Christ Alpha 3-4 LSCbasic User manual

Translation of the original operating manuel
sb-pe
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.: [phone] / 5007-0
Fax: [phone] / 5007-12
Web: www.martinchrist.de
E-mail: [e-mail]

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1General 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
2Layout 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
3Safety..................................................................................................................................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
4Storage 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
5Set-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
6Operation............................................................................................................................ 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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7Malfunctions 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
8Maintenance 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
9Disposal.............................................................................................................................. 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 AI2O3and 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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1.7 Scope of supply
Solvent package for round bottles (part no. 102394) includes:
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
Solvent package universal (part no. 102395) includes:
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
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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2 Layout and mode of operation

2.1 Layout of the freeze-dryer

2.1.1 Functional and operating elements
1Ice condenser
chamber
2LSCbasic user (see
chapter 6.4.1 - "User
interface")
3Mains power switch
Fig. 1: Total view of the freeze-dryer
4Pipe connection of the
vacuum sensor
5Pipe connection of the
vacuum pump (behind
the cover plate)
6Ice condenser
Fig. 2: Ice condenser chamber

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7Aeration valve
8Media drain valve
Fig. 3: Left side of the freeze-dryer
9Touchpanel
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
14Electrical connection of
the vacuum sensor
15Connection of the
vacuum sensor
16Power supply of the
pressure control valve
17Power supply of the
vacuum pump
18Mains fuse
19 Mains cable
20Equipotential bonding
screw
Fig. 5: Rear view of the freeze-dryer

2.1.2 Name plate
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

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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 high-
quality 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 deep-
freeze. 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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Fig. 8: Freeze-drying phases
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].

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
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
product.

2.2.2.1 PreparationThe 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.

2.2.2.2 Freezing 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 freeze-
drying process, the product temperature should be approximately 10°C
below the solidification point.
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.


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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 m3of vapour, at 0.1 mbar a
volume of 10 m3of 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.