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
CHRIST freeze-dryers have been solely designed for the freeze-drying of
solid or liquid products in ampoules, vials or dishes. They are, therefore,
solely intended for these applications.
The freeze-dryer is suitable
•for freeze-drying materials such as bacteria and virus cultures, blood
plasma, serum fractions, antibodies, sera, vaccines, and
pharmaceutical products
• for freeze-drying plant extracts, e.g. for biochemical tests
• for freeze-drying inorganic materials, e.g. nanoparticles
• for freeze-drying numerous other products (for further information
please contact our qualified personnel)
Any other use beyond this area of application is regarded as improper use.
Martin Christ Gefriertrocknungsanlagen GmbH cannot be held liable for any
damage resulting from such improper use.
The intended use also includes:
•observation of all the notes and instructions included in the operating
manual
•compliance with the inspection and maintenance instruction
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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
Non-compliance may be prosecuted under criminal law.
1.5 Explanation of symbols
In this operating manual, specialist terms that are explained in the glossary
(see chapter 12 - "Glossary") are marked by an arrow and printed in italics
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2.2 Mode of operation
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2.2.1 General information on freeze-drying
What is freeze-drying?
Freeze-drying or lyophilisation is a procedure for the gentle drying of highquality products. The product is dried by sublimation without passing
through the liquid phase.
What are typical applications for freeze-drying?
As far as their sheer quantity is concerned, foodstuffs are the major
application for freeze-drying. One widely known example is the production
of granulated instant coffee or the drying of fruit, e.g. for breakfast cereals.
Other areas of application are the restoration of water-damaged documents
or the drying of archaeological artefacts.
Another important area of application is the drying of biotechnological and
pharmaceutical products, e.g. tissues and tissue extracts, bacteria,
vaccines, and sera. Products that would not keep well when they are
dissolved in water can be preserved by freeze-drying. During this process,
the biological properties of these sensitive substances are preserved. The
compounds remain unchanged from a qualitative and quantitative point of
view. After the addition of water, the products will have the same
characteristics as the original products.
How does freeze-drying work?
Freeze-drying is a very gentle procedure for the extraction of water from a
product in the frozen state. The drying process takes place through sublimation, i.e. the direct transition of a product from the solid phase to the
gas phase. This happens under vacuum.
The following section describes the process of sublimation based on the
example of water, since most products that are processed by freeze-drying
are aqueous solutions. Their behaviour is based on identical fundamental
principles.
The vapour pressure curve above ice describes the phase transition as a
function of the pressure and temperature. The higher the temperature is,
the higher the vapour pressure.
•If the vapour pressure is higher than 6.11 mbar (A), water passes
through all three phases: solid, liquid, and gas (see the illustration).
• If the vapour pressure is below 6.11 mbar (B) and energy is added, the
ice will be directly converted into water vapour once the sublimation
curve is reached. This transition is called “sublimation”. If thermal
energy is added to pure ice with a temperature of less than –30°C at a
pressure of 0.37 mbar, it will be converted into water vapour once it
reaches –30°C (see figure).
The vacuum prevents the melting of ice when energy is added. If thermal
energy is added to a frozen product under vacuum, thawing of the product
will be prevented and the water that is contained within the product will be
released in the form of water vapour.
From a physical point of view, the freeze-drying process covers three
phases (see figure below):
(1) Freezing: The product to be dried is frozen under atmospheric pressure.
This can be done either directly in the freeze-dryer or in a separate deepfreeze. The freezing temperature should be approximately 10°C below the
solidification point of the product.
(2) Evacuation: When the product is sufficiently frozen, the vacuum pump is
activated. The pressure inside the drying chamber will be lowered to the
value that corresponds to the freezing temperature in accordance with the
vapour pressure curve above ice.
(3) Sublimation: Thermal energy is added to the product, thus starting the
sublimation process. Due to the added energy, the water in the product is
converted into water vapour. Since the ice condenser is much colder than
the product that is to be dried, the vapour pressure in the ice condenser is
considerably lower than above the product. As a result, the water vapour
that is released by the product streams to the ice condenser, where it
condenses on the condenser coils.
Once the free water has been extracted from the product during the main
drying phase, the last traces of bound water will also be removed at a final
pressure that is as low as possible and at higher temperatures. This takes
place by way of desorption. This drying phase is also called final drying.
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].
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2.2.2.2 Freezing
product.
The ice condenser chamber must be clean and dry. Any water residues
from a preceding drying run must be removed.
The media drain valve and the aeration valve must be closed.
In the case of units that are equipped with a pressure control valve
(standard on LSCplus units), the vacuum pump should be warmed up
(“warm-up”) for at least 15 minutes prior to the start of the main drying
phase. Do not subject the vacuum pump to condensable gases until the
operating temperature is reached. In this way, the service life of the
vacuum pump can be extended.
At the same time, the ice condenser is pre-cooled ("cool-down"). The ice
condenser temperature does not have any influence on the product
temperature. The sole purpose of the ice condenser is to bind the released
water vapour.
First, the product that is to be dried is frozen. This can be carried out either
directly in the freeze-dryer or in a separate deep-freeze. Especially in the
case of small filling quantities, we recommend pre-cooling the shelves as
well in order to prevent the product from thawing during the evacuation.
Two very different structures of the frozen material can be distinguished:
• crystalline structures with clearly distinguishable crystals
• amorphous structures with no crystal junctions at all (e.g. glass)
The majority of the freeze-drying products have a crystalline form.
When freezing these kinds of products, one must take into consideration
that too deep and too quick freezing leads to smaller ice crystals, which has
a negative effect on the duration of the drying process.
For every product to be dried, the solidification point must be determined as
a first step. This is the point at which the water that is contained in the
product has completely crystallised. In order to ensure an optimum freezedrying process, the product temperature should be approximately 10°C
below the solidification point.
A layer thickness of the product of 1-2 cm should not be exceeded, since
otherwise the drying duration would be negatively affected. If liquids are to
be dried in bottles with a layer thickness of more than 1 cm, we recommend
freezing them in a cooling bath with the aid of a shell or spin freezing
device (see figure). Due to the centrifugal force, the liquid to be frozen will
rise on the inner wall of the bottle and freeze. This procedure reduces the
layer thickness and, thereby, the total drying time will be shortened to a
considerable extent (see figures on the right side).
If the product that is to be dried contains solvents or high salt
concentrations, it may start to thaw during the drying process, which is
indicated by clearly visible foaming. In order to prevent this, the product
must be frozen as deeply as possible, e.g. with the aid of liquid nitrogen,
prior to putting it into the unit.
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2.2.2.3 Main drying
When the product is frozen to a sufficiently deep extent, the main drying
phase commences. The vacuum pump is switched on. The pressure inside
the drying chamber will be lowered to the value that corresponds to the
freezing temperature in accordance with the vapour pressure curve above
ice. At the same time, thermal energy will be added to the product. In the
case of products in round-bottom flasks, wide-neck bottles, etc., this is
realised through the environment that is considerably warmer (direct
contact heat), in the case of unheated shelves by way of thermal radiation
from the environment, and in the case of temperature-controlled shelves
directly via the shelves. As a result, the sublimation process starts.
At the beginning of the drying process, the maximum drying rate will be
reached. The more the sublimation area recedes into the product, the
further the produced water vapour must pass through the layers that have
already been dried.
Under certain conditions, it is possible that the vacuum inside the ice
condenser chamber increases during the main drying phase (e.g. from 0.63
mbar to 0.47 mbar) although the valve towards the vacuum pump is closed.
From a physical point of view, this is due to the pumping effect of the ice
condenser ("cryo-pumping effect").
The required drying time depends strongly on the drying vacuum. At 1.0
mbar, one gram of ice takes up a volume of 1 m3 of vapour, at 0.1 mbar a
volume of 10 m3 of vapour, and at 0.001 mbar a volume of 100 m3. The
closer the vacuum is to the solidification point, the smaller is the resulting
vapour volume. The drying rate increases and the drying time decreases.
The end of the main drying phase is reached, when the product
temperature and the shelf temperature are nearly identical. The
temperature difference between the shelf and the product should be
Final drying is an option whenever one requires a product with minimal
residual moisture. In the physical sense, this process is a desorption
process, i.e. the removal of adsorptively bound water. Final drying is
performed under the lowest possible final pressure that depends on the ice
condenser temperature in accordance with the vapour pressure curve
above ice as well as on the final vacuum of the vacuum pump that is used.
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The process is supported by a higher shelf temperature.
2.2.2.5 End of drying and aeration
The end of the drying process is reached when both the product and shelf
temperature are clearly in the positive range (+15 to +20°C) and if their
difference is not greater than 5 K.
Another indication of the end of the drying process is the behaviour of the
vacuum and of the ice condenser temperature. The ice condenser is no
longer subject to load and reaches the final temperature of approximately 55°C or -85°C. The pressure in the drying chamber decreases in
accordance with the ice condenser temperature.
The vacuum pump will be switched off and the drying chamber will be
aerated via a rubber valve or via the aeration valve. The aeration valve can
also be used to flood the unit with nitrogen or another inert gas instead of
ambient air.
•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.
The operator is obliged to ensure that the persons working with the freezedryer
• are 18 years old or older,
• have been specifically ordered to operate the unit and made aware of
dangers originating from the freeze-dryer, supply media, starting and
end products by the operator,
•are familiar with the fundamental regulations concerning workplace
safety and accident prevention
•have read and understood this operating manual (and in particular the
safety sections and warning notes) and confirmed this with their
signature.
The areas of responsibility of the personnel concerning the operation,
maintenance, and care of the unit must be clearly defined.
The safety-conscious work of the personnel in compliance with the
operating manual and the relevant EC and national health and safety
regulations as well as with the accident prevention regulations must be
checked at regular intervals (e.g. every month).
The operator is responsible for performing a risk assessment in terms of
disasters (e. g. fire) in the working area and, if necessary, for taking
constructional measures.
The operator is responsible to check the chemical compatibility of all
substances to be used inside the freeze-dryer (product to be processed,
cleaning media, etc.) with the material of the chamber walls, shelves, pipes,
and gaskets. Substances that may damage the material an degrade the
mechanical strength must not be used.
The freeze-dryer has to be maintained regularly (see chapter 8 "Maintenance and service").
Components that are not in a perfect state must be replaced immediately.
•Ensure that the freeze-dryer was set up and connected properly (see
chapter 5 - "Set-up and connection").
•Connections to customer-provided pipes must be force- and torque-
free.
•Maintain a safety distance of at least 30 cm (12 inches) around the
freeze-dryer.
•Do not store any dangerous goods in the safety area of the freeze-
dryer.
•Do not stay in the safety area longer than what is absolutely necessary
for the operation of the freeze-dryer.
•Only use accessories that have been approved by the manufacturer
(except for commercial vessels made of glass or synthetic materials).
We explicitly warn against the use of equipment of poor quality.
Breaking glass or bursting vessels can cause dangerous situations.
•Observe the instructions on the installation of accessories (see the
separate document).
•Ensure that the local mains voltage matches the nominal voltage that is
stated on the name plate.
•Do not place any dangerous material, e.g. glass vessels containing
liquid substances, within the safety area of 30 cm around the freezedryer. Spilled liquids may get into the freeze-dryer and damage the
electrical or mechanical components.
•Work on the power supply system must only be performed by certified
electricians.
•Inspect the electrical equipment of the unit regularly. Defects such as
loose or burnt cables must be eliminated immediately.
WARNING
• Do not use the freeze-dryer if it was installed incorrectly.
• Do not use the freeze-dryer without panels.
• Do not use the freeze-dryer with accessories that shows signs of
damage.
•Only use the freeze-dryer with accessories that have been approved by
the manufacturer. In case of doubt, contact the manufacturer (see
chapter 7.3 - "Service contact").
• Do not hit or move the freeze-dryer during its operation.
• Do not lean against or rest on the freeze-dryer during its operation.
• Check the freeze-dryer and the accessories before every start-up for
any visible signs of damage.
•Do not dry any substances that could damage the material of the ice
condenser chamber, drying chamber, lid, or accessories in any way,
e.g. highly corrosive substances such as hydrogen chloride (HCl).
•Stop the freeze-dryer immediately in the event of a malfunction.
Eliminate the malfunction (see chapter 7 - "Malfunctions and error
correction") or contact the after-sales service of Firma Martin Christ
Gefriertrocknungsanlagen GmbH (see chapter 7.3 - "Service contact").
•Ensure that all repairs are performed only by authorised and
specialised personnel.
• Do not use the freeze-dryer within hazardous locations where there is a
risk of explosion.
DANGER
•Wear suitable protective gloves when installing or removing
accessories. Do not reach into the ice condenser chamber without this
protection – your limbs may freeze onto the chamber walls!
DANGER
•Infectious, toxic, pathogenic, and radioactive substances must be dried
in suitable accessories. Take suitable precautions for your own safety!
•Do not dry products with a high solvent concentration or acidic
products without special protective measures or device-based
precautions (e.g. an additional cooling trap to protect the vacuum
pump). It is absolutely necessary to consult the manufacturer in these
cases (see chapter 7.3 - "Service contact").
•Special caution is necessary when handling azides, as a dangerous
explosive develops in combination with copper or nonferrous metals! It
is absolutely necessary to contact the manufacturer (see chapter 7.3 "Service contact").
WARNING
•Keep informed about local measures to avoid harmful emissions
(depending on the substances to be dried).
•As personal protective equipment, safety gloves are required for the
use of the freeze-dryer.
The materials to be dried may, however, require additional special
safety measures (e.g. drying of infectious, toxic, radioactive, or
pathogenic substances)
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surface temperatures of –85°C depending on the power.
3.6.5 Chemical and biological safety
If infectious, toxic, pathogenic, or radioactive substances are intended to be
dried, it is in the responsibility of the user to ensure that all necessary
safety regulations, guidelines, precautions, and practices are adhered to
accordingly.
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An internal system check system monitors the data transfer and sensor
signals with regard to plausibility. Errors are detected by continuous selfmonitoring of the system. Error messages are displayed in the main
window under "Process & equipment messages" ((see chapter 7.2 "Process and equipment messages")).
For the earth conductor check, there is an equipotential bonding screw on
the rear panel of the freeze-dryer. An earth conductor check can be carried
out with the aid of a suitable measuring instrument.
3.8 Procedures in the event of hazards and accidents
Hazardous electrical incident:
•Set the control switch to the "0" position in order to interrupt the power
supply completely.
Fire:
•A fire in the electrical control system must be extinguished with a CO2
fire extinguisher!
•Burning oil must be extinguished with a CO2 fire extinguisher or powder
fire extinguisher!
Electric shock:
•While ensuring your own safety, interrupt the circuit as quickly as
possible (control switch). Keep the affected persons warm and calm.
Get medical attention immediately! Check consciousness and
breathing continuously. In the case of unconsciousness of lack of
normal breathing, perform cardiopulmonary resuscitation (CPR).
Burns:
•Cool small-area burns (e.g. finger) immediately with cold water for
approximately 2 minutes.
•Do not cool if larger areas of the body surface are burnt since there is a
risk of hypothermia.
•Cover the burns loosely and in a sterile manner (e.g. with sterile
dressing).
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
Values for the freeze-dryer without a vacuum pump:
In order to ensure the protection against mechanical and climatic
influences, the guidelines of the German Federal Association for Wooden
Packages, Pallets, and Export Packaging (Bundesverband Holzpackmittel,
Paletten, Exportverpackung e.V.), the so-called HPE packaging guidelines,
must be applied when packing and storing the freeze-dryer.
•Use suitable packaging for the transport, and if at all possible, the
original packaging.
•Install all transport safety devices (see chapter 4.5 - "Transport safety
device").
•Over short distances, the freeze-dryer can be transported by a suitable
number of persons who reach under it from the sides.
•When lifting the freeze dryer, always reach under the freeze-dryer from
the side. Do not grab the unit at the plastic control panel (see figures
below).
Fig. 12: Lifting the freeze-dryer
•When setting the unit down, ensure that the feet are upright (see figures
Refrigeration problems of the freeze-dryer are often caused by insufficient
conditions at the location of use. This is why compliance with the following
conditions is absolutely mandatory!
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5 Set-up and connection
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Operate the freeze-dryer only in closed and dry rooms.
• The table must be stable and have a solid, even tabletop.
• Ensure sufficient ventilation. Do not place any paper, cloth, or similar
material behind or under the unit, since otherwise the air circulation will
be impaired.
•Keep a safety distance of at least 30 cm around the freeze-dryer so that
the vents in the unit remain fully effective.
•The ambient temperature must be in the range of +10°C to +25°C. A
potential night-time setback of the air conditioning system must be
taken into consideration.
•Prevent the room temperature from rising, for example due to closed
doors at night.
•Do not subject the freeze-dryer to thermal stress, e.g. by positioning it
near heat generators.
•Prevent thermal overload, e.g. caused by other equipment in the direct
vicinity of the freeze-dryer.
•Do not set up the vacuum pump directly next to the heat exchanger
(condenser).
•In the case of water-cooled systems, ensure that the water circuit
provides a sufficient amount of cooling water.
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CHRIST freeze-dryers are units of safety class I.
Alpha 1-4 LDplusand Alpha 2-4 LDplus units have a three-wire power
cord with a fixed cable(see chapter 10 - "Technical data").
An equipotential bonding screw is located on the back below the mains
power input (see chapter 2.1.1 - "Functional and operating elements"). This
equipotential bonding screw can be used to perform an earth conductor
check.
5.2.2 Customer-provided fuses
Typically, the freeze-dryer must be protected with 16 Amp G fuses that are
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.
It is absolutely essential to comply with the manufacturer’s instructions in
the separate operating manual of the vacuum sensor!
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5.4 Vacuum sensor
In order to protect the vacuum sensor against transport damage, it comes
supplied in its original packaging. Prior to commissioning the freeze-dryer,
the sensor must be installed.
Fig. 14: Position of the vacuum sensor and the connection socket
• Switch the unit off by actuating the mains power switch.
• Take the vacuum sensor out of its original packaging and fasten it to the
connector with a bow-shaped connecting piece, two clamping rings
(DIN16KF) and two centring rings (included in the scope of supply).
•Plug the connector to the connection socket and hand-tighten the
screws on the connector.
It is absolutely essential to refer to the separate instruction manual of the
vacuum pump and exhaust filter (if applicable)!
NOTE
The vacuum pump is supplied with power by the unit, but the maximum
current for the vacuum pump is limited. It is absolutely essential to refer to
the label of the electrical outlet for the vacuum pump (see the following
picture)!
If the current requirement of the vacuum pump is higher than the value that
is stated on the label, the pump must be supplied separately via an on-site
power socket.
1 Label indicating the
maximum current
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5.4.6 Vakuumpumpe
5.5 Vacuum pump
The vacuum pump must be connected to the vacuum connection of the unit
and to the electrical socket at the back of the unit, which is marked
accordingly (see chapter 2.1.1 - "Functional and operating elements").
Fig. 16: Indication of the maximum current for the vacuum pump (example)
The oil mist that escapes from the pump during operation must be retained
or discharged via an exhaust filter (oil mist separator).
• We strongly recommend using an oil mist separator. The filter prevents
the contamination of the air with oil mist.
• For discharging the oil mist, connect a suitable hose (RZ-2.5 and RC-6:
½", DUO 5 or DUO 10 ¾") to the exhaust connector of the vacuum
pump.
• The hose line must be laid in such a manner that any condensation
water cannot flow back into the pump. In the case of a rising hose line,
Observe the installation direction of the pressure control valve!
1 Pressure control valve
2 Vacuum pump
connection
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5.6 Pressure control valve
The pressure control valve is integrated in the suction pipe between the
vacuum pump and ice condenser chamber. During certain, specified
process phases, it interrupts the volume flow to the vacuum pump (see
chapter 2.2.1 - "General information on freeze-drying").
The rubber valves come supplied in an ungreased state. This is why a thin
layer of vacuum grease must be applied to the connector of the freezedryer as well as to the vessel connector prior to start-up in order to ensure
trouble-free operation.
The rubber valves (part no. 121860) enable the connection of round-bottom
flasks, wide-neck filter bottles, or distributors for ampoules to a manifold or
drying chamber. Depending on the connector of the components, the blue
plug can be removed.
Fig. 18: Rubber valve
In position A (see figure below), the aeration connector is open and the
vessel connector is closed. The accessory will be aerated while the vacuum
inside the drying chamber is maintained. As a result, vessels can be
exchanged without any interruption of the drying process.
In position B, the aeration connector is closed and the vessel connector is
open. The connected accessory is connected to the freeze-dryer.
In position C, the aeration connector and the vessel connector are closed.
The control system LDplus ("Lyo Display plus") was specifically developed
for the control of freeze-drying processes. The clear user interface enables
the intuitive operation of the unit.
Fig. 20: Start screen of the LDplus control system
Fig. 21: User interface of the LDplus control system
Function keys (1+2)
Function keys are keys whose function depends on the menu and
operating state of the unit. The current function is displayed directly next to
the key in the field with a black background.
Fig. 22: Indication of the current functions of the function keys; here, on the left, the "mode"
function and on the right the "menu" function.
"Up" and "down" keys (3+4)
These keys are used to select the functions and values that are available in
the menu or to change the selected parameters.
In addition, these keys also control the indication of the measurement value
channels in the value windows. The "up" key is assigned to the left value
window, whereas the "down" key controls the right value window.
• For a selection, press the "up" or "down" key repeatedly until the
desired measurement value channel is indicated in the respective value
window.
The main window of the display is divided into the value windows, an area
indicating the current function of the function keys, and a status line. The
main window displays all of the relevant process data, such as set and
actual values, menus, and process information (see the illustration).
Fig. 23: Layout of the LDplus control system display
Value windows (6)
The value windows are displayed after the initialisation of the control
system. There are two value windows with an identical layout. The
indication of the measurement value channels is controlled by way of the
"up" and "down" keys (see above).
Fig. 24: Value windows
The available measurement values can be displayed in the left as well as in
the right value window so that a combination of the following values can be
selected:
• Total time (indicates the total runtime of the process)
• Section time (indicates the runtime of an individual phase, e.g. freezing,
warm-up of the vacuum pump, or main drying)
• Ice condenser temperature
• Vacuum in mbar (indicates the vacuum in the drying chamber; only
possible if a vacuum sensor is installed)
• Vacuum converted into °C (indicates the vacuum inside the drying
chamber, converted based on the vapour pressure curve for ice and
water, see chapter 2.2.1 - "General information on freeze-drying"; only
possible if a vacuum sensor is installed)
Current function of the function keys (7)
See function keys (1+2)
operating state
14 Active phase
15 Symbol of pending
information
The freeze-dryer is in the standby mode. All of the various
units are switched off.
The freeze-dryer is in the run mode. The unit performs a
continuous run.
The freeze-dryer is in the run mode. The timer is activated.
Freezing
The ice condenser is cooled.
Warm-up
VP
The ice condenser is cooled and the vacuum pump is
activated while the pressure control valve is closed. If no
pressure control valve is integrated, the drying chamber
must be separated from the vacuum pump by way of a
manual valve or similar.
Main drying
The drying chamber is evacuated while the ice condenser is
cooled. If a vacuum control system is included, the vacuum
is controlled based on the corresponding set value for the
main drying phase.
Final drying
The final drying phase is only available if a vacuum control
system is included. It is possible to define different control
parameters (set vacuum, timer) for the main drying and final
drying phases.
The symbol flashes every second if there is pending
information concerning the process or the freeze-dryer (error
messages, process messages, or general information).
The information can be viewed under "Process & equipment
info" (see chapter 6.5.3.3 - "Process and equipment
information")
Status line (8)
The status line at the bottom of the screen indicates the current operating
state, active phase, and any pending information. The status line is visible
at all times.
It is possible to specify an automatic phase change from "Freezing" to
"Warm-up vacuum pump" (seechapter 6.5.3.4 - "Options" / Settings /
Automatic phase change).
NOTE
The set values for the "Final Drying" phase are only available if the
optional pressure control system is installed.
NOTE
It is possible to specify an automatic phase change from "Main drying" to
"Final drying" (seechapter 6.5.3.4 - "Options" / Settings / Automatic phase
change).
NOTE
For this set value, the optional vacuum control system must be installed.
Set values for the "freezing" phase
Timer
The timer is used to define the duration of the phase. Settings between one
minute and 200 hours are possible. If, when starting at 00:00 h:m, the
"down" key is pressed, the symbol will appear. It indicates that the timer
is deactivated and that the freeze-dryer is in the continuous mode.
After the preselected time has elapsed, the system enquires as to whether
the next phase is to be started.
Set values for the phases "Main drying" and "Final drying"
Timer
The timer is used to define the duration of the phase. Settings between one
minute and 200 hours are possible. If, when starting at 00:00 h:m, the
"down" key is pressed, the symbol will appear. It indicates that the timer
is deactivated and that the freeze-dryer is in the continuous mode.
Vacuum
The range of possible values goes from 6.1 mbar to 0.0010 mbar,
converted into steps of 1°C in accordance with the vapour pressure curve
for ice and water (see chapter 2.2.1 - "General information on freeze-
The freeze-dryer is equipped with one or several optional accessories. The
components can be controlled by way of this function.
• Select the "Special functions" function in the main menu.
• Select the option by way of the up/down keys. The selected value will
be displayed in a selection frame.
Fig. 34: "Special functions" menu
• Confirm with the right function key "enter". The possible functions will be
displayed.
• If an option is selected that is not installed, a corresponding message
will be displayed:
Fig. 35: Message if an option is not available
Defrosting the ice condenser
As standard, the freeze-dryer is equipped with a defrosting system. The ice
condenser chamber is supplied with heat that melts the ice off the ice
condenser.
The freeze-dryer must be in the standby mode and completely aerated.
• The defrosting time and temperature can be set in the main menu under
"Options" (see chapter 6.5.3.4 - "Options").
• Select the function "Defrosting ice condenser" under "Special functions"
in the main menu (see above).
• Start the defrosting process by way of the right function key "start".
The progress of the defrosting process will be displayed in a dialogue box.
Fig. 36: Progress bar of the defrosting process
When the specified defrosting time has elapsed, the defrosting process will
be stopped. The dialogue box disappears automatically.
The menu "Process & equipment info" provides the user with information
concerning error, process, and system messages.
In the event of a message, a sound signal will be issued, the symbol " "
will appear on the status line, and the process and equipment information
window will be displayed. If the user is currently in a menu, the window will
not be displayed until the user exits the main menu.
Fig. 38: Structure of the "Process & equipment info" menu
Regardless of the presence of a message, the menu can be activated at all
times in order to view any messages that are present.
• Select the "Process & equipment info" function in the main menu.
All of the information that is displayed receives a certain status:
The sound signal is issued until all of the information has been
acknowledged.
If the cause of the message is no longer present and if the information has
been acknowledged it will be removed from the process and equipment
information window.
The menu cannot be exited by way of the left function key "back" until all of
the information has been acknowledged.
The following values can be adjusted in the "Options" menu:
• Display contrast
• Language
• Settings
• Service menu
Fig. 39: "Options" menu
Changing the display contrast
• Select the menu "Change display contrast".
• Adjust the contrast by way of the up/down keys.
• Confirm the entry with the right function key "ok".
The vacuum checks must be carried out when the ice condenser is frozen.
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7 Malfunctions and error correction
Malfunctions are displayed in the dialog box "Process & equipment
messages" (see chapter 6.5.3.3 - "Process and equipment information").
An acoustic signal sounds when an error message is generated.
• Eliminate the source of the problem (see the following chapter).
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• Acknowledge the error message.
The control system continues with the process after a power failure. The
preselected conditions remain saved even during a process run.
In the event of a power failure in the drying phase, the batch may become
unusable. Whether the batch can be saved or not depends on the drying
phase in which the product was when the power failure occurred.
• In the final drying phase, the product has reached a residual moisture
content of approx. 5%. Below this value, the product is generally not
damaged even if the power failure lasts for a longer period of time.
• If the product is in the main drying phase, we recommend aerating the
unit, removing the product, and storing it in a deep-freeze. The
defrosted condensate must be drained off prior to the next start.
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7.1.2.2 Aeration and media drain valve
A malfunction of the aeration and media drain valve may have several
causes. One potential source are contaminants such as product residues
within the valve.
• Switch the freeze-dryer off and disconnect the mains plug.
• Clean the valve (see chapter 8.1.1.2 - "Aeration valve, media drain
valve").
• Put the freeze-dryer into operation again.
If there is still a leakage, the freeze-dryer must be checked by qualified
The inspection of the valve must be carried out by qualified specialist
personnel (see chapter 7.3 - "Service contact").
CAUTION
Ensure sufficient ventilation. Do not place any paper, cloth, or similar
material behind or under the unit, since otherwise the air circulation will be
impaired.
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pump are OK.
7.1.3 Insufficient ice condenser temperature
The refrigeration unit is equipped with a protective device against
overpressure in the refrigeration system and with a thermal motor
protection switch.
The protective devices trip
• when the ambient temperature is too high
• when the air circulation of the heat exchanger of the refrigeration
system is insufficient
• when the refrigeration system is overloaded.
In these cases, the refrigeration unit will be switched off automatically. If the
permissible operating conditions are re-established after a cool-down
The value of 6.11 mbar is not reached
within 15 minutes with an open pressure
control valve. The pressure control valve
will be closed and the vacuum pump will
be switched off.
•The aeration and media drain
valves are soiled.
•The small flange connections
are not properly connected.
• A seal is soiled or damaged.
• The cover or drying chamber is
not properly attached.
•The ground-in stopper is not
inserted correctly or it is
missing.
•The vacuum pump is switched
off or defective.
•Clean the valve (see chapter
8.1.1.2 - "Aeration valve, media
drain valve") and replace it if
necessary.
•Loosen the connection. Place
the centring ring with the inner
sealing ring in a centred manner
between the flange connections
and connect it with the clamping
ring. Ensure that the centring
ring neither slips out of place nor
gets jammed.
•Clean the seal and replace it if
necessary.
•Check the cover and drying
chamber.
•Grease the ground-in stopper
evenly and over the entire
sealing surface with vacuum
grease and install it.
•Switch the vacuum pump on.
Refer to the separate instruction
manual of the vacuum pump.
Defective vacuum sensor
The control system registers an invalid
measurement value.
•The vacuum sensor is not
connected correctly.
• The calibration is faulty.
• The vacuum sensor is soiled
(e.g. due to water residues).
•The vacuum sensor is
defective.
•Check the vacuum sensor
connectors.
•Calibrate the vacuum sensor
(see the separate operating
instructions of the vacuum
sensor).
• Clean the vacuum sensor.
• Check the vacuum display with
the aid of a reference device (if
available).
•See chapter 7.1.2.5 - "Vacuum
sensor".
Overpressure of refrigeration unit 1
•The overpressure switch of the
refrigeration unit has tripped.
• Let the freeze-dryer cool down.
• Ensure sufficient air circulation
(see chapter 7.1.3 - "Insufficient
ice condenser temperature").
phase of several minutes, the refrigeration unit will be switched on again
automatically.
The malfunctions are displayed in the process and equipment information
window.
The minimum ice condenser temperature of approx. -55°C or approx. –
85°C (depending on the type of freeze-dryer) is reached when the ice
condenser is not loaded and the ice condenser chamber is evacuated.
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•The overpressure switch of the
refrigeration unit has tripped.
• Let the freeze-dryer cool down.
• Ensure sufficient air circulation
(see chapter 7.1.3 - "Insufficient
ice condenser temperature").
Ice condenser overtemperature
Ice condenser temperature > +65°C. All
of the units will be switched off and the
freeze-dryer will be automatically set to
standby.
•The defrosting process has
been performed with the cover
closed.
•Remove the cover and let the
freeze-dryer cool down.
Ice condenser temperature > 20°C
The ice condenser temperature rises to
a non-permissible value during the
freeze-drying process. The pressure
control valve will close automatically in
order to prevent the vacuum pump from
being damaged.
• Insufficient cooling.
• Observe the behaviour of the
refrigeration system. If
necessary, inform the service
department (see chapter 7.3 "Service contact").
Defective ice condenser temperature
sensor
•The temperature sensor is not
connected or it is defective.
•Inform the service department
(see chapter 7.3 - "Service
contact").
Defective temperature sensor of the
defrosting heater
•The temperature sensor is not
connected or it is defective.
•Inform the service department
(see chapter 7.3 - "Service
contact").
Mains power failure (see chapter 7.1.1
- "Power failure")
•The power supply has been
interrupted.
•The mains power connector is
not connected.
• The fuses have tripped.
• The mains power switch has
been switched off.
• Check the mains fuse.
• Connect the mains power
connector firmly.
•Check the customer-provided
fuses.
•Switch the mains power switch
on.
Default settings loaded
All of the settings have been reset to the
delivery state of the freeze-dryer.
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life and prevents premature failure.
• Use soap water or other water-soluble, mild cleaning agents for
cleaning the freeze-dryer and the accessories.
• Do not use corrosive and aggressive substances.
• Do not use solvents.
• Do not use agents with abrasive particles.
• Do not expose the freeze-dryer or its accessories to intensive UV
radiation (e.g. sunlight) or thermal stress (e.g. by heat generators).
• Do not turn the unit upside down in order to clean it.
8.1 Maintenance
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8.1.1 General
The general state of the freeze-dryer must be checked at regular intervals.
Any defects must be eliminated immediately! The following points are of
particular importance:
• dirt
• leaks
• corrosion
• bent system components
• loose screw and flange connections
• higher noise levels
• loose cables
• open cable ducts
• missing or illegible safety notes and hazard warnings
• missing or illegible inscriptions on components, pipes (direction of flow)
• 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
Please refer to the separate operating manual of the vacuum pump!
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8.1.1.3 Heat exchanger (only for air-cooled freeze-dryers)
A lamellar heat exchanger is used for cooling the refrigerant that is
compressed by the refrigeration unit. This air-cooled heat exchanger is
located at the back of the unit (see chapter 2.1.1 - "Functional and
operating elements").
Dust and dirt impair the cooling effect of the air flow. Dust on the lamellas
prevents the exchange of heat and, thereby, impairs the performance and
power of the refrigeration unit. Strong soiling may cause the unit to fail.
This is why the selected set-up location should be as clean as possible.
• Check the heat exchanger at least once per month for soiling and clean
it if necessary.
• Please contact the Christ service department if you have any queries
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8.1.2 Vacuum pump
(see chapter 7.3 - "Service contact").
The stress of the vacuum pump in conjunction with a freeze-dryer is usually
not very high. This is why the recommendations in this operating manual
may differ from the information that is provided by the pump manufacturers.
Under normal operating conditions, the following maintenance tasks
concerning the vacuum pump must be performed at regular intervals:
• Check the oil level of the vacuum pump once per week. If necessary,
top it up with oil.
• Check the running pump for any unusual noise.
• Ensure that the pump has reached its operating temperature prior to
changing the oil.
• Perform the first oil change after approximately 100 operating hours.
• The other oil changes depend on the operating conditions. In general,
an interval of 500 to 1,000 operating hours is sufficient.
• Please contact the Christ service department if you have any queries
Please refer to the separate operating manual of the vacuum pump and
the exhaust filter!
NOTE
Please refer to the separate operating manual of the vacuum sensor!
CAUTION
For the care of the accessories, special safety measures must be
considered as these are measures that will ensure operational safety at
the same time.
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8.1.3 Exhaust filter (oil mist separator)
The oil mist that is emitted by the vacuum pump in quantities that depend
on the working pressure must be led to the outside or to an exhaust hood
or similar. If this is not possible, the pump must be equipped with an
exhaust filter (oil mist separator).
• Observe the liquid level in the collecting vessel of the filter.
• Remove the condensate in time (please refer to the information
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8.1.4 Vacuum sensor
provided by the manufacturer in the separate operating manual).
The vacuum sensor has only a limited service life. Especially carboncontaining substances, e.g. alcoholic compounds, reduce the service life
extremely.
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8.1.5 Accessories
• Remove any soiling on the outside with a cloth.
Chemical reactions as well as stress-corrosion (combination of oscillating
pressure and chemical reaction) can affect or destroy the metal and plastic
parts. Barely detectable cracks on the surface can expand and weaken the
material without any visible signs.
If dangerous materials (e.g. infectious and pathogenic substances) are
used, the freeze-dryer and accessories must be disinfected.
• Check the material regularly (at least once a month) for
– cracks
– visible damage of the surface
– pressure marks
– signs of corrosion
– other changes.
• Replace any damaged components immediately for your own safety.
• Immediately rinse off the accessories if any liquids that may cause
corrosion come into contact with them.
• Clean the accessories outside the freeze-dryer once a week or
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preferably after each use.
8.2 Disinfection of the drying chamber and accessories
• Use commercially-available disinfectants such as, for example, Incidur,
Meliseptol, Sagrotan, Buraton, or Terralin (available at specialised
trade).
• The freeze-dryers and the accessories consist of various materials. A
possible incompatibility must be considered.
• Before using cleaning or decontamination agents that were not
recommended by us, contact the manufacturer to ensure that such a
procedure will not damage the freeze-dryer.
• Please contact us if you have any queries (see chapter 7.3 - "Service
contact").
In the event of service work that requires the removal of the panels, there
is a risk of electric shock or mechanical injury. Only qualified specialist
personnel is authorised to perform this service work.
NOTE
If you would like to utilise our after-sales-service, please state the type of
your freeze-dryer and its serial number.
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8.3 Service
The freeze-dryer is subject to high mechanical stress. In order to be able to
withstand this high level of stress, high-quality components were used
during the production of the freeze-dryer. Nevertheless, wear cannot be
excluded and it may not be visible from the outside.
This is why we recommend having the freeze-dryer checked by the
manufacturer during an inspection once per year.
Information and appointments:
From Germany:
Contact
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode (Germany)
Tel. +49 (0) 55 22 / 50 07-44 44
E-mail: [email protected]
Outside Germany:
Contact our agency in your country. All agencies are listed at
www.martinchrist.de [Contacts] [Foreign agencies]
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8.4 Return of defective parts
Although we exercise great care during the production of our products, it
may be necessary to return a unit or accessory to the manufacturer.
In order to ensure the quick and economical processing of returns of
freeze-dryers, rotational vacuum concentrators, spare parts, or
accessories, we require complete and extensive information concerning the
process. Please fill in the following forms completely, sign them, enclose
them with the return package, and send them together with the product to:
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50
37520 Osterode (Germany)
We will return the part/unit if no declaration of decontamination is provided!
NOTE
The part/unit must be packaged in a transport-safe manner. Please use
the original packaging for the unit, if at all possible.
If the product is dispatched to us in unsuitable packaging, you will be
charged the cost for returning it to you in new packaging.
1. Declaration of decontamination
As a certified company and due to the legal regulations for the
protection of our employees and of the environment, we are obliged to
certify the harmlessness of all incoming goods. For this purpose, we
require a declaration of decontamination.
• The form must be filled in completely and signed by authorised and
specialised personnel only.
• Affix the original form in a clearly visible manner to the outside of the
packaging.
2. Form for the return of defective parts
This form is for the product-related data. They facilitate the assignment,
and they enable the quick processing of the return. If several parts are
returned together in one packaging, please enclose a separate problem
description for every defective part.
• A detailed problem description is necessary in order to perform the
repair quickly and economically.
• Upon request, we will prepare and submit to you a cost estimate
prior to performing the repair. Please confirm such cost estimate
within 14 days. If the cost estimate has still not been confirmed after
4 weeks, we will return the defective part/unit. Please note that you
must bear the incurred costs.
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9.1 Disposal of the freeze-dryer
Martin Christ Gefriertrocknungsanlagen GmbH is a registered manufacturer
of electric and electronic devices that are solely intended for commercial
use.
The technical documentation of this freeze-dryer (e.g. circuit diagram,
cooling system ) and the safety data sheets of the manufacturers of
refrigerant and heat transfer medium is not attached to this operating
manual.
1 Left function key
2 Right function key
3 "Up" key
4 "Down" key
5 Display
NOTE
Ensure that the layer thickness of 1 to 2 cm is not exceeded, since
otherwise the drying time needs to be extended.
NOTE
Recommendation: Store the product vessels on the aluminium shelves or,
if possible, the entire rack with the shelves in the deep- freeze. The
advantage is that due to the higher cold storage capacity of the aluminium
material, the product will remain frozen for a longer period of time so that
the sample will not thaw.
Fig. 54: LDplus user interface
Step-by-step instructions – shelf drying
1 Freeze the sample separately, e.g. in a deep-freeze.
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.
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.
CAUTION
Ensure that no water gets into the pipe connection of the vacuum pump or
vacuum sensor.
NOTE
Ensure that the layer thickness of 1 to 2 cm is not exceeded, since
otherwise the drying time needs to be extended.
12 The operating panel displays the vacuum, the ice condenser
temperature, and the current operating mode.
13 The end of the process is reached when the ice condenser is no longer
loaded and when it again reaches a final temperature of approximately -
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature.
14 Switch the vacuum pump off and aerate the drying chamber via the
media drain valve or via a rubber valve.
15 Switch the unit off by actuating the mains power switch and take the
product out of the freeze-dryer.
16 Switch the unit on again and start the defrosting process (button
"Operating mode: select/start" – "Defrosting”).
17 Drain the defrosting water via the media drain valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel.
18 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
service life of the vacuum sensor.
Step-by-step instructions – drying in a flask
1 Freeze the sample separately, e.g. in a deep-freeze.
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.
NOTE
The vacuum pump always runs with maximum power.
With this type of freeze-dryer, the power of the vacuum pump cannot be
controlled.
NOTE
The drying time depends on the layer thickness of the sample, the solids
content of the sample, and the amount of heat that is supplied during the
drying process. In the case of a layer thickness of 1 cm, the freeze-drying
process usually takes 24 hours.
CAUTION
Ensure that no water gets into the pipe connection of the vacuum pump or
vacuum sensor.
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 -
50°C to -54°C. The pressure decreases as a function of the ice
condenser temperature.
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 (button
"Operating mode: select/start" – "Defrosting").
12 Drain the defrosting water via the defrosting water valve on the left-hand
side of the unit. To do so, connect a hose to the hose connector and
collect the defrosting water in a suitable vessel.
13 Keep the freeze-dryer open (i.e. without the lid or drying chamber) when
it is not in use so that moisture can evaporate. This increases the
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