of any gaseous or liquid media. Since absolutely tight components simply do not exist, a leak rate is determined. The parameters for the leakage test have been developed by Martin Christ Gefrier­trocknungsanlagen specifically for freeze-dryers. In a first step, these parameters (vacuum, ice condenser temperature) must be reached. It is not until the conditions are fulfilled that the pressure control valve closes. Then, the actual leakage test is performed in a second step. The leak rate that is calculated after the end of the test provides information concerning the tightness of the system.
USB process recorder
see also chapter 6.4.1.1 - "Main window "Process"", dialogue box "Tools" This feature enables the recording of a running process on a USB storage
medium. After the end of the process recording, the process data can be viewed on the PC with LyoLogplus and be printed. It is also possible to import the data directly into an Excel file.
LyoLogplus data logging software
LyoLogplus is a data logging software program by Martin Christ Gefriertrocknungsanlagen GmbH that is specifically adapted to the requirements of freeze-drying processes. Apart from the graphical representation of the measurement data of currently running processes, it
also enables the data export for additional evaluation.
6.6 Switching the freeze-dryer OFF
The freeze-dryer must be in the standby status.
Switch the freeze-dryer off by pressing the mains switch.
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Type of error
Possible reason
Correction
No indication on the display
No power in the mains supply (see chapter 7.1.1 - "Power failure").
Power cord is not plugged in.
Fuses have tripped.
The mains power switch is set
to off.
Check the mains power supply fuse.
Plug in the power cord correctly.
Check the on-site fuses
Switch mains power switch ON.
The touchpanel does not react at all or it does not react correctly
The sensitivity of the touchpanel is misadjusted.
Contact the service department (see chapter 7.3 - "Service contact")
The password input fails
The password is not correct.
Inform the administrator.
If you have lost the administrator
password: contact the service department (see chapter 7.3 ­"Service contact")
Insufficient vacuum
Incorrect connection of the small flange connection(s).
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.
Dirty or damaged lid or door seal.
Clean the lid or door seal and replace it if necessary.
The ground-in stopper of the attached drying chamber is not installed correctly.
Grease the ground-in stopper evenly and over the entire sealing surface with vacuum grease.
Leakage in the media drain valve
The media drain valve is soiled with drying residues or wool particles from cleaning cloths.
The O-rings are worn
Clean the media drain valve (see
chapter 8.1.3 - "Aeration valve, media drain valve")and replace it if necessary.
Replace the O-rings.
Leakage in a rubber valve
The valve is soiled.
Check the valves individually
(see chapter 7.1.2.4 - "Rubber valves")
7 Malfunctions and error correction
Malfunctions are displayed in the dialogue box "Process & equipment messages" (see chapter 7.2 - "Process and error messages"). An acoustic signal sounds when an error message is generated.
Eliminate the source of the problem (see the following chapter).
7.1 General malfunctions
Acknowledge the error message.
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Type of error
Possible reason
Correction
The displayed vacuum value is not correct
Incorrect calibration
The vacuum sensor is soiled
(e.g. due to water residues)
The vacuum sensor is defective.
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"
The vacuum pump is not activated
See the separate operating instructions of the vacuum pump.
See the separate operating instructions of the vacuum pump.
Insufficient ice condenser or shelf temperature
The overpressure switch of the refrigeration unit has tripped.
The thermal circuit breaker has tripped.
Let the unit cool down.
Ensure sufficient air circulation
(see chapter 7.1.3 - "Insufficient ice condenser temperature")
During the start, the error message "Refrigeration unit 1.2 overpressure" is displayed
Excessive ambient temperature
Longer period of non-utilisation
of the freeze-dryer
Decrease the ambient temperature.
Acknowledge the message. If the message is displayed repeatedly, inform the service department (see chapter 7.3 ­"Service contact")
NOTE
If it is impossible to eliminate the errors, contact the Christ service department!
7.1.1 Power failure
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.
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NOTE
The vacuum checks must be carried out when the ice condenser is frozen.
Fig. 53: Small flange and centring ring
Fig. 54: Small flange with centring ring and small flange
Fig. 55: Attaching the clamping ring
Fig. 56: Tightened clamping ring
7.1.2 Insufficient vacuum
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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NOTE
The inspection of the valve must be carried out by qualified specialist personnel (see chapter 7.3 - "Service contact").
7.1.2.2 Aeration valve, media drain valve
A malfunction of the aeration valve or the 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 8.1.3 - "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
specialist personnel (see chapter 7.3 - "Service contact").
7.1.2.3 Pressure control valve
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.
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.
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 pump are OK.
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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.
7.1.3 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 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. -105°C is reached when the ice condenser is not loaded and the ice condenser chamber is
evacuated.
7.2 Process and error messages
The control system displays the complete process and error messages (see chapter 6.4.1.1 - "Main window "Process"", dialogue box "Process and equipment messages"), which is why they are not included in this operating manual.
You can order these documents from our service department.
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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: support.lab@martinchrist.de
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 manufacturercannot be held liable or subject to any warranty claims.
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
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).
8.1 Maintenance
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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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
moisture can evaporate.
Cleaning the drying chamber and the cover
In case of a contamination with toxic, radioactive or pathogenic
substances, clean immediately with a suitable decontamination agent.
Clean immediately after use at a low temperature, with a short
application time and low alkalinity.
Do not use cleaning agents with abrasive particles.
Do not use abrasive sponges for cleaning.
Avoid longer periods of application of strongly alkaline media at more
than 70°C.
Avoid strong mechanical stress during cleaning.
8.1.2 Ice condenser chamber
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.
8.1.3 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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1Valve opening 2Valve core 3O-rings
Fig. 57: 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").
8.1.4 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 (see chapter 7.3 - "Service contact").
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NOTE
Please refer to the separate operating manual of the vacuum pump!
NOTE
Please refer to the separate operating manual of the vacuum pump and the exhaust filter!
8.1.5 Vacuum pump
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,
Check the running pump for any unusual noise.
Ensure that the pump has reached its operating temperature prior to
Perform the first oil change after approximately 100 operating hours.
The other oil changes depend on the operating conditions. In general,
Please contact the Christ service department if you have any queries
top it up with oil.
changing the oil.
an interval of 500 to 1,000 operating hours is sufficient.
(see chapter 7.3 - "Service contact").
8.1.6 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
provided by the manufacturer in the separate operating manual).
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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.
8.1.7 Vacuum sensor
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.
8.1.8 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.
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 preferably after each use.
Use only the accessories that have been specified by Martin Christ
Gefriertrocknungsanlagen GmbH.
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DANGER
If dangerous materials (e.g. infectious and pathogenic substances) are used, the freeze-dryer and accessories must be disinfected.
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.
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
8.3 Service
contact").
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: support.lab@martinchrist.de
Outside Germany:
Contact our agency in your country. All agencies are listed at www.martinchrist.de [Sales Partners]
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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.
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)
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 specialist 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 www.martinchrist.de [Service] [Overhaul, repair and leak testing].
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9 Disposal
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.
Comply with all local rules and regulations.
9.2 Disposal of the packaging
Dispose of the packaging, after having separated the individual materials.
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 3-4 LSCbasic
Part number
102394, 102395
Performance data
Ice condenser
- capacity
- performance
- temperature
- chamber volume
4 kg max
2.5 kg / 24 h max approx. –105°C approx. 11 l
Max. shelf surface area ( double chamber method): drying outside the ice condenser chamber
3 shelves, Ø 200 mm each A
total
=0.094m2
drying in round bottom flasks
12 pieces
Connection requirements (without vacuum pump and accessories)
Electrical connection:
1 x 230 V / 50 Hz (other supply data on request)
Protection class:
I
IP protection category according to DIN 60529:
11
Apparent power:
1.8 kVA
Nominal current:
8.0 A
Mains fuse:
12 A
Pressure control valve connection:
230 V, 50/60 Hz, 20 VA max.
Vacuum pump connection:
230 V, 50/60 Hz, 4.0 A max.
Filling quantity
Flammable refrigerants:
- R1270:
- R1150:
Filling quantity CO2 equivalent 108 g < 0,01 t
60 g < 0,01 t
Physical data (without vacuum pump and accessories)
Dimensions
- height
- width
- depth
415 mm 780 mm 555 mm + 80 mm vacuum connection
Weight
approx. 86 kg
Noise level according to DIN 45635
54 dB(A)
EMC according to EN 55011
Class B
Heat emission
1.3 kW min
1.7 kW max
10 Technical data
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Equipment connections
Vacuum connection
Small flange connection DN25KF (ISO 28403, DIN 2861)
Media drain valve
Hose nozzle DN10 (outside diameter 12 mm)
Aeration valve
Hose nozzle DN6 (outside diameter 10 mm max.)
Vacuum sensor
SUB D-9
Option: data interface (LAN)
RJ 45
Special equipment: water cooling system
Cooling water consumption
max. 0.24 m3/h
Heat carried off via the cooling water
1.7 kW
Cooling water feed flow connection
R3/4" with hose nozzle DN13
Cooling water return flow connection
R3/4" with hose nozzle DN13
10.1 Umgebungsbedingungen
10.1 Ambient conditions
10.1 Umgebungsbedingungen
The figures are valid for an ambient temperature of +20°C.
Allowable ambient temperature +10 °C to +25 °C.
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 (e.g. for refrigerant) is not attached to this operating manual.
You can order these documents from our service department.
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11 Appendix
11.1 EC declaration of conformity in accordance with the EC Machinery Directive
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12 Glossary
Cold trap operation
Cold traps are used for the condensation of moisture or solvents in combination with vacuum pumps. CHRIST freeze-dryers can be used as cold traps.
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.
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 pressure increase test for determining the end of the drying process. In freeze-dryers without active shelf cooling, the samples need to be prefrozen externally, e.g. in a deep­freeze or freezer cabinet. After the transfer of the product into the freeze­dryer, the actual sublimation is started.
Eutectic point
The eutectic point is the point at which a homogeneous 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.
Reference designation
Within the life cycle of industrial systems, a uniform equipment identification system is required for planning, design, implementation, operation, maintenance and dismantling so that all of the objects within the system can be clearly identified at any time. The reference designations (also known as device tags) are affixed to the equipment or components and entered into the technical documents (e.g. circuit diagram).
Safety pressure
Since the vacuum has a dominating influence on the product temperature, Martin Christ Gefriertrocknungsanlagen GmbH has integrated a safety pressure feature into the freeze-dryers in order to ensure the protection of the product. If the pressure inside the drying chamber increases too strongly so that it exceeds the safety limit, the energy supply of the shelves will be interrupted and the sublimation process slows down. This prevents the product from melting.
The safety pressure value that is entered should correspond to a temperature value that is 5°C below the melting point of the product on the vapour pressure curve for ice and water.
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Single-chamber method
(not available for freeze-dryers with an LSCbasic control system) With the single-chamber method, the freezing as well as the subsequent
drying of the product take place inside 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 single-stage systems or -85°C in the case of double­stage systems). During this process, the inside of the chamber can be cooled down to approx. -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.
Sublimation
Sublimation (from Latin "sublimis" = high up in the air, raised) is a thermodynamic process of the direct transition of a substance from the solid phase to the gas phase.
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13 Index
A
Access protection....................................... 60
Accessories ......................................... 30, 79
Accessories (installation) ........................... 41
Accident prevention ................................... 24
Acids .......................................................... 29
Acids (hazards) .......................................... 27
Administration ............................................ 57
Aeration ............................................... 35, 66
Aeration valve ...................................... 36, 84
Aeration valve (cleaning and care) ............. 76
Aeration valve, malfunction ........................ 72
Ambient conditions ..................................... 84
Ambient temperature ........................... 35, 84
Anschluss für Vakuummesssonde ............. 14
Anschluss Vakuummesssonde .................. 14
Apparent power ................................... 14, 83
B
Beeper ....................................................... 59
Behaviour of the pressure control valve in the
case of insufficient ice condenser cooling
............................................................... 59
Belüftungsventil ......................................... 13
Button "Standard unit test" ......................... 52
Button "Stop" ............................................. 54
C
CE mark in compliance with the directive
2006/42/EC ............................................ 21
Changing of operating supplies .................. 29
Chemical reactions .................................... 79
China RoHS 2 – Declaration of conformity . 87
Circuit diagram ........................................... 84
Cleaning .................................................... 29
Cleaning agents ................................... 75, 80
Cleaning of the freeze-dryer ....................... 76
Cleaning the freeze-dryer and the
accessories ............................................ 75
Click on touch ............................................ 59
Cold trap operation .................................... 56
Condensate, contaminated (hazards) ........ 28
Connection................................................. 36
Connection (hazards) ................................. 26
Connection requirements ........................... 83
Contaminated condensate (hazards) ......... 28
Contaminated defrosting water (hazards) .. 28
Control system type ................................... 65
Cooling system ................................ .......... 84
Copyright ................................................... 10
Corrosion ............................................. 75, 79
Cost estimate ............................................. 81
Cracks ....................................................... 79
Customer-provided fuses ........................... 36
D
Dangerous materials .................................. 80
Data interface (LAN) .................................. 84
Date/Time .................................................. 58
Declaration of conformity – China RoHS 2 . 87 Declaration of conformity (Machinery
Directive) .......................................... 10, 85
Declaration of conformity (Pressure
Equipment Directive) .............................. 89
Declaration of decontamination .................. 81
Decontamination agents ............................ 80
Defrosting ............................................ 20, 66
Defrosting water, contaminated (hazards) .. 28
Defrosting with hot gas............................... 20
Desorption ................................................. 91
Details ........................................................ 50
Details concerning the software version ..... 65
Device options ........................................... 61
Device tag .................................................. 91
Dialogue box "Operating mode: select/start"
............................................................... 51
Dialogue box "Process and equipment
messages ............................................... 49
Dialogue box "Schematic system diagram" 47
Dialogue box "Tools" .................................. 48
Dimensions .......................................... 32, 83
Direct hazard to the life and health ............. 22
Disinfectants .............................................. 80
Disinfection of the drying chamber and
accessories ............................................ 80
Displayed vacuum value is not correct ....... 70
Disposal of the freeze-dryer ....................... 82
Disposal of the packaging .......................... 82
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Double-chamber method ...................... 56, 91
Double-chamber method LyoCube (outside)
............................................................... 56
E
Earth conductor check ............................... 28
EC declaration of conformity (Machinery
Directive) .......................................... 10, 85
EC declaration of conformity (Pressure
Equipment Directive) .............................. 89
Electrical connection .................................. 83
Electricity (hazards) ................................... 26
EMC according to EN 55011 ...................... 83
Entering set values .................................... 66
Environmental protection ........................... 24
Equipment connections .............................. 84
Equipotential bonding screw ................ 28, 36
Error correction .......................................... 69
Error messages ......................................... 28
Eutectic point ............................................. 91
Exhaust filter .............................................. 78
Explanation of symbols .............................. 10
Explanation of the symbols and notes ........ 22
External data storage device ...................... 46
F
Failure memory .......................................... 62
Filling quantity ............................................ 83
Final drying ................................................ 19
Form for the return of defective parts ......... 81
Freeze-dryer type ....................................... 65
Freeze-dryer, cleaning and care ................ 76
Freeze-drying phases ................................ 17
Freeze-drying process ......................... 18, 56
Freeze-drying process, start ...................... 65
Funktions- und Bedienelemente ................. 12
G
General conditions ................................ ..... 10
General information on freeze-drying ......... 15
General malfunctions ................................. 69
General work (maintenance) ...................... 75
H
Hazard warnings .................................... 9, 10
Hazards (acids) .......................................... 27
Hazards (connection) ................................. 26
Hazards (contaminated condensate).......... 28
Hazards (contaminated defrosting water) ... 28
Hazards (electricity) ................................... 26
Hazards (general, transport to
commissioning) ...................................... 25
Hazards (products, harmful) ....................... 27
Hazards (refrigeration system) ................... 27
Hazards (set-up) ........................................ 25
Hazards (surfaces, cold) ............................ 28
Hazards (surfaces, hot) .............................. 28
Hazards (transport) .................................... 25
Health and safety rules and regulations and
regulations for the prevention of accidents
............................................................... 23
Heat emission ............................................ 83
Heat exchanger ......................................... 77
Hot-gas defrosting ...................................... 20
I
Ice condenser ............................................ 83
Ice condenser chamber.............................. 12
Ice condenser chamber, cleaning and care 76
Importance of the operating manual ............. 9
Important information ................................. 22
Infectious substances ................................ 80
Informal safety notes .................................. 24
Initial start-up ............................................. 44
Inspection by the manufacturer .................. 80
Installation of accessories .......................... 41
Insufficient ice condenser or shelf
temperature ............................................ 70
Insufficient ice condenser temperature ....... 73
Insufficient vacuum .............................. 69, 71
Intended use ................................................ 9
IP protection category according to DIN
60529 ..................................................... 83
L
Language ................................................... 55
Layout of the freeze-dryer .......................... 12
Leakage in a rubber valve .......................... 69
Leakage in the media drain valve ............... 69
Leakage test .................................. 53, 66, 68
Location of use .......................................... 35
LSCbasic control system ............................ 45
Lyes ........................................................... 29
LyoLogplus data logging software .............. 68
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M
Main drying ................................................ 19
Main window "?" ......................................... 65
Main window "Options" .............................. 55
Main window "Process" .............................. 46
Mains fuse ................................................. 83
Maintenance ........................................ 29, 64
Maintenance (general work) ....................... 75
Maintenance (vacuum sensor) ................... 79
Maintenance and service ........................... 75
Malfunction of the pressure control valve ... 72
Malfunctions ............................................... 69
Manufacturer ............................ 75, 80, 82, 83
Manufacturer contact data ......................... 65
Marking of the unit ..................................... 21
Max. humidity ............................................. 84
Maximum current for the vacuum pump ..... 39
Media drain ................................................ 66
Media drain valve ................................. 37, 84
Media drain valve (cleaning and care) ........ 76
Media drain valve, malfunction ................... 72
Medienablaufventil ................................ ..... 13
Mode of operation ...................................... 15
N
Name plate .......................................... 14, 36
Network ..................................................... 58
Network drive ............................................. 46
Netzabsicherung ........................................ 14
Netzkabel ................................................... 14
No indication on the display ....................... 69
Noise level ................................................. 83
Nominal current ......................................... 83
Nominal voltage ................................... 14, 26
Notes on safety and hazards ....................... 9
Notes on transport ..................................... 33
O
Oil mist separator ....................................... 78
Operating hours ......................................... 62
Operating mode: select/start ...................... 51
Operating personnel .................................. 24
Operating state .......................................... 46
Operating voltage....................................... 36
Operational safety ...................................... 79
Operator/maintenance/administrator
password ................................................ 61
Option: Leakage test .................................. 53
Option: USB process recording .................. 49
Optional extensions ................................... 68
P
Packaging ............................................ 34, 82
Part number ......................................... 14, 83
Password input fails ................................... 69
Password timer runtime ............................. 60
Pathogenic substances ........................ 76, 80
Performance data ...................................... 83
Performance test........................................ 52
Physical data ............................................. 83
Potential hazard to the life and health ........ 22
Potentially hazardous situation................... 22
Power failure .............................................. 70
Power supply ............................................. 36
Preparation .......................................... 18, 44
Pressure control valve ............................... 40
Pressure control valve, malfunction ........... 72
Pressure marks .......................................... 79
Prevention of accidents ................................ 9
Procedures in the event of hazards and
accidents ................................................ 29
Process and equipment messages ............ 49
Process and error messages ..................... 73
Process data .............................................. 46
Products, harmful (hazards) ....................... 27
Protection class ......................................... 83
R
Radioactive substances ............................. 76
Rated current ............................................. 14
Reference designation ................... 50, 62, 91
Refrigerant ................................ ................. 83
Refrigerant data ......................................... 14
Refrigeration problems
Conditions at the location of use ............. 35
Refrigeration system (hazards) .................. 27
Remaining hazards .................................... 31
Responsibility of the operator ..................... 23
Return of defective parts ............................ 81
Rubber valves ...................................... 42, 72
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S
Safety and hazard notes ............................ 24
Safety data sheets ..................................... 84
Safety devices ........................................... 28
Safety distance .................................... 26, 35
Safety instructions .................................. 9, 10
Safety notes concerning set-up and
connection .............................................. 25
Safety notes concerning the initial start-up . 25
Safety notes concerning the operation ....... 26
Safety notes concerning the transport ........ 25
Safety pressure .......................................... 91
Scale unit (unit of measurement) ............... 56
Schematic system diagram ........................ 47
Scope of supply ......................................... 11
Sensor adjustment ................................ ..... 64
Serial number .......................... 14, 65, 74, 80
Serielle Schnittstelle ................................... 14
Service ................................................. 62, 80
Service contact ................................ .......... 74
Service life ................................................. 75
Service work .............................................. 80
Set process values ..................................... 49
Set-up (hazards) ........................................ 25
Set-up and connection ............................... 35
Signs of corrosion ...................................... 79
Single-chamber method ............................. 92
Small flange connections ........................... 71
Solvents ..................................................... 29
Solvents. .................................................... 75
Spannungsversorgung Drucksteuerventil ... 14
Spannungsversorgung Vakuumpumpe ...... 14
Special equipment:water cooling system ... 84
Specialist personnel ................. 72, 77, 80, 81
Standard unit test ....................................... 52
Standards and regulations ......................... 10
Starting a freeze-drying process ................ 65
Status line .................................................. 46
Storage ...................................................... 32
Storage and transport ................................ 32
Storage conditions ..................................... 32
Stress-corrosion ......................................... 79
Sublimation ................................................ 92
Supply voltage ........................................... 36
Surfaces, cold (hazards) ............................ 28
Surfaces, hot (hazards) .............................. 28
Switching the freeze-dryer OFF ................. 68
Switching the freeze-dryer on..................... 44
System check ............................................ 28
System properties ...................................... 58
T
Technical data ........................................... 83
Technical documentation ........................... 84
Thermal stress ..................................... 35, 75
Tools .......................................................... 48
Topping-up of operating supplies ............... 29
Touch panel ............................................... 13
Touchpanel ................................................ 13
Touchpanel does not react ......................... 69
Toxic substances ....................................... 76
Transport ................................................... 32
Transport (hazards) ................................... 25
Transport locking devices .......................... 34
Transport to commissioning (hazards,
general) .................................................. 25
Type..................................................... 14, 83
U
USB process recorder ................................ 68
USB process recording .............................. 49
User interface ............................................ 45
UV radiation ......................................... 35, 75
V
Vacuum connection ................................... 84
Vacuum pump ............................................ 39
Vacuum pump connection .......................... 83
Vacuum pump is not activated ................... 70
Vacuum pump oil change ........................... 63
Vacuum pump, cleaning and care .............. 78
Vacuum sensor .............................. 37, 72, 84
Vacuum sensor (maintenance) .................. 79
Vakuumanschluss ...................................... 14
Value windows ........................................... 47
Vapour pressure curve for ice and water ........
......................................................... 16, 48
Ventilation .................................................. 73
Vents ......................................................... 35
Viewing or editing the set values ................ 66
W
Wärmetauscher ......................................... 14
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Warranty and liability .................................. 10
Water cooling system ................................. 84
Weight ................................................. 32, 83
Y
Year of manufacture .................................. 14
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