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0% found this document useful (0 votes)
242 views111 pages

BA Alpha 1-2 LSCbasic 2022-07 1-0 en

Uploaded by

Asin
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 111

Translation of the original operating manual

sb-ja

Rev. 1.0 of 19/07/2022


Alpha 1-2 LSCbasic
Version 07/2022

Alpha 1-2 LSCbasic


part no. 101700, 101702, 101704

Freeze-dryer

Operating Manual

Please retain for later use!


Freeze-dryer Alpha 1-2 LSCbasic

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In case of inquiries, please state the following numbers:

Order number:

Serial number:

© Copyright by
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode am Harz
Germany
Tel.: +49 (0) 5522 / 5007-0
Fax: +49 (0) 5522 / 5007-12
Web: www.martinchrist.de
E-mail: [email protected]

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Table of contents

1 General information ............................................................................................................. 9


1.1 Importance of the operating manual.................................................................................. 9
1.2 Intended use ..................................................................................................................... 9
1.2.1 Freeze-drying of solvent-containing products (non-aqueous media) .......................... 10
1.2.2 Freeze-drying of acid-containing products ................................................................. 11
1.3 Warranty and liability....................................................................................................... 12
1.4 Copyright ........................................................................................................................ 12
1.5 Explanation of symbols ................................................................................................... 12
1.6 Standards and regulations .............................................................................................. 12
1.7 Scope of supply .............................................................................................................. 13
2 Layout and mode of operation .......................................................................................... 14
2.1 Layout of the freeze-dryer ............................................................................................... 14
2.1.1 Functional and operating elements ............................................................................ 14
2.1.2 Name plate ................................................................................................................ 16
2.2 Mode of operation ........................................................................................................... 17
2.2.1 General information on freeze-drying ......................................................................... 17
2.2.2 Freeze-drying process ............................................................................................... 19
2.2.2.1 Preparation ........................................................................................................ 19
2.2.2.2 Freezing ............................................................................................................. 20
2.2.2.3 Main drying ........................................................................................................ 20
2.2.2.4 Final drying ........................................................................................................ 21
2.2.2.5 End of drying and aeration ................................................................................. 21
2.2.2.6 Defrosting .......................................................................................................... 22
3 Safety .................................................................................................................................. 23
3.1 Marking of the unit .......................................................................................................... 23
3.2 Explanation of the symbols and notes ............................................................................. 24
3.3 Responsibility of the operator.......................................................................................... 25
3.3.1 Freeze-drying of solvent-containing products............................................................. 26
3.4 Requirements concerning the personnel ......................................................................... 26
3.5 Informal safety notes....................................................................................................... 27
3.6 Safety notes concerning the transport, set-up and connection and initial start-up of the
freeze-dryer .................................................................................................................... 28
3.6.1 General hazards ........................................................................................................ 28
3.6.2 Hazards caused by improper transport ...................................................................... 28
3.6.3 Hazards caused by improper set-up .......................................................................... 28
3.6.4 Hazards caused by improper connection ................................................................... 29

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3.7 Safety notes concerning the operation ............................................................................ 29
3.7.1 Hazards caused by electricity .................................................................................... 29
3.7.2 Hazards caused by the refrigeration system (natural, flammable refrigerants) ........... 30
3.7.3 Hazards caused by harmful products ......................................................................... 30
3.7.4 Hazards caused by solvents in the products .............................................................. 30
3.7.5 Hazards caused by acids in the products................................................................... 31
3.7.6 Hazards caused by contaminated condensate (defrosting water) .............................. 31
3.7.7 Oil-sealed vacuum pump: hazards caused by contaminated vacuum pump exhaust
gases ......................................................................................................................... 31
3.7.8 Oil-sealed vacuum pump: hazards caused by hot and contaminated vacuum pump oil
.................................................................................................................................. 32
3.7.9 Hazards caused by noise........................................................................................... 32
3.7.10 Hazards caused by hot surfaces ................................................................................ 32
3.7.11 Hazards caused by cold surfaces .............................................................................. 32
3.8 Safety devices ................................................................................................................ 33
3.8.1 System check ............................................................................................................ 33
3.8.2 Earth conductor check ............................................................................................... 33
3.9 Procedures in the event of hazards and accidents .......................................................... 33
3.10 Maintenance and cleaning of the freeze-dryer ................................................................ 34
3.11 Measures to be taken to ensure safe operation of the freeze-dryer................................. 34
3.12 Remaining hazards ......................................................................................................... 35
4 Storage and transport ....................................................................................................... 36
4.1 Dimensions and weight ................................................................................................... 36
4.2 Storage conditions .......................................................................................................... 36
4.3 Notes on transport .......................................................................................................... 37
4.4 Packaging ....................................................................................................................... 38
4.5 Transport safety device................................................................................................... 38
5 Set-up and connection ...................................................................................................... 39
5.1 Location of use ............................................................................................................... 39
5.2 Power supply .................................................................................................................. 40
5.2.1 Type of connection .................................................................................................... 40
5.2.2 Customer-provided fuses ........................................................................................... 40
5.3 Aeration and media drain valve ....................................................................................... 41
5.4 Vacuum sensor ............................................................................................................... 41
5.5 Vacuum pumps ............................................................................................................... 43
5.5.1 Oil-sealed vacuum pump and exhaust filter (oil mist separator) ................................. 43
5.6 Use of an interface box ................................................................................................... 44
5.7 Pressure control valve .................................................................................................... 47
5.8 Rubber valves ................................................................................................................. 48

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6 Operation............................................................................................................................ 49
6.1 Initial start-up .................................................................................................................. 49
6.2 Installation of accessories ............................................................................................... 49
6.3 Preparation ..................................................................................................................... 49
6.4 Switching the freeze-dryer on ......................................................................................... 49
6.5 LSCbasic control system ................................................................................................ 50
6.5.1 User interface ............................................................................................................ 50
6.5.1.1 Main window "Process" ...................................................................................... 51
6.5.1.2 Main window "Options" ...................................................................................... 59
6.5.1.3 Main window "?"................................................................................................. 69
6.5.2 Starting a freeze-drying process ................................................................................ 69
6.5.2.1 Entering set values ............................................................................................ 70
6.6 Optional extensions ........................................................................................................ 72
6.7 Switching the freeze-dryer OFF ...................................................................................... 72
7 Malfunctions and error correction .................................................................................... 73
7.1 General malfunctions ...................................................................................................... 73
7.1.1 Power failure.............................................................................................................. 74
7.1.2 Insufficient vacuum .................................................................................................... 75
7.1.2.1 Small flange connections ................................................................................... 75
7.1.2.2 Aeration valve, media drain valve ...................................................................... 76
7.1.2.3 Pressure control valve........................................................................................ 76
7.1.2.4 Rubber valves .................................................................................................... 76
7.1.2.5 Vacuum sensor .................................................................................................. 76
7.1.3 Insufficient ice condenser temperature ...................................................................... 77
7.2 Process and error messages .......................................................................................... 77
7.3 Service contact ............................................................................................................... 78
8 Maintenance and service................................................................................................... 79
8.1 Maintenance ................................................................................................................... 79
8.1.1 General...................................................................................................................... 79
8.1.2 Ice condenser chamber ............................................................................................. 80
8.1.3 Aeration valve, media drain valve .............................................................................. 81
8.1.4 Heat exchanger (only for air-cooled freeze-dryers) .................................................... 82
8.1.5 Electrical system ........................................................................................................ 82
8.1.6 Vacuum pump ........................................................................................................... 82
8.1.7 Exhaust filter (oil mist separator)................................................................................ 83
8.1.8 Refrigeration system .................................................................................................. 83
8.1.9 Vacuum sensor.......................................................................................................... 84
8.1.10 Accessories ............................................................................................................... 84
8.2 Disinfection of the drying chamber and accessories ....................................................... 85
8.3 Service ........................................................................................................................... 85
8.4 Return of defective parts ................................................................................................. 86

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9 Disposal.............................................................................................................................. 88
9.1 Disposal of the freeze-dryer ............................................................................................ 88
9.2 Disposal of the packaging ............................................................................................... 88
10 Technical data .................................................................................................................... 89
10.1 Ambient conditions ......................................................................................................... 90
10.2 Technical documentation ................................................................................................ 90
11 Appendix ............................................................................................................................ 91
11.1 Brief operating instructions ............................................................................................. 91
11.2 EC declaration of conformity in accordance with the EC Machinery Directive ................. 97
11.3 Declaration of conformity – China RoHS 2 ...................................................................... 99
11.4 EC declaration of conformity in accordance with the Pressure Equipment Directive ..... 101
11.5 Table of the sublimation pressure curve........................................................................ 103
12 Glossary ........................................................................................................................... 105
13 Index ................................................................................................................................. 107

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1 General information

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


Freeze-dryer
Do not use the freeze-dryer unless the following requirements are fulfilled:
• The freeze-dryer has been properly installed.
• The freeze-dryer is in a perfect technical state.
• The freeze-dryer is not located in an area with an explosion hazard.
• No unauthorised design modifications, additions or conversions without
the written approval by Martin Christ Gefriertrocknungsanlagen GmbH
have been performed.
• The vacuum pump used is approved by Martin Christ
Gefriertrocknungsanlagen GmbH. The vacuum pumps approved for this
system are listed in chapter 5.5 - "Vacuum pumps".
• The accessories used have been approved by Martin Christ
Gefriertrocknungsanlagen GmbH. This does not apply to commercially
available freeze-drying vessels made of glass or plastic.

The freeze-dryer has been exclusively designed for the freeze-drying of


solid or liquid products in ampoules, vials or dishes. It is, therefore, solely
intended for this application.
The freeze-dryer is suitable for freeze-drying solid substances and aqueous
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 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 (see
chapter 8 - "Maintenance and service").

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1 General information
Exclusion of liability
Any use of the freeze-dryer other than the one described here or any use
going beyond this description is regarded as improper use. Martin Christ
Gefriertrocknungsanlagen GmbH cannot be held liable for any damage
resulting from such improper use.

Requirements concerning the products used in the freeze-dryer


• The product must not damage the material of the components of the
freeze-dryer or affect its mechanical strength.
• A reaction of the product following the supply of high amounts of energy
during the freeze-drying process must be excluded.
• The product must not be explosive or highly flammable since certain
components of the freeze-dryer are a potential source of ignition.

The additional information concerning special products in the following


chapters must be absolutely observed (see chapter 1.2.1 - "Freeze-drying
of solvent-containing products (non-aqueous media)" and chapter 1.2.1 -
"Freeze-drying of solvent-containing products (non-aqueous media)")!
NOTE

1.2.1 Freeze-drying of solvent-containing products (non-aqueous media)


With regards of corrosion resistance, the use of some organic solvents in
aqueous solutions with low concentrations is acceptable.
A freeze-dryer is designed to be chemically resistant to most compounds
that are commonly used in freeze-drying processes. However, by
necessity, the freeze-dryer is comprised of several different materials,
some of which may be attacked and degraded by certain chemicals.
The methods of fabrication and/or conditions of exposure of an acrylic door,
as well as the way the chemicals are applied, can influence the results.
Some of these factors are listed below:
• Fabrication: Stress generated while sawing, sanding, machining,
drilling, polishing, and/or forming.
• Exposure: Length of exposure, stresses induced during the life of the
product due to various loads, changes in temperature etc.
• Application of chemicals: by contact, rubbing, wiping, spraying etc.

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1 General information
The following table can be used as a general guide for the expected
degradation during normal freeze-drying processes of organic solvents with
a total max. concentration of 10 vol-% in aqueous solutions.
Solvent Acrylic Stainless Silicon EPDM
glass steel rubber
Acetic acid 20% + + + o
Formic acid up to 10% + o o -
Trifluoracetic acid (TFA) - + o +
Calcium chloride + + + +
Sodium phosphate + + - +
Acetone - + + +
Acetonitrile - + - o
Carbon tetrachloride - + - -
Cyclohexane + + - -
Dioxane - + - o
Methyl-t-butyl ether + + o -
Pyridine - + - o
Methanol - + + +
Ethanol o + o +
tert-Butanol - + - o
DMSO - + - +
Legend: + No degradation to be expected
o Moderate degradation; limited use
- Severe degradation; infrequent use recommended;
immediate thorough cleaning required

The chemical attack on devices and accessory components can be


significantly reduced by immediate cleaning after the end of operation. All
parts of the freeze-dryer that have come in contact with the product must
be checked regularly for damages and replaced if necessary.

Solvents that are not listed in the table above, or the listed solvents in a
concentration higher than 10% by volume, must not be used!
NOTE

1.2.2 Freeze-drying of acid-containing products


Freeze-drying of products containing acids (with the exception of the sub-
stances already listed under chapter 1.2.1 - "Freeze-drying of solvent-
containing products (non-aqueous media)" in the concentrations stated
there) is only permissible if special protective measures and equipment-
related precautions are taken. Otherwise, there is a risk of damage to
property and personal injury. Consultation of Martin Christ
Gefriertrocknungsanlagen GmbH is absolutely mandatory in order to define
the measures that need to be taken!

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1 General information

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 11.4 - "EC declaration of conformity in accordance
with the Pressure Equipment Directive")

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1 General information

1.7 Scope of supply


The scope of supply comprises:
• 1 tube of high-vacuum grease Part no. 126210
• 1 drain hose 0.4 m (silicone 9 x 12 mm) Part no. 513200
• 1 operating manual

Additional items if a vacuum pump is included:


• Pump-specific accessories
• Suitable tools depending on the vacuum pump type

Accessories and commissioning


According to your order, our order confirmation, and our delivery note.

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2 Layout and mode of operation


2

Layout and mode of operation
2.1 Layout of the freeze-dryer

2.1.1 Functional and operating elements

1 Ice condenser
chamber with an
internal ice condenser
2 User interface (see
chapter 6.5.1 - "User
interface")
3 Mains power switch

Fig. 1: Front and right side of the freeze-dryer

4 Pipe connection of the


vacuum pump (behind
the cover plate)
5 Ice condenser

Fig. 2: Ice condenser chamber

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6 Aeration and media


drain valve

Fig. 3: Left side of the freeze-dryer

7 Power supply of the


pressure control valve
8 Name plate (see
chapter 2.1.2 - "Name
plate")
9 Power supply of the
vacuum pump
10 Equipotential bonding
screw
11 Mains connection
12 Vacuum connection
13 Connection of the
vacuum sensor
14 Option: data interface
for further accessories
15 Heat exchanger of the
refrigeration unit

Fig. 4: Rear view of the freeze-dryer

16 User interface with


touch panel

Fig. 5: User interface with touchpanel

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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 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

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

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].
NOTE

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 Preparation
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.

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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.

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.

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2.2.2.4 Final drying


Final drying is an option whenever one requires a product with minimal
residual moisture. In the physical sense, this process is a desorption
process, i.e. the removal of adsorptively bound water. Final drying is
performed under the lowest possible final pressure that depends on the ice
condenser temperature in accordance with the vapour pressure curve 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


The end of the drying process is reached when both the product and shelf
temperature are clearly in the positive range (+15 to +20°C) and if their
difference is not greater than 5 K.
Another indication of the end of the drying process is the behaviour of the
vacuum and of the ice condenser temperature. The ice condenser is no
longer subject to load and reaches the final temperature of approximately -
55°C or -85°C. The pressure in the drying chamber decreases in
accordance with the ice condenser temperature.
The vacuum pump will be switched off and the drying chamber will be
aerated via a rubber valve or via the aeration valve. The aeration valve can
also be used to flood the unit with nitrogen or another inert gas instead of
ambient air.
Then, the product can be removed from the unit.

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2.2.2.6 Defrosting
Defrosting of the ice condenser is carried out at room temperature or with
warm water.
• At a maximum, the ice condenser chamber may be half filled with water.
• Ensure that no water gets into the pipe connection of the vacuum pump
and the vacuum sensor (behind the cover plate, see figure)

1 Cover plate

Fig. 9: Eis condenser chamber

• Drain the condensate through the media drain valve at the left side of
the freeze-dryer by attaching a hose on the nozzle (included in the
scope of supply) and placing a vessel underneath.
In order to avoid damage, the condensate must be removed directly after
the completion of the defrosting process. Then, any residual water must be
removed from the ice condenser chamber by way of a cloth.

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3

Safety
3.1 Marking of the unit
The following symbols are used for Christ freeze-dryers:

Dangerous voltage
I On (Power)

Hot surface
0 Off (Power)

Name plate (see chapter


Caution! Risk of bruising
2.1.2 - "Name plate")

Attention, consult the Filled with natural


operating manual inflammable refrigerants

CE mark in compliance
Protective earth (ground) with the directive
2006/42/EC

China RoHS 2 mark


Earth (ground)
(only for China)

Unplug the mains plug

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.

NOTE

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3.2 Explanation of the symbols and notes


This operating manual uses the following names and symbols to indicate
hazards:

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


DANGER life-endangering injuries.

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


DANGER life-endangering injuries.

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


WARNING to life-endangering injuries.

This symbol indicates a potentially hazardous situation

Non-observance of these notes can cause minor injuries or damage to


CAUTION property.

This symbol indicates important information.

NOTE

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3.3 Responsibility of the operator


The operator is the person who uses the freeze-dryer for commercial or
economic purposes or lets a third party use it and who bears the legal
product responsibility for the protection of the users, personnel or third
parties during operation.

Operating personnel
The operator is obliged to ensure that
• the persons working on/with the freeze dryer
– have been specifically ordered to operate the system by the
operator,
– have been trained in terms of the operation of this system,
– 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 read and understood this operating manual (in particular the
safety sections and warning notes) and confirmed this with their
signature.
• the areas of responsibility of the personnel concerning the operation,
maintenance and care of the unit are clearly defined.
• the safety-conscious work of the personnel in compliance with the
operating manual and the relevant EC health and safety directives and
the national laws concerning health and safety and the prevention of
accidents are checked at regular intervals (e.g. every month).

Work area
The operator must
• perform a risk assessment concerning potential accidents in connection
with the freeze-dryer and take design-related countermeasures, if
necessary.
• check the sound pressure level at the workplace of the operating
personnel after the setup of the freeze-dryer. The sound pressure level
depends on the local conditions (e.g. sound reflected from the ceiling
and surrounding walls, external sources of noise). If necessary, the
operating personnel must wear suitable personal protective equipment
or other suitable protective measures must be taken in line with the
applicable legal provisions in order to avoid noise-induced hearing loss.
• perform a risk assessment in view of the specific hazards associated
with specific products that are freeze-dried in the freeze-dryer (e.g.
ignition/explosion hazard, discharge of harmful product residues at the
outlets of the chamber) and take the corresponding measures, if
necessary.
• 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. Substances that damage the material or weaken the
mechanical strength must not be used.

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• ensure that the freeze dryer is operated with one of the vacuum pumps
approved by Martin Christ Gefriertrocknungsanlagen GmbH (see
chapter 5.5 - "Vacuum pumps").
• have the system maintained at regular intervals (see chapter 8 -
"Maintenance and service").
• replace without delay any parts or components that are not in perfect
working order.

3.3.1 Freeze-drying of solvent-containing products


With regards of corrosion resistance, the use of some organic in aqueous
solutions with low concentrations is acceptable.
Under certain circumstances, the freeze-drying of products containing
solvents may lead to the formation of explosive mixtures. This is why the
operator must draw up special operating instructions/SOPs including
precise instructions
• concerning the deactivation of specific components (see chapter 1.2.1 -
"Freeze-drying of solvent-containing products (non-aqueous media)"),
• concerning the inspection of the freeze-dryer in view of damage caused
by the solvent that is used (see chapter 1.2.1 - "Freeze-drying of
solvent-containing products (non-aqueous media)").
The operator ensures sufficient air exchange in the room where the freeze-
dryer is used if nitrogen is used as the aeration/inertisation medium.

3.4 Requirements concerning the personnel


Risk of injury if the personnel are not sufficiently qualified
If unqualified personnel perform work on the freeze-dryer or are present in
the danger zone of the freeze-dryer, hazards result that can cause serious
injuries and considerable damage to property.
DANGER • Ensure that all the tasks are performed by personnel with the
corresponding qualifications.
• Ensure that unqualified personnel stay clear of the danger zones.
Risk of fatal injury to unauthorised persons due to hazards in the
danger zone or work area
Unauthorised persons who do not fulfil the requirements described herein
are not aware of the hazards in the work area. This is why there is a risk
DANGER of serious or even fatal injuries for unauthorised persons.
• Ensure that unauthorised persons stay clear of the danger zone and
work area.
• If in doubt, address these persons and instruct them to leave the
danger zone and work area.
• Interrupt any running work if unauthorised persons are present in the
danger zone or work area.

This manual uses the following personnel qualifications for various areas of
activity:

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Operating personnel (users)
The operating personnel operates and monitors the freeze-dryer during
normal operation and within the framework of its intended use. In the event
of malfunctions or other problems, the operating personnel informs the
respective specialised personnel.
It must be ensured that the persons operating the system
• have been specifically ordered to operate the system by the operator,
• have been trained in terms of the operation of this system,
• are familiar with the fundamental health, safety and accident prevention
regulations,
• have read and understood this operating manual (in particular the safety
sections and warning notes) and confirmed this with their signature.

Specialised personnel
Due to their special training, knowledge, experience and familiarity with the
relevant regulations, specialised personnel are in the position to perform
any tasks assigned to them and to autonomously identify and prevent
possible hazards.

Qualified electrician
Due to their special training, knowledge, experience and familiarity with the
relevant standards and regulations, qualified electricians are in the position
to perform work on electrical systems and to autonomously identify and
prevent possible hazards.

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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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
all persons and property.

3.6.1 General hazards


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.
WARNING 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)!

3.6.2 Hazards caused by improper transport

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 -
DANGER "Storage and transport" thoroughly!

3.6.3 Hazards caused by improper set-up


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.
WARNING
• 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!

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3.6.4 Hazards caused by improper connection


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.
WARNING
• 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 freeze-
dryer. 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.
• Have the electrical equipment of the unit inspected regularly.
• Defects such as loose or burnt cables must be eliminated immediately.

3.7 Safety notes concerning the operation


The following notes and instructions concerning the operation of the freeze-
dryer must be observed in order to protect all persons and property.

3.7.1 Hazards caused by electricity


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
DANGER 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.

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3.7.2 Hazards caused by the refrigeration system (natural, flammable refrigerants)


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.
DANGER
• 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!

3.7.3 Hazards caused by harmful products


Risk of poisoning/infection caused by the products
When loading and unloading the drying chamber, the personnel are
exposed to the product.
Skin contact or the inhalation of particles may cause severe damage to
DANGER health depending on the product in question.
• Wear suitable protective clothes, gloves, and respiratory protection!
Risk of poisoning/infection caused by the products
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.
DANGER Skin contact or the inhalation of particles may cause severe damage to
health depending on the product in question.
• Take suitable decontamination measures prior to commencing the
maintenance!
• Wear suitable protective clothes, gloves, and respiratory protection!

3.7.4 Hazards caused by solvents in the products


Explosion hazard caused by solvents in the products
When freeze-drying products containing solvents, gas mixtures may form.
These gas mixtures may be ignited on certain components of the freeze-
dryer.
DANGER There is an explosion hazard.
• Solvents that are not included in the table in chapter 1.2.1 - "Freeze-
drying of solvent-containing products (non-aqueous media)", or the
listed solvents in a concentration higher than 10% by volume, must not
be used!
• Refer to the safety data sheets of the products that are used!

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3.7.5 Hazards caused by acids in the products


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.
DANGER
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!

3.7.6 Hazards caused by contaminated condensate (defrosting water)


Risk of poisoning/infection caused by contaminated condensate
(defrosting water)
The condensate may contain harmful substances originating from the
product.
WARNING 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
when performing any work on the drain system (especially when
cleaning the valves and replacing the seals)!

3.7.7 Oil-sealed vacuum pump: hazards caused by contaminated vacuum pump


exhaust gases
Risk of poisoning/infection caused by vacuum pump exhaust gases
The exhaust gases of the vacuum pump may contain harmful substances
originating from the product.
Inhalation may cause severe damage to health.
WARNING
• Use the freeze-dryer only if it is equipped with a pipe that is properly
connected to the outlet of the vacuum pump/exhaust filter (oil mist
separator) and led to the outside via the roof!
• Depending on the product that is dried in the freeze-dryer, it may be
necessary to install a suitable filter system in the exhaust gas pipe!
• Compliance with the local rules and regulations concerning the
protection of the environment must be ensured!

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3.7.8 Oil-sealed vacuum pump: hazards caused by hot and contaminated vacuum
pump oil
Risk of scalding caused by the vacuum pump oil
When working on the vacuum pump and exhaust gas filter (especially
when changing the oil or filter), the maintenance personnel are exposed to
the hot vacuum pump oil.
WARNING There is a risk of scalding in the event of skin contact.
• Work on the vacuum pump must only be carried out by qualified
specialist personnel!
Risk of poisoning/infection caused by the vacuum pump oil
When working on the vacuum pump and exhaust gas filter (especially
when changing the oil or filter), the maintenance personnel are exposed to
the vacuum pump oil, which may contain harmful substances originating
WARNING from the product. In addition, synthetic oils can release toxic fumes when
they are ignited or heated above 300°C.
The inhalation of the fums that are released by the oil, or contact with the
skin, can cause severe damage to health.
• Work on the vacuum pump must only be carried out by qualified
specialist personnel!
• Ensure the environmentally sound disposal of the oil in compliance
with the local rules and regulations!
• Do not let the oil come into contact with tobacco products!

3.7.9 Hazards caused by noise


Risk of noise-induced hearing loss
Depending on the local conditions, a harmful sound pressure level may
occur.
High sound pressure levels can cause noise-induced hearing loss.
WARNING • Wear suitable personal hearing protection if necessary!

3.7.10 Hazards caused by hot surfaces


Risk of burns on hot surfaces
After a drying process, 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!
WARNING
• Do not touch the surfaces on purpose!

3.7.11 Hazards caused by cold surfaces


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.
WARNING • Wear suitable protective clothes and gloves!
• Do not touch the surfaces on purpose!

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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 self-
monitoring of the system. Error messages are displayed in the main
window under "Process & equipment messages" (chapter 6.5.1.1 - "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.

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)!

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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.

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 freeze-
dryer. 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.

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Accessories
• Do not use the freeze-dryer with accessories that shows signs of
damage.
• Only use accessories that have been approved by the manufacturer
(except for commercial vessels made of glass or synthetic materials).
We explicitly warn against the use of equipment of poor quality!
Breaking glass or bursting vessels can cause dangerous situations.

Handling hazardous materials


• The generally applicable regulations for handling flammable substances
in laboratories / workplaces must be observed.
• During sample preparation, loading and unloading of samples and
defrosting, appropriate safety precautions must be observed.
• Depending on the used solvent, hot gas defrosting should be avoided.
• Caution when handling hazardous materials such as strong acids or
bases, radioactive substances and volatile organics: If such substances
are spilled, they must be cleaned up immediately.
• If a sample with hazardous materials such as strong acids or bases,
radioactive substances or volatile organics is spilled inside a chamber,
they must be cleaned up immediately.
• Caution when handling solvents: Keep sources of ignition away from
solvents.
• When using flammable or hazardous solvents, the vacuum pump must
be vented to or operate inside a fume hood.

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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4 Storage and transport


4.1 Dimensions and weight


Values for the freeze-dryer without a vacuum pump:
Alpha 1-2 LSCbasic

Height: 345 mm

Width: 315 mm

Depth (including vacuum connection): 470 mm

Weight: approx. 32 kg

4.2 Storage conditions


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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4.3 Notes on transport


• Use suitable packaging for the transport, and if at all possible, the
original packaging.
• Install all transport safety devices (see chapter 4.5 - "Transport safety
device").
• Over short distances, the freeze-dryer can be transported by a suitable
number of persons who reach under it from the sides.
• When lifting the freeze dryer, always reach under the freeze-dryer from
the side. Do not grab the unit at the plastic control panel (see figures
below).
correct incorrect

Fig. 10: Lifting the freeze-dryer

The freeze-dryer Alpha 1-2 LSCbasic weighs approx. 32 kg!

CAUTION

• When setting the unit down, ensure that the feet are upright (see figures
below).

Fig. 11: Unit feet

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4.4 Packaging
The freeze-dryer is packaged in a cardboard box or in a wooden crate,
depending on the scope of supply.
• After opening the packaging, take out the box containing the
accessories.
• Remove the packaging material.
• Lift the freeze-dryer upwards and out of the crate/cardboard box. When
lifting the unit, always reach under the freeze-dryer from the side.

The freeze-dryer Alpha 1-2 LSCbasic weighs approx. 32 kg!

CAUTION

• Retain the packaging for any possible future transport of the freeze-
dryer.

4.5 Transport safety device


Prior to start-up, the vacuum sensor must be installed (see chapter 5.4 -
"Vacuum sensor").

Prior to any transport, the vacuum sensor must be deinstalled.

NOTE

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5 Set-up and connection


5.1 Location of use


Use the freeze-dryer solely in closed and dry spaces.

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!
NOTE

• 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 +5°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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5 Set-up and connection


5.2 Power supply


5.2.1 Type of connection


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
DANGER 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.

The operating voltage on the name plate must correspond to the local
supply voltage!
DANGER

Christ freeze-dryers are units of protection class I. Freeze-dryers of this


type have a three-wire power cord with an IEC C13 connector (see chapter
10 - "Technical data").

The removable power cord must not be replaced with a power cord of
inadequate rating!
NOTE

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


Sufficiently rated fuse protection of the freeze-dryer in the electrical system
of the building is required.

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5 Set-up and connection


5.3 Aeration and media drain valve


The aeration and media drain valve is located on the left side of the unit
(see chapter 2.1.1 - "Functional and operating elements").
After the end of a freeze-drying process, the unit will be aerated via the
aeration valve.
Additionally, it is used to drain off the condensate and the defrosting water.
• Connect the drain hose (included in the scope of supply) to the hose
connector.
• Place a collecting vessel under the unit.
The hose must be laid with a continuous slope and the end of the hose
must always be above the liquid level in the collecting vessel. This prevents
water and dirt residues from being sucked into the ice condenser chamber
if there is negative pressure when the media drain valve is opened.

5.4 Vacuum sensor

Please refer to the separate operating manual of the vacuum sensor!

NOTE

The freeze-dryer is equipped with a Pirani vacuum sensor.

Capacitive vacuum sensors cannot be used.

NOTE

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Installation of the vacuum sensor
In order to protect the vacuum sensor against transport damage, it comes
supplied in its original packaging. Prior to commissioning the freeze-dryer,
the sensor must be installed.

1 Vacuum sensor
2 Clamping rings
3 Connection socket

Fig. 12: Position of the vacuum sensor and the connection socket

• Switch the unit off by actuating the mains power switch.


• Take the vacuum sensor out of its original packaging and fasten it to the
connector with a bow-shaped connecting piece, two clamping rings
(DIN16KF) and two centring rings (included in the scope of supply).
• Plug the connector to the connection socket and hand-tighten the
screws on the connector.

It is absolutely essential to comply with the manufacturer’s instructions in


the separate operating manual of the vacuum sensor!
NOTE

The vacuum sensor comes supplied in a calibrated state.

NOTE

After the freeze-dryer has been switched on, the vacuum sensor needs
several minutes until it is ready for operation.

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5.4.6 Vak uumpumpe →

5.5 Vacuum pumps


To ensure its intended use, the freeze-dryer Alpha 1-2 LSCbasic must be
used with one of the following vacuum pumps:

Oil-sealed vacuum pumps:


• Rotary vane pump Vacuubrand RZ2.5
• Rotary vane pump Edwards RV3

5.4.6 Vak uumpumpe →

5.5.1 Oil-sealed vacuum pump and exhaust filter (oil mist separator)

It is absolutely essential to refer to the separate instruction manual of the


vacuum pump and exhaust filter (if applicable)!
NOTE

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").
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)!
NOTE 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. Alternatively, it can be connected to the freeze-dryer
via an interface box (see chapter 5.6 - "Use of an interface box").

1 Label indicating the


maximum current

Fig. 13: Indication of the maximum current for the vacuum pump (example)

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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,
we recommend using a condensate trap (Woulff bottle or wash bottle).

5.6 Use of an interface box


The current consumption of certain vacuum pumps is higher than what is
permissible for use with the freeze-dryer (see the label stating the
maximum current values for the vacuum pump at the IEC C13 connector,
illustration above). These pumps must be provided with power via a
customer-provided power outlet and they must be operated separately.
Alternatively, they can be connected to the freeze-dryer via the interface
box. The advantage of the interface box is that, in this case, the vacuum
pump can be controlled/actuated via the freeze-dryer.
Its connection requires separate dedicated circuits and power sockets for
the freeze-dryer and for the interface box.

Connection of the interface box

Fig. 14: Connection of the interface box (schematic diagram)

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• Connect the connecting cable of the vacuum pump with the designated
IEC C13 connector of the interface box (see the following picture,
item 1).
1 IEC C13 connector
for the vacuum pump

Abb. 15: Connector for the vacuum pump at the interface box

• Connect the built-in connecting cable of the interface box (see the
following picture, item 2) to the IEC C13 connector for the vacuum
pump at the back of the freeze dryer (item 4).
• Connect the mains power cable of the interface box to the designated
IEC C14 connector (see the following picture, item 3) and establish the
power supply.
• Establish the power supply of the freeze-dryer.
2 Connection with the
freeze-dryer
3 Mains power connector
of the interface box

Fig. 16: Connectors for mains power and freeze-dryer at the interface box

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4 IEC C13 connector
for the vacuum pump
at the back of the
freeze-dryer

Fig. 17: Back of the freeze-dryer (example)

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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").

Observe the installation direction of the pressure control valve (see


illustration below)!
CAUTION

1 Pressure control
valve

Fig. 18: Installation of the pressure control valve

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5.8 Rubber valves


The rubber valves (part no. 121860) enable the connection of round-bottom
flasks, wide-neck filter bottles, or distributors for ampoules to a manifold or
drying chamber. Depending on the connector of the components, the blue
plug can be removed.

1 Locking handle
2 Aeration connection
3 Vessel connection
4 Rubber plug
5 Connection to freeze-
dryer (e.g. via a
manifold)

Fig. 19: Rubber valve

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 freeze-
dryer as well as to the vessel connector prior to start-up in order to ensure
trouble-free operation.
NOTE

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. 20: Possible positions of the locking handle

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6 Operation

6 Operation
6.1 Initial start-up

Before the initial start-up, please ensure that your freeze-dryer is properly
set up and installed (see chapter 5 - "Set-up and connection")
WARNING

6.2 Installation of accessories


The accessories must be completed in accordance with the drying method
that is applied as well as in accordance with the scope of supply.

6.3 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.

6.4 Switching the freeze-dryer on


• Actuate the mains switch.
The control unit performs a self-test and an initialisation. This may take
several seconds.

• Follow the safety instructions and hazard warnings (see chapter 3 -


"Safety")!

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6.5 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. 21: Start screen of the LSCbasic control unit (example)

6.5.1 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. 22: User interface LSCbasic

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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.

6.5.1.1 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.
1 Status line
2 Schematic system
diagram
3 Value windows
4 Button "Tools"
5 Button "Set" (set
values)
6 Button "Process
and equipment
messages"
7 Button "Operating
mode: select/start"
8 Button "Stop"

Fig. 23: Overview of the main window "Process"

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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 battery-
buffered and must be reset after a failure (chapter 6.5.1.2 - " 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:
...

No
No USB storage device or LAN network connected
symbol

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.

If the double-chamber method has been selected for the freeze-drying


process, the system diagram always includes a drying chamber even if a
manifold is installed.
NOTE

Fig. 24: Schematic system diagram with the name and reference designation of the
component

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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)

Fig. 25: 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.

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Vapour pressure curve for ice and water
A diagram shows the relationship between the pressure and sample
temperature for aqueous systems. 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. 26: Dialogue box “Vapour pressure curve for ice and water”

Option: USB process recording


(see chapter 6.6 - "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. 27: Dialogue box "USB process recording"

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Option: Lifting hoist1
(see chapter 6.6 - "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
6.5.2.1 - "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.
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. 28: 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.

1
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

Fig. 29: 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.
Use the arrow buttons to open the individual windows.

The error message text is always followed by an error code. Always


indicate the error code in the event of enquiries or service requests!
NOTE

4 Error message
5 Error code
6 Detailed information
7 Error counter and
time stamp of the
last error
8 Arrow buttons

Fig. 30: Details concerning an error message

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6 Operation

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.
NOTE

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 6.5.2 - "Starting a freeze-drying
process").

Fig. 31: Dialogue box "Operating mode: select/start"


(The version of the dialogue box that is displayed depends on the equipment of the
freeze-dryer.)

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. 32: Dialogue box "Standard unit test"

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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

Prior to performing a test, ensure that the chamber is dry and unloaded
and that the ice condenser is defrosted!
NOTE

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).

Fig. 33: Results of the performance tests

Evaluation:
Please contact Martin Christ Gefriertrocknungsanlagen GmbH for an
assessment of the results.

Button "Stop" (8)


Pressing this button stops the current process. The freeze-dryer switches to
standby.

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6.5.1.2 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
"General" options:
1 "Language"
2 "Scale unit"
3 "Freeze-drying
process"

Fig. 34: 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. 35: Dialogue box "Change language"

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Scale unit (2)
This dialogue box is used to change the unit of measurement for the
temperature and vacuum values.

Fig. 36: Dialogue box "Change scale unit"

Freeze-drying process (3)

This function depends on the type of freeze-dryer and is not available for
all types.
NOTE

Prior to the start of the process, the correct process must be selected. The
following processes are available:
• → Cold trap operation: Use of the freeze-dryer as a cold trap
• → Double-chamber method (outside): drying outside the ice condenser
chamber on shelves in a drying chamber or in bottles or flasks in
combination with a manifold
• Double-chamber method LyoCube: Drying outside the ice condenser
chamber, but with the CHRIST LyoCube (a rectangular drying
chamber that can be loaded from the front)

Fig. 37: Dialogue box "Freeze-drying process"

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Administration
"Administration"
options:
1 "Date/Time"
2 "Network"
3 "System properties"
4 "Access protection"
5 "Device options"

Fig. 38: Dialogue box "Options" / "Administration"

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. 39: Dialogue box “Change date/time

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Network (2)
This dialogue box is used to change the network settings.

The changes will not become effective until after a restart of the freeze-
dryer.
NOTE

Fig. 40: Dialogue box "Change network settings"

System properties (3)


This dialogue box is used to change the system settings.

Fig. 41: 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.

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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").

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. 42: Dialogue box "Access protection"

The other buttons cannot be activated unless the access protection is


active.
NOTE

Password timer runtime: In order to prevent unauthorised access, the


system will automatically switch back to the default setting after a pre-
defined 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. 43: Countdown of the password timer and the button with the lock symbol

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• The button with the lock symbol blocks any access immediately and the
system switches to the default setting.

Fig. 44: Access blocked, data editing not possible

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.
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)

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
(see chapter 6.6 - "Optional extensions"). Options that require a series-
number-specific release code are marked with the symbol " ".

Fig. 45: Dialogue box "Device options" (example)

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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.

The changes will not become effective until after a restart of the freeze-
dryer.
NOTE

Later installation of a vacuum sensor


In freeze-dryers that have been delivered without a vacuum sensor, the
device option "Sensor: vacuum not installed" is activated at the factory in
order to suppress error messages during operation.
If a vacuum sensor is installed at a later time, this option must be
deactivated as described hereinabove.

Fig. 46: Device option "Sensor: vacuum not installed"

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6 Operation
Service
"Service" options:
1 "Operating hours"
2 "Failure memory"
3 "Vacuum pump oil
change"
4 "Maintenance"
5 "Sensor adjustment"

Fig. 47: 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. 48: 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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6 Operation

Always indicate the error code in the event of enquiries or service


requests!
NOTE

Fig. 49: 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. 50: Dialogue box "Vacuum pump oil change"

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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. 51: Dialogue box "Maintenance"

Sensor adjustment (5)


In this dialogue box, the sensors are adjusted based on a predefined
reference value.

Sensors that are not properly adjusted will lead to incorrect


measurements which, in turn, will have a negative effect on the process
control.
CAUTION

Only specialised personnel are authorised to perform the sensor


adjustment.
NOTE

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6.5.1.3 Main window "?"


This main window includes the most important information concerning your
freeze-dryer:

1 Freeze-dryer type
2 Control system type
3 Serial number
4 Manufacturer contact
data
5 Details concerning the
software version

Fig. 52: Freeze-dryer system information (example)

In the event of enquiries at the manufacturer, please state the data that is
stated here.
NOTE

6.5.2 Starting a freeze-drying process


Freeze-drying processes are started in the main window "Process".

Prior to any freeze-drying process, the correct method must be selected


(chapter 6.5.1.2 - " Main window "Options"", "Freeze-drying process (3)").
NOTE

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 6.5.2.1 - "Entering set values"). Then, the freeze-
drying process can be started via the dialogue box "Operating mode:
select/start".

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.
NOTE

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If the value "∞" (infinite) is selected for a process phase, the next phase
must be started manually via the button "Operating mode: select/start".
NOTE

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 "Warm-
up" phase, a dialogue box opens:

Fig. 53: 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 freeze-
dryer 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.

6.5.2.1 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.

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Viewing or editing the set values:
• Press the button "Set" (see chapter 6.5.1.1 - "Main window "Process"").
The following dialogue box will be displayed:

1 "Defrosting" button

Fig. 54: 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.
Numerical values can be edited with the aid of a numerical keypad:
1 Set value display
2 Button for changing the
sign (e.g. when entering
temperature values)
3 "" (infinite)
4 Button for editing the
value in pre-defined
steps
5 Selection of a possible
maximum or minimum
value
6 Input of a value via the
numerical keypad
7 Button for deleting the
displayed value

Fig. 55: 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".

If the dialogue box is closed by the button "return", the changes will be
discarded.
NOTE

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6.6 Optional extensions


The basic unit is extendable with the following optional functions:

USB process recorder


see also chapter 6.5.1.1 - "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.

LAN process recording (RJ45)


This feature enables the recording of a running process directly on a
PC/laptop computer. During the process recording, the process data can be
viewed on the PC with LyoLogplus and they can be printed. It is also
possible to import the data directly into an Excel file after the completion of
the process recording.

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.
chapter 6.5.1.1 - "Main window "Process""

6.7 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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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).
• Acknowledge the error message.

7.1 General malfunctions


Type of error Possible reason Correction

No indication on the display • No power in the mains supply • Check the mains power supply
(see chapter 7.1.1 - "Power fuse.
failure").
• Power cord is not plugged in. • Plug in the power cord correctly.
• Fuses have tripped. • Check the on-site fuses
• The mains power switch is set • Switch mains power switch ON.
to off.

The touchpanel does not react at all • The sensitivity of the • Contact the service department
or it does not react correctly touchpanel is misadjusted. (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 • Loosen the connection. Place


small flange connection(s). 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 • Clean the lid or door seal and
seal. replace it if necessary.

• The ground-in stopper of the • Grease the ground-in stopper


attached drying chamber is not evenly and over the entire
installed correctly. sealing surface with vacuum
grease.

Leakage in the media drain valve • The media drain valve is soiled • Clean the media drain valve
with drying residues or wool (see chapter 8.1.3 - "Aeration
particles from cleaning cloths. valve, media drain valve") and
replace it if necessary.
• The O-rings are worn • 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")

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Type of error Possible reason Correction

The displayed vacuum value is not • Incorrect calibration • Calibrate the vacuum sensor
correct (see the separate operating
instructions of the vacuum
sensor).
• The vacuum sensor is soiled • Clean the vacuum sensor.
(e.g. due to water residues)
• The vacuum sensor is • Check the vacuum display with
defective. 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 • See the separate operating
instructions of the vacuum instructions of the vacuum
pump. pump.

Insufficient ice condenser or shelf • The overpressure switch of the • Let the unit cool down.
temperature refrigeration unit has tripped.
• The thermal circuit breaker has • Ensure sufficient air circulation
tripped. (see chapter 7.1.3 - "Insufficient
ice condenser temperature")

The error message "Refrigeration • Leakage on the low pressure • Acknowledge the message.
unit x.x overpressure" is displayed side (suction side) of the If the message is displayed
during a freeze-drying process refrigeration system leads to a repeatedly, inform the service
pressure increase department (see chapter 7.3 -
"Service contact")

If it is impossible to eliminate the errors, contact the Christ service


department!
NOTE

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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7.1.2 Insufficient vacuum

The vacuum checks must be carried out when the ice condenser is
frozen.
NOTE

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.

Fig. 56: Small flange and centring ring Fig. 57: Small flange with centring ring
and small flange

Fig. 58: Attaching the clamping ring Fig. 59: Tightened clamping ring

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7.1.2.2 Aeration valve, media drain valve


Risk of poisoning/infection caused by contaminated condensate
(defrosting water)
The condensate may contain harmful substances originating from the
product.
WARNING Contact with the condensate may cause severe damage to health.
• Wear suitable protective clothes, gloves, and respiratory protection
when performing any work on the drain system (especially when
cleaning the valves and replacing the seals)!

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.

The inspection of the valve must be carried out by qualified specialist


personnel (see chapter 7.3 - "Service contact").
NOTE

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.

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7.1.3 Insufficient ice condenser temperature

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.
CAUTION

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. -55°C or approx.
–85°C (depending on the type of freeze-dryer) is reached when the ice
condenser is not loaded and the ice condenser chamber is evacuated.

7.2 Process and error messages


The control system displays the complete process and error messages
(see chapter 6.5.1.1 - "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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7.3 Service contact


In the event of queries, malfunctions, or spare part enquiries:

From Germany:
Contact
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode (Germany)
Tel. +49 (0) 55 22 / 50 07-44 44
E-mail: [email protected]

Outside Germany:
Contact our agency in your country. All agencies are listed at
www.martinchrist.de → [Sales Partners]

If you would like to utilise our after-sales-service, please state the type of
your freeze-dryer and its serial number.
NOTE

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8 Maintenance and service


The freeze-dryer and the accessories are subject to high mechanical and
chemical stress. Thorough maintenance performed by the user extends the
service life and prevents premature failure.

If corrosion or other damage occurs due to improper care, the


manufacturer cannot be held liable or subject to any warranty claims.
CAUTION

• Thoroughly clean the freeze-dryer immediately after use to prevent or at


least significantly reduce the damage to the materials of construction
(see also chapter 1.2.1 - "Freeze-drying of solvent-containing products
(non-aqueous media)").
• Use soap water or other water-soluble, mild cleaning agents for
cleaning the freeze-dryer and the accessories.
• Do not use corrosive and aggressive substances.
• Do not use solvents.
• Do not use agents with abrasive particles.
• Do not expose the freeze-dryer or its accessories to intensive
UV radiation (e.g. sunlight) or thermal stress (e.g. by heat generators).
• Do not turn the unit upside down in order to clean it.

8.1

Maintenance
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
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.
WARNING
• Wear suitable protective clothes and gloves!
• Do not touch the surfaces on purpose!
• Let the chamber cool down prior to commencing the maintenance!
Risk of poisoning/infection caused by the products
When performing maintenance work on parts coming into contact with the
product (e.g. all parts inside the chamber, vacuum pump), the personnel
may be exposed to product residues.
DANGER Skin contact or the inhalation of particles may cause severe damage to
health depending on the product in question.
• Take suitable decontamination measures prior to commencing the
maintenance!
• Wear suitable protective clothes and gloves!

• 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.

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.

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8.1.3 Aeration valve, media drain valve


Risk of poisoning/infection caused by contaminated condensate
(defrosting water)
The condensate may contain harmful substances originating from the
product.
WARNING Contact with the condensate may cause severe damage to health.
• Wear suitable protective clothes, gloves, and respiratory protection
when performing any work on the drain system (especially when
cleaning the valves and replacing the seals)!

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.

1 Valve opening
2 Valve core
3 O-rings

Fig. 60: Valve opening and valve core with O-rings, here: drain valve (example illustration)

• If necessary, apply a thin layer of high vacuum grease (part no. 126210)
to the valve insert and reinsert it.
• Put the freeze-dryer into operation again.
If the vacuum is still insufficient, the freeze-dryer must be checked by
qualified specialist personnel (see chapter 7.3 - "Service contact").

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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").

8.1.5 Electrical system


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
DANGER paralysis.
• Only qualified electricians 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.

8.1.6 Vacuum pump

Please refer to the separate operating manual of the vacuum pump!

NOTE

The stress of the vacuum pump in conjunction with a freeze-dryer is usually


not very high. This is why the recommendations in this operating manual
may differ from the information that is provided by the pump manufacturers.
Under normal operating conditions, the following maintenance tasks
concerning the vacuum pump must be performed at regular intervals:
• Check the oil level of the vacuum pump once per week. If necessary,
top it up with oil.
• Check the state of the oil at regular intervals (depending on the
frequency of use of the freeze-dryer and the product that is used). It
must be changed when it becomes cloudy, contains particles or
changes colour.
• Check the running pump for any unusual noise.

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• Ensure that the pump has reached its operating temperature prior to
changing the oil.
• Perform the first oil change after approximately 100 operating hours.
• The other oil changes depend on the operating conditions. In general,
an interval of 500 to 1,000 operating hours is sufficient.
• Please contact the Christ service department if you have any queries
(see chapter 7.3 - "Service contact").

8.1.7 Exhaust filter (oil mist separator)

Please refer to the separate operating manual of the vacuum pump and
the exhaust filter!
NOTE

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).

8.1.8 Refrigeration system


Risk of explosion due to refrigerants
The natural refrigerants used are highly flammable and can form an
explosive mixture if their concentration in the ambient air is sufficiently
high.
DANGER 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!

The refrigerant circuit is a closed system. Only certified and qualified


persons are authorised to perform work on the refrigeration system!

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8.1.9 Vacuum sensor

Please refer to the separate operating manual of the vacuum sensor!

NOTE

The vacuum sensor has only a limited service life.


• The vacuum sensor is maintenance-free.
• Remove any soiling on the outside with a cloth.

8.1.10 Accessories

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.
CAUTION

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.

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8.2 Disinfection of the drying chamber and accessories

If dangerous materials (e.g. infectious and pathogenic substances) are


used, the freeze-dryer and accessories must be disinfected.
DANGER

• Use commercially-available disinfectants such as, for example, Incidur,


Meliseptol, Sagrotan, Buraton, or Terralin (available at specialised
trade).
• The freeze-dryers and the accessories consist of various materials. A
possible incompatibility must be considered.
• Before using cleaning or decontamination agents that were not
recommended by us, contact the manufacturer to ensure that such a
procedure will not damage the freeze-dryer.
• Please contact us if you have any queries (see chapter 7.3 - "Service
contact").

8.3 Service

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.
DANGER

The freeze-dryer is subject to high mechanical stress. In order to be able to


withstand this high level of stress, high-quality components were used
during the production of the freeze-dryer. Nevertheless, wear cannot be
excluded and it may not be visible from the outside.
This is why we recommend having the freeze-dryer checked by the
manufacturer during an inspection once per year.

Information and appointments:


From Germany:
Contact
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode (Germany)
Tel. +49 (0) 55 22 / 50 07-44 44
E-mail: [email protected]

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Outside Germany:
Contact our agency in your country. All agencies are listed at
www.martinchrist.de → [Sales Partners]

If you would like to utilise our after-sales-service, please state the type of
your freeze-dryer and its serial number.
NOTE

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.

We will return the part/unit if no declaration of decontamination is


provided!
NOTE

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.

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8 Maintenance and service

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.
NOTE

The forms can be downloaded online from


www.martinchrist.de → [Service] → [Overhaul, repair and leak testing].

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9 Disposal

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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10 Technical data

10 Technical data
Manufacturer: Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode (Germany)

Type: Alpha 1-2 LSCbasic

Part number: 101700 (230 V / 50 Hz, air-cooled)


101704 (115 V / 60 Hz, air-cooled)
101702 (230 V / 60 Hz, air-cooled)

Performance data

Ice condenser
- capacity: 2.5 kg max.
- performance: 2 kg / 24 h max.
- temperature: approx. –55°C
- chamber volume: approx. 3.5 l

Shelf or product temperature


during freezing in the ice condenser chamber approx. –20°C

Max. shelf surface (→ double chamber method):


drying outside the ice condenser chamber 3 shelves, Ø 200 mm, Atotal=0.092m2
distance up to 80 mm, with accessory, part no. 120893

drying in injection vials with sealing under vacuum or 2 shelves,  200 mm, Atotal=0.054 m2
nitrogen atmosphere outside the ice condenser chamber distance 25-70 mm, with accessory, part no. 121015

drying in round bottom flasks 8 pieces, with accessory, part no. 121450

Connection requirements
(without vacuum pump and accessories)

Electrical connection: 1 x 230 V / 50 Hz


1 x 230 V / 60 Hz
1 x 115 V / 60 Hz

Protection class: I

IP protection category according to DIN 60529: 11

Apparent power: 0.8 kVA (at 230 V / 50 Hz)


0.85 kVA (at 230 V / 60 Hz)
0.75 kVA (at 115 V / 60 Hz)

Nominal current: 3.5 A (at 230 V / 50 Hz)


3.8 A (at 230 V / 60 Hz)
6.3 A (at 115 V / 60 Hz)

Power supply of the pressure control valve: 230 V, 50/60 Hz, 20 VA / 0.5 A max.

Power supply of the vacuum pump: 230 V, 50/60 Hz, 3.0 A max.

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Refrigerant data

Refrigerant: R1270
- Global warming potential (GWP): 3
- Filling quantity: 36 g
- Max. permissible pressure: 25 bar
- CO2 equivalent: < 0.01 t

Refrigerant: R170
- Global warming potential (GWP): 3
- Filling quantity: 6g
- Max. permissible pressure: 25 bar
- CO2 equivalent: < 0.01 t

Physical data
(without vacuum pump and accessories)

Dimensions
- height: 345 mm
- width: 315 mm
- depth (incl. vacuum connection): 470 mm

Weight: approx. 32 kg

Noise level 49 dB(A)


according to DIN 45635:

EMC according to EN 55011: Class B

Heat emission: 0.51 kW min.


0.91 kW max.

Equipment connections

Vacuum connection: Small flange connection DN25KF


(ISO 28403, DIN 2861)

Aeration and media drain valve: Hose nozzle DN10 (outside diameter 12 mm)

Mains input: IEC C13 connector

Vacuum sensor: SUB D-9


VCP 63

Option: Data interface (LAN): RJ45

→ 10.1 Umgebungs beding ung en

10.1
→ 10.1
Ambient conditions
Umgebungs beding ung en

• Use in closed spaces


• Altitudes up to 2,000 m
• Ambient temperature between +5°C and +25°C
• Maximum relative humidity of 80%
• Mains voltage fluctuations of up to ± 10% of the rated voltage

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 Appendix

11.1 Brief operating instructions


Functional and operating elements

1 Ice condenser chamber


with an internal ice
condenser
2 User interface
3 Mains power switch

Fig. 61: Front and left side of the freeze-dryer

4 Pipe connection of the


vacuum pump (behind
the cover plate)
5 Ice condenser

Fig. 62: Ice condenser chamber

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6 Aeration and media


drain valve

Fig. 63: Right side of the freeze-dryer

7 Power supply of the


pressure control valve
8 Name plate
9 Power supply of the
vacuum pump
10 Equipotential bonding
screw
11 Mains connection
12 Vacuum connection
13 Connection of the
vacuum sensor
14 Option: data interface for
further accessories
15 Heat exchanger of the
refrigeration unit

Fig. 64: Rear view of the freeze-dryer


16 Touchpanel

Fig. 65: User interface with touchpanel

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Step-by-step instructions – shelf drying
1 Freeze the sample separately, e.g. in a deep-freeze.

Ensure that the layer thickness of 1 to 2 cm is not exceeded, since


otherwise the drying time needs to be extended.
NOTE

2 Check the ice condenser chamber and ensure that it is completely free
from water residues.
3 Close the media drain valve and install the base plate.
4 Switch the unit on 20 to 30 minutes prior to the start of the drying
process in order to let the vacuum pump warm up.
5 Place the plate rack on the base plate.
6 Transport the frozen samples as quickly as possible from the deep-
freeze to the freeze-dryer and place them on the shelves.
Recommendation: Store the product vessels on the aluminium shelves or,
if possible, the entire rack with the shelves in the deep- freeze. The
advantage is that due to the higher cold storage capacity of the aluminium
material, the product will remain frozen for a longer period of time so that
NOTE the sample will not thaw.

7 nstall the drying chamber. Prior to doing so, check whether the O-ring
is completely free of dirt particles. The ground-in stopper of the acrylic
glass bell must be greased with high-vacuum grease.
8 Ensure that all of the valves of the acrylic glass bell are closed.
9 Ensure that the aeration valve is closed.
10 Ensure that the media drain valve is closed.
11 Start the main drying process either by opening the manual shut-off
valve or by waiting for the electromagnetic valve to open. Vacuum is
applied to the chamber and the freeze-drying process commences.

The vacuum pump always runs with maximum power. With this type of
freeze-dryer, the power of the vacuum pump cannot be controlled.
NOTE

12 The operating panel displays the vacuum, the ice condenser


temperature, and the current operating mode.
13 The end of the process is reached when the ice condenser is no longer
loaded and when it again reaches a final temperature of approximately -
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature.
14 Switch the vacuum pump off and aerate the drying chamber via the
media drain valve or via a rubber valve.
15 Switch the unit off by actuating the mains power switch and take the
product out of the freeze-dryer.

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16 Switch the unit on again and start the defrosting process.

Ensure that no water gets into the pipe connection of the vacuum pump or
vacuum sensor.
CAUTION

17 Drain the defrosting water via the media drain valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel.
18 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
service life of the vacuum sensor.

Step-by-step instructions – drying in a flask


1 Freeze the sample separately, e.g. in a deep-freeze.

Ensure that the layer thickness of 1 to 2 cm is not exceeded, since


otherwise the drying time needs to be extended.
NOTE

2 Check the ice condenser chamber and ensure that is completely free
from water residues.
3 Install the drying chamber. Prior to doing so, check whether the O-ring
is completely free of dirt particles. The ground-in stopper of the acrylic
glass bell must be greased with high-vacuum grease.
4 Ensure that all of the valves are closed.
5 Let the vacuum pump warm up 20 to 30 minutes before the freeze-
drying processes commences.
6 Connect a frozen sample to a valve.

After the pressure has fallen below 1.030 mbar, a frozen sample can be
connected to a valve. The next frozen sample cannot be connected to
another valve until the pressure is again lower than 1.030 bar.
CAUTION

The vacuum pump always runs with maximum power.


With this type of freeze-dryer, the power of the vacuum pump cannot be
controlled.
NOTE

7 The operating panel displays the vacuum, the ice condenser


temperature, and the current operating mode.
8 The end of the process is reached when the ice condenser is no longer
loaded and when it again reaches a final temperature of approximately -

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11 Appendix
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature.

The drying time depends on the layer thickness of the sample, the solids
content of the sample, and the amount of heat that is supplied during the
drying process. In the case of a layer thickness of 1 cm, the freeze-drying
process usually takes 24 hours.
NOTE

9 Switch the vacuum pump off and aerate the drying chamber via the
media drain valve or via a rubber valve.
10 Switch the unit off by actuating the mains power switch and take the
product out of the freeze-dryer.
11 Switch the unit on again and start the defrosting process.

Ensure that no water gets into the pipe connection of the vacuum pump or
vacuum sensor.
CAUTION

12 Drain the defrosting water via the defrosting water valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel.
13 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
service life of the vacuum sensor.

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11.2 EC declaration of conformity in accordance with the


EC Machinery Directive

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11.3 Declaration of conformity – China RoHS 2

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11.4 EC declaration of conformity in accordance with the Pressure


Equipment Directive

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11.5 Table of the sublimation pressure curve

°C = mbar °C = mbar °C = mbar °C = mbar

0 6,110 -20 1,030 -40 0,120 -60 0,011

-1 5,620 -21 0,940 -41 0,110 -61 0,009

-2 5,1770 -22 0,850 -42 0,100 -62 0,008

-3 4,760 -23 0,770 -43 0,090 -63 0,007

-4 4,370 -24 0,700 -44 0,080 -64 0,006

-5 4,020 -25 0,630 -45 0,070 -65 0,0054

-6 3,690 -26 0,570 -46 0,060 -66 0,0047

-7 3,390 -27 0,520 -47 0,055 -67 0,0041

-8 3,010 -28 0,470 -48 0,050 -68 0,0035

-9 2,840 -29 0,4202 -49 0,045 -69 0,0030

-10 2,560 -30 0,370 ,50 0,040 -70 0,0026

-11 2,380 -31 0,340 -51 0,035 -71 0,0023

-12 2,170 -32 0,310 -52 0,030 -72 0,0019

-13 1,980 -33 0,280 -53 0,025 -73 0,0017

-14 1,810 -34 0,250 -54 0,024 -74 0,0014

-15 1,650 -35 0,220 -55 0,021 -75 0,0012

-16 1,510 -36 0,200 -56 0,018 -76 0,0010

-17 1,370 -37 0,180 -57 0,016 -77

-18 1,250 -38 0,160 -58 0,014 -78

-19 1,140 -39 0,140 -59 0,012 -79

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12 Glossary

12 Glossary
Desorption
Desorption (from Latin de-sorbere, sorbere = sup up, suck in) describes a
phenomenon whereby molecules are released from the surface of a solid.
In order to be able to desorb, the particle must have, or be provided with, a
sufficient amount of energy in order to overcome the binding energy.

Eutectic point
The eutectic point is the point at which a homogenous mixture (e.g. a
eutectic alloy) passes directly from the liquid to the solid phase without the
formation of a crystal mixture that consists of different phases.

Single-chamber method
At the single-chamber method, the freezing as well as the subsequent
drying of the product are both performed in the ice condenser chamber.
The sample is frozen as a result of the low temperature of the ice
condenser
(–55°C in the case of one-stage systems or –85°C in the case of two-stage
systems). The inside of the chamber can be cooled to approximately –20°C
or –40°C. The moderate supply of the frozen sample with energy, which is
necessary during the main drying phase, is ensured by heatable shelves on
which the product is placed.

Double-chamber method
Drying on shelves outside the ice condenser chamber is referred to as a
double-chamber system. The advantage compared to the → single-
chamber method is the considerably higher product capacity. In addition,
the product chamber can be isolated from the ice condenser chamber by
an intermediate valve in order to perform a so-called → pressure increase
test for determining the end of the drying process. In freeze-dryers without
an active shelf cooling, the samples need to be pre-frozen externally, e.g. in
a deep-freeze or freezer cabinet. After the transfer of the product into the
freeze-dryer, the actual → sublimation is started.

Reference designator
During the service life of industrial systems, a standardised reference
designation system is required for the planning, design, realisation,
maintenance, and disassembly stages in order to be able at all times to
identify every single component within the system in an unambiguous
manner. The reference designators) are affixed to the components and
entered into the technical documentation (e.g. circuit diagrams).

Sublimation
Sublimation (from Latin "sublimis" = high up in the air, raised), is a
thermodynamic process of the direct transition of a substance from the
solid phase to the gas phase.

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Index

13 Index

A Compliance with the EC health and safety


directives ................................................ 25
Access protection....................................... 63
Condensate, contaminated (hazards) ............
Accessories ............................. 13, 35, 79, 84 ................................................... 31, 76, 81
Accident prevention ............................. 25, 27 Connection................................................. 34
Accident prevention regulations ................. 25 Connection (hazards) ................................. 29
Acids .................................................... 11, 34 Connection of the vacuum sensor .............. 15
Acids (hazards) .......................................... 31 Connection requirements ........................... 89
Administration ............................................ 61 Contaminated condensate (hazards) .............
Aeration ............................................... 39, 70 ................................................... 31, 76, 81
Aeration valve ................................ 15, 41, 90 Contaminated defrosting water (hazards) ......
Aeration valve (cleaning and care) ............. 81 ................................................... 31, 76, 81
Aeration valve, malfunction ........................ 76 Control system type ................................... 69
Ambient conditions..................................... 90 Cooling system .......................................... 90
Ambient temperature ........................... 39, 90 Copyright ................................................... 12
Apparent power ................................... 16, 89 Corrosion ............................................. 79, 84
Areas of responsibility ................................ 25 Cost estimate ............................................. 86
B Cracks ....................................................... 84
Customer-provided fuses ........................... 40
Beeper ....................................................... 62
Behaviour of the pressure control valve in the D
case of insufficient ice condenser cooling Damage to the materials of construction .... 79
............................................................... 63 Dangerous materials .................................. 85
Brief operating instructions......................... 91 Data interface ............................................ 15
Button "Standard unit test" ......................... 57 Data interface (LAN) .................................. 90
Button "Stop" ............................................. 58 Date/Time .................................................. 61
C Declaration of conformity – China RoHS 2 . 99
CE mark in compliance with the directive Declaration of conformity (Machinery
2006/42/EC ............................................ 23 Directive) .......................................... 12, 97
Changing of operating supplies .................. 34 Declaration of conformity (Pressure
Chemical reactions .................................... 84 Equipment Directive) ............................ 101
China RoHS 2 – Declaration of conformity . 99 Declaration of decontamination .................. 86
Circuit diagram ........................................... 90 Decontamination agents ............................ 85
Cleaning .................................................... 34 Defrosting .................................................. 70
Cleaning agents ................................... 79, 85 Defrosting water, contaminated (hazards) ......
................................................... 31, 76, 81
Cleaning of the freeze-dryer ....................... 80
Desorption ............................................... 105
Cleaning the accessories ........................... 79
Details........................................................ 56
Cleaning the freeze-dryer........................... 79
Details concerning the software version ..... 69
Click on touch ............................................ 63
Device options ........................................... 64
CO2 equivalent ........................................... 90
Dialogue box "Operating mode: select/start"
Cold trap operation .................................... 60 ............................................................... 57
Commissioning .......................................... 13
Compatibility test........................................ 25
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Dialogue box "Process and equipment Freeze-dryer type....................................... 69
messages ............................................... 55 Freeze-dryer, cleaning and care ................ 80
Dialogue box "Schematic system diagram" 52 Freeze-drying of acid-containing products.. 11
Dialogue box "Tools" .................................. 53 Freeze-drying of solvent-containing products
Dimensions .......................................... 36, 90 ......................................................... 10, 26
Direct hazard to the life and health ............. 24 Freeze-drying phases ................................ 19
Disinfectants .............................................. 85 Freeze-drying process ......................... 19, 60
Disinfection of the drying chamber and Freeze-drying process, start ...................... 69
accessories ............................................ 85 Freezing ..................................................... 20
Displayed vacuum value is not correct ....... 74 Functional and operating elements ............ 14
Disposal of the freeze-dryer ....................... 88
G
Disposal of the packaging .......................... 88
General conditions ..................................... 12
Double-chamber method.................... 60, 105
General information on freeze-drying ......... 17
Double-chamber method LyoCube (outside)
............................................................... 60 General malfunctions ................................. 73
General work (maintenance) ...................... 79
E
Global warming potential (GWP) ................ 90
Earth conductor check ............................... 33
H
EC declaration of conformity (Machinery
Directive) .......................................... 12, 97 Handling hazardous materials .................... 35
EC declaration of conformity (Pressure Hazard warnings .................................... 9, 12
Equipment Directive) ............................ 101 Hazardous materials, handling ................... 35
Electrical connection .................................. 89 Hazards (acids) .......................................... 31
Electrical system (maintenance) ................ 82 Hazards (connection) ................................. 29
Electricity (hazards) ....................... 29, 40, 82 Hazards (contaminated condensate)..............
EMC according to EN 55011 ...................... 90 ................................................... 31, 76, 81
End of drying and aeration ......................... 21 Hazards (contaminated defrosting water) .......
Entering set values .................................... 70 ................................................... 31, 76, 81
Environmental protection ........................... 27 Hazards (electricity) ....................... 29, 40, 82
Equipment connections .............................. 90 Hazards (general, transport to
commissioning) ...................................... 28
Equipotential bonding screw .......... 15, 33, 40
Hazards (noise) ......................................... 32
Error correction .......................................... 73
Hazards (products, harmful) ................. 30, 80
Error messages ......................................... 33
Hazards (refrigeration system) ................... 30
Eutectic point ........................................... 105
Hazards (set-up) ........................................ 28
Exhaust filter ........................................ 44, 83
Hazards (solvents) ..................................... 30
Exhaust filter (Oil mist separator) ............... 43
Hazards (surfaces, cold) ............................ 32
Exhaust gases (hazards) ........................... 31
Hazards (surfaces, hot) ........................ 32, 80
Explanation of symbols .............................. 12
Hazards (transport) .................................... 28
Explanation of the symbols and notes ........ 24
Hazards (vacuum pump exhaust gases) .... 31
External data storage device ...................... 52
Hazards (vacuum pump oil) ....................... 32
F
Health and safety ....................................... 25
Failure memory .......................................... 66 Health and safety rules and regulations and
Filling quantity (refrigerant) ........................ 90 regulations for the prevention of accidents
Final drying ................................................ 21 ......................................................... 25, 27
Fire prevention ........................................... 34 Heat emission ............................................ 90
Form for the return of defective parts ......... 86 Heat exchanger ......................................... 82

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Heat exchanger of the refrigeration unit ..... 15 Maintenance and service ........................... 79
Humidity ..................................................... 90 Maintenance performed by the user ........... 79
I Malfunction of the pressure control valve ... 76
Malfunctions............................................... 73
Ice condenser ............................................ 89
Manufacturer............................ 79, 85, 88, 89
Ice condenser chamber.............................. 14
Manufacturer contact data ......................... 69
Ice condenser chamber, cleaning and care 80
Marking of the unit ..................................... 23
Importance of the operating manual ............. 9
Materials of construction, damage ............. 79
Important information ................................. 24
Max. humidity............................................. 90
Infectious substances ................................ 85
Maximum current for the vacuum pump ..... 43
Informal safety notes.................................. 27
Measures to be taken to ensure safe
Initial start-up ............................................. 49
operation ................................................ 34
Inspection by the manufacturer .................. 85
Media drain ................................................ 70
Installation of accessories .......................... 49
Media drain valve ........................... 15, 41, 90
Instruction .................................................. 25
Media drain valve (cleaning and care)........ 81
Insufficient ice condenser or shelf
Media drain valve, malfunction ................... 76
temperature ............................................ 74
Mode of operation ...................................... 17
Insufficient ice condenser temperature....... 77
Insufficient vacuum .............................. 73, 75 N
Intended use ................................................ 9 Name plate .......................................... 15, 16
Interface box .............................................. 44 Network ..................................................... 62
IP protection category according to DIN Network drive ............................................. 52
60529 ..................................................... 89 No indication on the display ....................... 73
L Noise (hazards) ......................................... 32
LAN process recording (RJ45) ................... 72 Noise level ................................................. 90
Language ................................................... 59 Nominal current ......................................... 89
Layout of the freeze-dryer .......................... 14 Nominal voltage ................................... 16, 29
Leakage in a rubber valve .......................... 73 Notes on safety and hazards ....................... 9
Leakage in the media drain valve............... 73 Notes on transport ..................................... 37
Leakage test .............................................. 70 O
Location of use .......................................... 39 Oil mist separator ................................. 44, 83
LSCbasic control system............................ 50 Oil mist separator (exhaust filter) ............... 43
Lyes ........................................................... 34 Oil-sealed vacuum pump ........................... 43
LyoLogplus data logging software .............. 72 Operating elements.................................... 14
M Operating hours ......................................... 66
Main drying ................................................ 20 Operating mode: select/start ...................... 57
Main window "?"......................................... 69 Operating personnel .................................. 25
Main window "Options" .............................. 59 Operating state .......................................... 52
Main window "Process" .............................. 51 Operating voltage....................................... 40
Mains power switch.................................... 14 Operation ................................................... 34
Mains voltage............................................. 90 Operational safety ...................................... 84
Maintenance ........................................ 34, 68 Operator (responsibility) ............................. 25
Maintenance (electrical system) ................. 82 Operator/maintenance/administrator
password ................................................ 64
Maintenance (general work) ....................... 79
Option: data interface................................. 15
Maintenance (vacuum sensor) ............. 41, 84
Option: USB process recording .................. 54
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Optional extensions ................................... 72 Requirements concerning the personnel .... 26
P Responsibility of the operator ..................... 25
Return of defective parts ............................ 86
Packaging ............................................ 38, 88
Risk assessment ........................................ 25
Part number ......................................... 16, 89
Rubber valves ...................................... 48, 76
Password input fails ................................... 73
Password timer runtime ............................. 63 S
Pathogenic substances ........................ 80, 85 Safe operation ........................................... 34
Performance data ...................................... 89 Safety and hazard notes ............................ 27
Performance test........................................ 58 Safety area ................................................ 34
Physical data ............................................. 90 Safety data sheets ..................................... 90
Potential hazard to the life and health ........ 24 Safety devices ........................................... 33
Potentially hazardous situation................... 24 Safety distance .................................... 29, 39
Power failure .............................................. 74 Safety instructions.................................. 9, 12
Power supply ............................................. 40 Safety notes concerning set-up and
Power supply of the pressure control valve .... connection .............................................. 28
......................................................... 15, 89 Safety notes concerning the initial start-up . 28
Power supply of the vacuum pump ...... 15, 89 Safety notes concerning the operation ....... 29
Preparation .......................................... 19, 49 Safety notes concerning the transport ........ 28
Pressure (refrigerant) ................................. 90 Safety-conscious work ............................... 25
Pressure control valve ............................... 47 Scale unit (unit of measurement) ............... 60
Pressure control valve (power supply) ....... 89 Schematic system diagram ........................ 52
Pressure control valve, malfunction ........... 76 Scope of supply ......................................... 13
Pressure marks .......................................... 84 Sensor adjustment ..................................... 68
Prevention of accidents ................................ 9 Serial number .......................... 16, 69, 78, 86
Procedures in the event of hazards and Service................................................. 66, 85
accidents ................................................ 33 Service contact .......................................... 78
Process and equipment messages ............ 55 Service life ................................................. 79
Process and error messages ..................... 77 Service work .............................................. 85
Process data .............................................. 51 Set process values..................................... 55
Products containing acids .......................... 11 Set-up ........................................................ 34
Products, harmful (hazards) ................. 30, 80 Set-up (hazards) ........................................ 28
Protection class ......................................... 89 Set-up and connection ............................... 39
Q Signs of corrosion ...................................... 84
Qualified electrician.................................... 27 Single-chamber method ........................... 105
Small flange connections ........................... 75
R
Solvent-containing products ....................... 10
Radioactive substances ............................. 80
Solvents ..................................................... 34
Rated current ............................................. 16
Solvents (hazards) ..................................... 30
Reference designation ......................... 56, 66
Solvents. .................................................... 79
Reference designator ............................... 105
Specialised personnel .......................... 27, 81
Refrigerant data ................................... 16, 90
Specialist personnel ....................... 76, 85, 86
Refrigeration problems
Standard unit test ....................................... 57
Conditions at the location of use ............. 39
Standards and regulations ......................... 12
Refrigeration system (hazards) .................. 30
Starting a freeze-drying process ................ 69
Remaining hazards .................................... 35
Status line .................................................. 52

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Freeze-dryer Alpha 1-2 LSCbasic

Index
Step-by-step instructions – drying in a flask 94 Type of connection..................................... 40
Step-by-step instructions – shelf drying...... 93 U
Storage ...................................................... 36
USB process recorder ................................ 72
Storage and transport ................................ 36
USB process recording .............................. 54
Storage conditions ..................................... 36
Use of an interface box .............................. 44
Stress-corrosion ......................................... 84
User interface ................................ 14, 15, 50
Sublimation .............................................. 105
UV radiation ......................................... 39, 79
Supply voltage ........................................... 40
V
Surfaces, cold (hazards) ............................ 32
Surfaces, hot (hazards) ........................ 32, 80 Vacuum connection ............................. 15, 90
Switching the freeze-dryer OFF ................. 72 Vacuum pump (oil-sealed) ......................... 43
Switching the freeze-dryer on..................... 49 Vacuum pump (power supply).................... 89
System check ............................................ 33 Vacuum pump exhaust gases (hazards) .... 31
System properties ...................................... 62 Vacuum pump is not activated ................... 74
Vacuum pump oil (hazards) ....................... 32
T
Vacuum pump oil change........................... 67
Table of the sublimation pressure curve... 103
Vacuum pump, cleaning and care .............. 82
Technical data ........................................... 89
Vacuum sensor .............................. 41, 76, 90
Technical documentation ........................... 90
Vacuum sensor (maintenance) ............ 41, 84
Thermal stress ..................................... 39, 79
Value windows ........................................... 53
Tools .......................................................... 53
Vapour pressure curve for ice and water ........
Topping-up of operating supplies ............... 34 ......................................................... 18, 54
Touch panel ............................................... 15 Ventilation .................................................. 77
Touchpanel does not react......................... 73 Vents ......................................................... 39
Toxic substances ....................................... 80 Viewing or editing the set values ................ 71
Training ...................................................... 25
W
Transport ................................................... 36
Warranty and liability .................................. 12
Transport (hazards) ................................... 28
Weight ................................................. 36, 90
Transport safety device .............................. 38
Transport to commissioning (hazards, Y
general) .................................................. 28 Year of manufacture .................................. 16
Type..................................................... 16, 89

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