Christ Freeze Dryers Operational Manual
Christ Freeze Dryers Operational Manual
Christ Freeze Dryers Operational Manual
Freeze Dryer
Order Number:
Serial Number:
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Preface
Dear customer
Congratulations on purchasing a CHRIST freeze dryer.
The freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC is equipped
with a lot of user-friendly options which make the operation easier
for you.
The newly designed ALPHA 1-4 LSC / ALPHA 2-4 LSC is a
universally usable CHRIST freeze dryer for laboratories, R&D
departments and scientific institutes. Our well proven range of
accessories allows application-oriented configuration of the
equipment for almost all types of drying processes in round bottom
flasks, dishes, ampoules, injection bottles, etc.
A special advantage is the easy-to-use and self-explaining LSC
control system (Lyo Screen Control):
- ¼ VGA-LC-Display
- graphical user interface with one knob operation („turn and
push“)
- clearly arranged overview of process data in a freeze dryer
flow sheet
- input of a maximum of 32 freeze drying programs in tabular
form (optional)
- WINDOWS-NT-based software available.
Our new freeze dryer program offers a wide range of functions for
a variety of practical applications.
We thank you for your confidence and wish you a successful
application of your freeze dryer.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Contents
1. General Information 1
1.1. Introduction ......................................................................................................1
1.2. Areas of application .........................................................................................2
1.3. Technical data of freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC .................3
1.4. Standards and regulations ...............................................................................6
1.5. Safety instructions............................................................................................6
1.5.1. CAUTION! Disconnect the mains plug! ..............................................6
1.5.2. CAUTION! Solvents!...........................................................................6
1.5.3. ADVICE! Cleaning and Maintenance of the Unit!...............................6
1.5.4. WARNING! Freezing of limbs to surfaces! .........................................6
1.5.5. NOTE! Transport instructions! ............................................................7
1.6. Prohibited freeze drying processes .................................................................8
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Contents • iii
5. LSC Control System 39
5.1. Introduction ....................................................................................................39
5.1.1. LSC control panel .............................................................................39
5.1.2. Brief description of operation............................................................40
5.2. Visual components of the LSC control system ..............................................41
5.2.1. Menu bar...........................................................................................41
5.2.2. Window area.....................................................................................42
5.2.3. Pop-up menus ..................................................................................43
5.2.4. Status bar .........................................................................................47
5.3. Function keys .................................................................................................48
5.4. Manual mode .................................................................................................49
5.4.1. Input of set values in the manual mode............................................50
5.4.2. Set values for manual freezing .........................................................51
5.4.3. Set values for manual main drying and final drying .........................52
5.4.4. Manual defrosting (option)................................................................52
5.4.5. Manual pressure increase measurement (optional) .........................53
5.4.6. Preselection ......................................................................................54
5.5. Programmer module (optional) ......................................................................55
5.5.1. General information ..........................................................................55
5.5.2. Creating a new Program...................................................................57
5.5.3. Editing a program .............................................................................57
5.5.4. Loading a program ...........................................................................60
5.5.5. Copying a program ...........................................................................61
5.5.6. Deleting a program ...........................................................................61
5.5.7. Delta t freezing/drying.......................................................................62
5.5.8. Pressure increase measurement during drying................................62
5.6. Process and equipment information system..................................................63
5.6.1. Process messages ...........................................................................64
5.7. Options...........................................................................................................66
5.7.1. Info....................................................................................................66
5.7.2. Display contrast ................................................................................66
5.7.3. Language..........................................................................................67
5.7.4. Changing the date and time .............................................................67
5.7.5. Maintenance of the freeze dryer.......................................................68
5.7.6. Maintenance intervals of the vacuum pump.....................................69
5.7.7. Process.............................................................................................69
5.7.8. Unlocking ..........................................................................................70
5.7.9. Security.............................................................................................70
5.7.10. System calibration ..........................................................................71
5.8. Integrated brief description ............................................................................72
6. Troubleshooting 73
6.1. Power failure ..................................................................................................73
6.2. Insufficient vacuum ........................................................................................73
6.3. Unit does not work .........................................................................................74
6.4. Heating unit is not activated...........................................................................75
6.5. Fan (ice condenser chamber) is not activated...............................................75
6.6. Insufficient ice condenser temperature or shelf temperature ........................75
6.7. Process and equipment information system..................................................76
6.7.1. Error messages ................................................................................76
7. Maintenance 81
7.1. Ice condenser chamber .................................................................................81
7.2. Heat exchanger..............................................................................................81
7.3. Calibration and maintenance of the vacuum sensor VSP62 .........................81
7.3.1. Maintenance of the vacuum sensor: ................................................81
7.3.2. Replacement and calibration ............................................................82
7.4. Rubber valves ................................................................................................83
iv • Contents Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
7.5. Vacuum pump ................................................................................................83
7.6. Exhaust filter ..................................................................................................84
7.7. Cleaning .........................................................................................................84
7.7.1. Cleaning the freeze dryer .................................................................84
7.7.2. Cleaning the accessories .................................................................84
7.7.3. Maintenance of the aeration valve and the drain valve....................85
7.7.4. Disinfecting the drying chamber, the lid and the accessories ..........85
7.7.5. Checks by the operator ....................................................................86
8. Options 87
8.1. Process control system LPC-32, software.....................................................87
8.2. Process control system LPC-32, software with PC hardware .......................87
8.3. Programmer module PGM 30 ........................................................................87
8.4. Extension unit HED-16 LSC...........................................................................87
8.5. LyoLog LL-1 (documentation software) .........................................................87
8.6. Pressure increase test ...................................................................................87
8.7. Lyocontrol.......................................................................................................87
8.8. Electrical lifting device....................................................................................88
8.9. Solvent-resistant version................................................................................88
8.10. IQ / OQ...........................................................................................................88
8.11. Cooling bath CB 18-40...................................................................................88
8.12. Cooling bath ...................................................................................................88
9. Enclosures 89
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Contents • v
1. General Information
1.1. Introduction
What is freeze drying (lyophilisation)?
Freeze drying means: Extraction of water from frozen material.
The drying process takes place by avoiding the liquid state through
sublimation, i.e. direct conversion from ice to vapor. This happens
under vacuum and the temperature in the product is normally less
than -10°C.
The aim of freeze drying is to obtain a readily water-soluble
product which has the same characteristics as the original product
after addition of water.
As the drying process takes place in the frozen state at very low
temperatures it is possible, for example, to dry proteins which will
not denature. Also most of the other chemical compounds will be
qualitatively and quantitatively unchanged.
Through freeze drying the product, mainly of biological origin -
such as tissues, tissue extracts, bacteria, vaccines and sera - is
transformed into a dry product. During this process enzymatic,
bacterial and chemical changes are largely avoided.
Freeze drying (lyophilisation) is the gentlest process for preserving
the biological properties of sensitive tissue and tissue components.
Lyophilisation is also the best method when drying inorganic
products – e.g. nanoscale dispersions – the particle surfaces of
which should remain unchanged.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information • 1
1.2. Areas of application
The freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC is a high-
performance universal laboratory and pre-production unit for
freeze drying of solid or liquid products in ampoules, vials, glass
flasks, plasma bottles or dishes. All operations necessary for
freeze drying can be realized in one and the same unit:
• Freezing of the products
• Freeze drying (sublimation) of the products at user-defined
temperature limit values and pressure limit values
• Final drying of the products at user-defined temperature
limits and high final vacuum for the removal of capillarily or
molecularly bound water.
The freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC is suitable for
drying bacteria and virus cultures, blood plasma, serum fractions,
antibodies, sera, vaccines and pharmaceutical products such as
chloramphenicol, streptomycin, vitamins, ferments as well as plant
extracts for biochemical tests.
2 • General Information Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
1.3. Technical data of freeze dryer
ALPHA 1-4 LSC / ALPHA 2-4 LSC
Possible shelf
temperatures when
freezing and drying
inside the ice condenser approx. -25 °C to approx. -50°C to
chamber (process A) 1): +99°C +99°C
Possible shelf
temperatures when
drying outside the ice
condenser chamber room temperature room temperature
(process B) 1): to +99°C to +99°C
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information • 3
Performance data ALPHA 1-4 LSC ALPHA 2-4 LSC
Drying in round-bottom
flasks; please notice that
the max. ice condenser
capacity is 4 kg 12 pieces or 12 pieces or
(process B): 24 pieces 24 pieces
Physical data
(without vacuum
pump):
Filling quantities:
Connection
requirements with
vacuum pump
0.4 KVA:
4 • General Information Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Performance data ALPHA 1-4 LSC ALPHA 2-4 LSC
Main fuse rating: 10.0 A 12.0 A
Equipment
connections:
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information • 5
1.4. Standards and regulations
Please refer to the enclosed EU Declaration of Conformity.
6 • General Information Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
1.5.5. NOTE! Transport instructions!
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information • 7
1.6. Prohibited freeze drying processes
1. Operation of the freeze dryer when it is not properly installed.
2. Operation of the freeze dryer without panels.
3. Operation of the freeze dryer by non-authorized personnel.
4. Operation of the freeze dryer when the shelves are not
properly installed.
5. Operation of the freeze dryer with highly corrosive substances.
It is not allowed to dry these substances, at least special safety
measures have to be observed. The corrosive substances
must not cause damage to material and or degrade the
mechanical strength of the ice condenser chamber, the drying
chamber, the lid or the accessory components.
6. Operation of the freeze dryer with accessories not allowed by
the manufacturer, except for commercial freeze drying vessels
made of glass or plastic. The user is explicitly warned against
using equipment of low quality. Breaking glass or bursting
vessels can cause dangerous situations during freeze drying.
7. Operation of the freeze dryer in hazardous locations.
8. Do not push or move the freeze dryer during operation. Do not
lean on the freeze dryer.
9. Do not place potentially dangerous material, e.g. glass vessels
containing liquids, near the freeze dryer.
10. Products which could react to the supply of high energy during
the freeze drying process must not be dried.
11. Do not freeze-dry explosive or highly flammable substances.
12. Infectious, toxic, pathogenic and radioactive substances may
only be dried in suitable vessels.
13. Substances which could damage the material of the shelves
and of the chamber must not be dried or only if special safety
measures are taken.
8 • General Information Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
2. General Information on Freeze
Drying
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information on Freeze Drying • 9
Sublimation
The principle of sublimation is briefly explained using the phase
diagram of water (freeze drying of mainly aqueous solutions, see
vapor pressure curve). If the atmospheric pressure is higher than
6.11 mbar, water passes through all three phases (solid, liquid,
gas) when the temperature is lowered or raised. At 6.11 mbar the
melting pressure curve, vapor pressure curve and sublimation
pressure curve meet in one point called triple point. At this point,
all three phases occur in parallel (simultaneously). Below this
point, i.e. when the pressure is lower than 6.11 mbar, the ice is
converted directly from a solid to a gaseous phase on reaching the
sublimation pressure curve (vapor pressure curve above ice).
1mbar = 10²Pa
10 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Conversion table "Vapor pressure above ice" (sublimation
curve)
Pressure units: 1mbar = 100Pa
1Pa = 0.01mbar
Temperature units: T = t + 273
t = T − 273
t F = 1.8 ⋅ t + 32
t − 32
t= F
1 .8
T = thermodynamic temperature K (Kelvin)
t = temperature in degree Celsius °C
tF = temperature in degree Fahrenheit °F
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information on Freeze Drying • 11
2.2. Preparation
In case the unit is equipped with a pressure control valve the
vacuum pump should be warmed up. The operating
temperature should be reached before loading the vacuum pump
with condensable gases. In this way, the service life of the vacuum
pump can be considerably extended.
The vacuum pump can be operated already during the freezing
process when the pressure control valve is closed. The vacuum
pump should be warmed up for at least 15 minutes or it should be
switched on at least 15 minutes before starting the main drying
process.
It may occur that the vacuum in the ice condenser chamber or in
the drying chamber goes up during the main drying process (e.g.
from 0.63 mbar to 0.47 mbar) although the valve to the vacuum
pump is closed. This can be explained physically by the pumping
effect of the ice condenser (“Cryo Pumping Effect”).
2.3. Freezing
Small product quantities are frozen directly inside the ice
condenser chamber of the ALPHA 1-4 LSC / ALPHA 2-4 LSC.
Larger quantities are pre-frozen in a deep-freeze.
If liquids are to be dried in bottles with a layer thickness of more
than 1 cm we recommend that pre-freezing is carried out with a
shell or spin freezing device in a cooling bath (see picture). Due to
the centrifugal force the liquid to be frozen will rise on the wall of
the bottle and freeze. With this freezing process the layer
thickness is reduced and thus the total drying period is shortened
considerably.
12 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Freezing inside the unit is not necessary if the product is pre-
frozen or stored in e. g. a deep-freeze. In this case, especially
when freeze drying small quantities, it is advisable to pre-cool the
shelves in order to avoid partial thawing during the evacuation.
Possible water residue must be removed from the ice condenser
chamber. The drain valve and the aeration valve are closed.
The ground-in stopper of the drying chamber must be greased with
high-vacuum grease!
The layer thickness of the product should not exceed 1 to 2 cm as
otherwise this has a negative effect on the duration of the drying
process.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information on Freeze Drying • 13
Warning:
Acidic products or products with a high solvent concentration
cannot be dried without special safety measures and devices,
such as an additional LN2 cooling trap for protection of the vacuum
pump (if necessary contact our company). Another possibility is to
use chemical-resistant vacuum hybrid pumps (e.g. RC-5).
14 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
During the main drying phase the moisture is removed by
sublimation, during final drying the bound moisture is removed by
desorption.
This small quantity of water vapor generated during the final drying
phase can be pumped off by the vacuum pump even when the gas
ballast valve is closed (for some hours).
In general, operation with closed gas ballast valve is not
necessary. The recommended vacuum pump reaches with open
gas ballast valve a final pressure which corresponds to the water
vapor partial pressure that can be reached.
The residual moisture of the dried product depends mainly
on:
• the temperature of the dried product during the final
drying process,
• the final vacuum reached during the final drying
process.
The end of the main drying phase is reached, when the product
temperature is nearly the same as the shelf temperature
(temperature difference between shelf and product approx. 3 K to
5 K). If the adsorptively bound water is to be removed from the
product, the final drying phase can be started.
The following picture shows the drying process for a product
containing approx. 10 % solid matter. During the first quarter of the
main drying phase 50 % of the water content is condensed. During
the next quarter of the main drying phase 50 % of the remaining
water content is condensed. This continues until the drying curve
approaches the time axis asymptotically. This typical drying curve
is due to the fact that the area of sublimation recedes into the
product and the water vapor still to be extracted has to pass
through the already dried layers. During the drying process the
inner resistance increases. Thus the drying curve is primarily
determined by the latent heat of sublimation and the water vapor
transport speed. In order to increase the specific heat conduction
properties of the product to be dried and to keep the water vapor
volume as low as possible it is necessary that drying takes place
as close as possible to the solidification point (eutectic point).
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information on Freeze Drying • 15
The drying time depends heavily on the drying vacuum. The
nearer the vacuum to the solidification point in accordance with the
vapor pressure curve above ice, the shorter the drying time.
Interesting correlations:
1.0 gram of ice at
1.0 mbar assumes a volume of 1 m³ vapor
0.1 mbar assumes a volume of 10 m³ vapor
0.01 mbar assumes a volume of 100 m³ vapor
16 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Heat transfer takes place via the heated shelves by direct contact
with the bottom of the vessel and/or by convection via the shelf
and vessel or product.
At the beginning of sublimation the transfer of heat is very effective
from the wall of the vessel to the frozen product. However, soon
an area develops which is ice-free, porous and dried and has a
corresponding temperature gradient between the wall of the vessel
and the product. The poor heat conductivity of the already dried
product can lead to an increase in temperature of the ice core. If
the core temperature rises above the solidification temperature,
the product begins to thaw. This applies especially to
inhomogeneous products and to great layer thicknesses. During
this drying phase it is important to regulate the heat supply and
control temperature and pressure precisely.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC General Information on Freeze Drying • 17
2.6. End of drying and aeration
A rough indication of the end of drying is the vacuum and the ice
condenser temperature. The ice condenser is no longer loaded
and reaches the final temperature of approx. -55°C to
-85°C. The pressure in the drying chamber decreases according to
the ice condenser temperature.
The end of the drying process is reached when the temperature of
the product and that of the shelves are about 15 to 20°C. At the
same time, both temperatures should not deviate by more than 5 K
from each other.
The vacuum pump is switched off and the drying chamber is
aerated via a rubber valve or the aeration valve. The aeration
valve can also be used to “flood” the unit with nitrogen or another
inert gas instead of using air.
Then the unit is switched off and the product is removed.
2.7. 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.
When defrosting the ice condenser with (warm) water, it is of
crucial importance that no water gets into the pipe connection for
the vacuum pump and the vacuum sensor (see figure)!
The condensate as well as the defrosting water is drained through
the drain valve at the left side of the unit. To do this, a hose is put
onto the nozzle. The condensate and the defrosting water are
collected in a vessel.
Connection pipe for vacuum sensor
18 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
3. Description of the Freeze
Drying Processes
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Description of the Freeze Drying Processes • 19
In order to seal the bottles, the shelf must be completely filled. For
small quantities, at least three spacers must be distributed evenly
on each shelf (according to the height of the bottles with inserted
rubber stoppers).
Suitable spacers are available upon request.
The product can also be dried outside the ice condenser chamber.
In this case, the product has to be frozen first, e.g. in a deep-
freeze.
Possible water residue is removed from the ice condenser
chamber. The drain valve is opened so that the water residue can
drain off. The ice condenser chamber should be wiped out if
necessary.
The refrigeration unit and the vacuum pump are activated via the
control system to pre-cool the ice condenser and to warm up the
vacuum pump. The valve is closed during the warm-up of the
vacuum pump. In case the unit is not equipped with an
electromagnetic pressure control valve, we recommend using a
manual stop valve. Without such a valve, the vacuum pump
cannot be warmed up.
The rack is set onto the base plate or onto the intermediate valve
with a base plate. In the case of small samples, it is recommended
to pre-cool the shelves in order to avoid partial thawing during the
evacuation.
The heating current is supplied to the shelves via two connection
cables with banana plugs. The connection cables are plugged into
the two sockets of the electrical leadthrough and into the holes in
the rack or in the sealing device.
20 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
To control the shelf temperature, one shelf with a measuring
sensor has to be connected. The plug of the shelf with the
measuring sensor has to be connected to the socket of the
vacuum-tight electrical leadthrough.
All shelves are supplied with the same heating power. It is not
possible to consider different heat requirements of the upper and
lower shelves. Thus, slight differences in temperature between the
shelves cannot be avoided.
When freezing and drying is performed separately outside the ice
condenser chamber, the system starts directly with the main drying
phase. In case the unit is equipped with a pressure control valve,
the vacuum pump is activated and warmed up.
As soon as the shelves with the pre-frozen samples have been put
into the unit, the unit and the drying chamber are sealed.
The main drying process has to be activated in the control system
so that the pressure control valve opens and the main drying
phase starts.
When the pressure falls below the pre-selected „Heater safety
pressure“, the heater of the shelves is activated. The heater
remains on until the nominal value of the shelf is reached.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Description of the Freeze Drying Processes • 21
3.3. Separate freezing and drying outside the ice
condenser chamber (process B) with sealing
device
Possible water residue is removed from the ice condenser
chamber. The drain valve is opened so that the water residue can
drain off. The ice condenser chamber should be wiped out if
necessary.
The refrigeration unit and the vacuum pump are activated via the
control system to pre-cool the ice condenser and to warm up the
vacuum pump. The valve is closed during the warm-up of the
vacuum pump. In case the unit is not equipped with an
electromagnetic pressure control valve, we recommend using a
manual stop valve. Without such a valve, the vacuum pump
cannot be warmed up.
The rack is set onto the base plate or onto the intermediate valve
with a base plate.
The sealing device is used to seal injection bottles under vacuum
or inert gas with serrated rubber stoppers. Depending on the type
of sealing device, the bottles are sealed on 1 to 2 shelves or on 1
to 4 shelves. To do this, the shelves are moved against each other
by a pressure plate using a spindle.
The height of the pressure plate must be adjusted according to the
height of the bottles. To do so, the threaded pin for the height
adjustment is removed. The threaded rod is screwed into the lower
shelf until its slotted head is on the same level as the rack (upper
edge).
Then the pressure plate is fastened with the threaded pin in such a
way that it will rest on top of the rubber stopper or slightly above it.
When using two or more shelves, every additional shelf is set
directly onto the rubber stoppers or slightly above them, just like
the pressure plate.
Instead of the stopper, the vacuum-tight rotary leadthrough is put
into the internal ground-in connection of the drying chamber.
Before the insertion, the ground-in surface of the leadthrough is
greased with vacuum grease.
After completion of the drying process the lever of the rotary
leadthrough is turned to the right until a resistance is felt.
In order to seal the bottles, the shelf must be completely filled. For
small quantities, at least three spacers must be distributed evenly
on each shelf (according to the height of the bottles with inserted
rubber stoppers).
Suitable spacers are available upon request.
22 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
3.4. Separate freezing and drying of liquids in flasks
(process B)
Possible water residue is removed from the ice condenser
chamber. The drain valve is opened so that the water residue can
drain off. The ice condenser chamber should be wiped out if
necessary.
The refrigeration unit and the vacuum pump are activated via the
control system to pre-cool the ice condenser and to warm up the
vacuum pump. The valve is closed during the warm-up of the
vacuum pump. In case the unit is not equipped with an
electromagnetic pressure control valve, we recommend using a
manual stop valve. Without such a valve, the vacuum pump
cannot be warmed up.
Several manifolds and attachable drying chambers with
connections for rubber valves are available for drying outside the
ice condenser chamber (see accessories catalogue). The drying
chamber with connections for rubber valves is mounted directly on
the sealing ring in the base plate. Manifolds with standard ground
joints NS 45/40 are connected via the internal ground-in
connection of the acrylic lid.
In order to ensure a vacuum-tight connection and to simplify the
removal of the accessories, the ground-in surfaces must be slightly
greased with vacuum grease before use. The accessory is then
attached and turned by 360° for an even distribution of the grease.
The ground-in surfaces have to be cleaned and greased before
any further installation of accessories.
Before the drying process can start, it is necessary to check that
all valves are closed.
The main drying process has to be activated in the control system
so that the pressure control valve opens and the main drying
phase starts.
Attention:
The frozen samples can only be connected to the valves when the
pressure has fallen below 1.030 mbar.
Liquids are frozen in flasks according to the shell freezing
principle, by hand or with a rotator. These freezing methods
reduce the layer thickness and thus also the drying time to a
considerable extent.
Most of the available manifolds and valves allow a continuous
connection and removal of flasks during the drying process. Every
connection has a stop valve and an aeration valve.
If the rubber valves or stainless steel valves are stiff, they must be
dismantled, cleaned, slightly greased with vacuum grease and
reassembled.
It is also possible to connect a distributor for 15 ampoules to every
rubber valve.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Description of the Freeze Drying Processes • 23
Using a distributor, a maximum of 15 ampoules can be
simultaneously frozen in the cooling bath and connected to the
manifold.
24 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
4. Installation and
Commissioning of the Unit
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 25
The following connections are required at the site:
4.5. Aeration
The aeration valve at the upper left side of the unit is used to
aerate the ice condenser chamber.
If penicillin bottles have to be sealed under nitrogen and not in a
vacuum, the ice condenser chamber can be flooded with nitrogen
via the hose nozzle of the aeration valve.
CAUTION! Max. 0.2bar overpressure!
26 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
4.7. Vacuum pump exhaust gases
During the main drying phase, the separate vacuum pump must be
operated with open gas ballast valve. The oil mist that is produced
is normally trapped in an exhaust filter. If this is not the case, the
oil mist has to be discharged.
A ½" hose can be connected to the exhaust flange of the vacuum
pump RZ-2 or RC-5 and a ¾" hose can be connected to the
exhaust flange of the vacuum pump DUO 5 or DUO 10. The hose
either leads into the open air or into a vent.
During installation of the pipe special care must be taken that
condensate cannot flow back into the pump. With upward leading
pipes it is safest to use a separator (Woulfe's bottle or wash bottle)
in the pipe.
We strictly recommend using an exhaust filter (oil mist separator).
This filter prevents air pollution by oil mist which is emitted by the
vacuum pump in varying quantities depending on the working
pressure.
The filter is fastened to the exhaust flange of the vacuum pump.
The filter is equipped with a pressure relief valve indicating the
saturation of the filter. The filter cartridge has to be cleaned or
replaced at the latest when the pressure relief valve is activated.
The collected oil is visible in the sight glass and discharged via the
discharging screw.
Since spring 2004, most of the vacuum pumps delivered by
CHRIST have been equipped with an automatic oil recirculation
system. This system reuses the oil separated by the exhaust filter
to feed the pump. A manual removal is no longer necessary.
(Please refer to separate operating manual of the vacuum pump!)
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 27
4.8. Initial start-up
ATTENTION! Prior to start-up, make sure that the freeze dryer has
been properly set up and installed (see section 4.1 “Site of
installation” and the following points).
Aeration valve
Drying chamber
Ø300
Ice condenser
Mains switch
Additional interface
connection
(option, sep. accessory)
Serial interface
Vacuum pump power supply
connection
Power supply connection
of pressure control valve
and stop valve
Mains fuse
Mains cable
Equipotential bonding screw for
Name plate Vacuum connection protective ground wire check and
Heat exchanger of refrigeration unit central ground connection
28 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
4.8.2. Vacuum sensor, vacuum pump and pressure control
valve connection
Connection diagram
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 29
The accessory components are connected to the ALPHA 1-4 LSC
/ ALPHA 2-4 LSC freeze dryer according to the connection
diagram. Please observe the following:
Centering rings and clamping rings with wing nuts are used as
connecting elements (small flange connections in accordance with
ISO 28403 and DIN 2861, see also the following instructions).
Small flange and centering ring Small flange with centering ring
and small flange
30 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Installation of the VSP62 vacuum sensor
The vacuum sensor has to be connected to the vacuum
connection at the back of the unit in an upright position using a
centering ring and a clamping ring. The sensor connecting cable
has to be connected to the corresponding socket at the back of the
unit.
After power-on, the vacuum sensor needs a few minutes to reach
its operating temperature.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 31
Installation of the vacuum pump
The vacuum pump has to be connected to the unit and to the
socket at the back panel of the unit.
Make sure that the vacuum exhaust gases are filtered or carried
off.
32 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
4.8.3. Installation of accessory components
Further accessories (e.g. shelves, connections for round-bottom
flasks) are added in accordance with the scope of supply.
The drying chamber or a lid is placed on top of the ice condenser
chamber.
Accessories
Process B
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 33
Process B
34 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Process B
Distributor
Drying vessel,
e.g. round bottom flask
Drying vessel,
e.g. ampoule
Drying vessel,
e.g. injection bottles
5 shelves max.,
Ø375 heated
Product dish
Connection flange
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 35
Process B
Ground-in stopper
Drying chamber
Ø300mm
Rack with
10 shelves max.,
Ø200mm
Base plate
36 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Process A
Sealing device
Acrylic lid
Drying vessel,
Shelf Ø200 e.g. injection bottle
4.8.5. Power-on
Press the mains switch on the right side of the unit to switch the
unit on.
At first, the LSC control system performs a self-test. This may take
several seconds.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Installation and Commissioning of the Unit • 37
5. LSC Control System
5.1. Introduction
LSC (Lyo Screen Control) stands for a graphical user interface that
is used to control freeze drying processes. The operation of the
unit is very easy and self-explaining with the “turn & push” button.
Most of the process data are displayed either in a detailed table or
in a clear flow diagram.
Fig. 1
1. ¼“ VGA LC display
2. Turn & push button
3. Function key “Standby”
4. Function key “Run”
5. Function key “°C mbar”
6. Function key “Lock/Unlock”
7. Help function “?”
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 39
5.1.2. Brief description of operation
The LSC control system is operated via the central turn & push
button and four function keys at both sides of the control panel
. The turn & push button is the main element for
operating the control system. Turning the turn & push button
positions the focus on the desired function in the menu or in the
window. Pressing the turn & push button activates the selected
function. Parameters (set values, etc.) are entered in the same
way.
40 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.2. Visual components of the LSC control system
The LC display is divided into the three following areas:
• Menu bar
• Window area
• Status bar
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 41
Press the button to confirm the selected menu.
42 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.2.3. Pop-up menus
There are two different types of pop-up menus: Pop-up menus that
are opened by selecting one of the main menu tabs (first-level
pop-up) and second-level pop-ups that are opened by selecting a
menu item from a first-level pop-up menu. The main menu tab is
also used to close the menu of a first-level pop-up.
Close menu
Symbol for a
second-level pop-up
Second-level pop-up
First-level pop-up
Symbol for
second-level pop-up
Close second-level
pop-up
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 43
equipment information system is an exception since this dialog box
is opened automatically by the system.
• Button:
Buttons are used to confirm or to close a window.
• Scrollbar:
The scrollbar is used to enter higher-order parameters.
• Radio button:
A radio button is used to select a certain configuration.
• Parameter field:
All other fields that can be focused are used to enter
parameters, e.g. for set values, time constants, etc.
44 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
The lower part of the window shows an animated mimic diagram
with active components (symbols). The active components of the
unit are the ice condenser, the vacuum pump, valves, the electrical
heating unit for shelves and the fan in the ice condenser chamber.
The symbols are shown completely filled-up during operation.
Anfang ALPHA1-4/2-4LSC
Fig. 11 Ice condenser and fan for ice condenser chamber are not active
Fig. 12 Ice condenser and fan for ice condenser chamber are active
The mimic diagram is always shown after the unit has been
switched on.
It is possible to jump from the mimic diagram to the values window
by selecting the menu VALUES Æ Show values window.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 45
Values window
The values window compares set values and actual values of the
running process in a clear manner.
Fig. 15 Dialog box for the configuration of six positions for actual values
46 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
The following actual values can be selected via the sub-scrollbar:
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 47
5.3. Function keys
Function key “Standby”
The function key “Standby” is used to switch off all aggregates.
This function is always available (from every opened window).
Usually, the drying process is finished with the “Standby”
function before starting the manual aeration.
48 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Fig. 18 Dialog box “Device locked!“
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 49
switch manually to the next phase without setting the unit to the
standby mode. When all desired phases are finished – usually
after the final drying phase – the process is finished by pressing
the function key “Standby” . In the manual mode, the duration of
the different phases is determined by the operator. It is not timer-
controlled.
The following phases can be selected in the manual mode:
• Freezing (Only available with process A!)
• Freezing + Warm-Up VP (process A)
Cooling IC + Warm-Up VP (process B)
• Main-drying
• Final-drying
The phase “Warm-Up VP” activates the vacuum pump with closed
pressure control valve. This phase should last for at least 20
minutes to increase the service life of the pump.
50 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Fig. 21 Dialog box for the input of set values in the manual mode
Now set the focus to the set value to be modified with and
confirm with . The editing mode is now active. The set value can
be set in defined steps with the help of . Confirm with to exit
the editing mode and to save the new set value.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 51
5.4.3. Set values for manual main drying and final drying
Fig. 25 Nominal value set for main drying and final drying
The set values “vacuum” and “safety pressure” are locked against
each other. In this way the input of inadmissible nominal values is
prevented. (Only a certain safety pressure can be selected. The
corresponding temperature of the ice pressure curve of this
pressure must be at least 5K higher than the one of the set value
for the vacuum.)
52 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
automatically after the set defrosting time (see VALUES Æ Set
Values for Manual Mode).
It is not possible to start the defrosting phase during an active
phase (freezing, main drying, final drying). The unit has to be in
the standby mode. During the defrosting process, it is not possible
to select any of the other phases (freezing, main drying, final
drying). In this case it is also necessary to switch the unit to the
standby mode first. In addition, it is important that the chamber is
completely vented, i.e. the actual vacuum value must be "Atm".
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 53
Pressure difference = actual vacuum value at the beginning of the
measurement - current actual vacuum value
Open Close
intermediate valve intermediate valve
Fig.28 Intermediate valve between the drying chamber and the ice condenser
5.4.6. Preselection
Preselection for pressure control and air injection.
All preselections will be reactivated after:
• a phase change
• a program has been loaded
• a switch-over from “Run” to “Standby”
54 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.5. Programmer module (optional)
Fig. 30 The programmer module uses the section time and the set values of the
current section and of the previous section and calculates a linear function (ramp)
for the shelf temperature and the vacuum in the drying chamber.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 55
warm-up phase. As a result, the pressure inside the chamber is
not affected.
Fig. 31 The programmer module shifts the warm-up phase into the freezing
phase so that it takes place prior to the first drying section
56 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.5.2. Creating a new Program
In order to create a new program, select a free location under
Program Æ New. Free program locations are marked by < ----
>. After the selection of a program location, the program editing
mode is activated. As a program base, the standard program
named “Christ” is created. The standard program can be
customized by changing set values or by deleting or adding
sections. The date of creation of the program is set to the current
date.
The CHRIST standard program is a suggestion for drying aqueous
solutions with a freezing point >-10°C in accordance with process
A (freezing and drying on cooled shelves inside the ice condenser
chamber).
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 57
entered. The user code is defined under OPTIONS Æ Misc. Æ
Security.
58 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
exit the editing frame, select the top focus position (section
number).
Inserting a section
This button inserts a new section at the section position in the
editing frame. The set values are copied from the selected section.
A maximum of 32 sections can be defined.
Deleting a section
This button deletes a section at the section position in the editing
frame. A program consists of at least 3 sections.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 59
Fig. 37 General program information
60 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.5.5. Copying a program
Select the program to be copied (source program location) under
PPROGRAM Æ Copy. Only program locations that actually contain
a program can be copied. If a program location is free, the
selection will be ignored. If all 32 program locations already
contain a program, the selection will be ignored, too. After the
selection of the program, a dialog box opens showing general
program information. The LSC control system suggests a free
program location as the target program location. If necessary, this
suggested location can be changed (through only free program
locations can be selected). Press to copy the source
program to the target program location. The dialog box is closed.
Select to exit the copying mode and to return to the
program selection.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 61
5.5.7. Delta t freezing/drying
Preselection of the maximum admissible difference between the
shelf temperature and the product temperature at the end of a
section. The unit only switches to the next process phase if the
actual difference is below the set value.
If, for example, the shelf temperature during the freezing process
is set to -40°C and a product temperature of at least -30°C has to
be ensured before the “main drying” process can start, the
admissible difference is +10K. In this case, enter “10” for the set
value for delta t freezing.
If, for example, the shelf temperature during the drying process is
set to +20°C and a product temperature of at least +15°C has to
be ensured before the “final drying” process can start, the
admissible difference is 5K.
If the difference is not reached within the preset section time, the
section will continue until either the value is reached or the value
falls below or exceeds the set value. A corresponding message is
displayed in the process and equipment information system.
The temperature difference can be set in a range between 1 and
25. In order to ensure the beginning of the next process step,
select a temperature difference that is not too small.
“delta t freezing” is measured by the temperature sensor “actual
value product 1“. If the measurement is not desired or if it is not
possible to use any product sensors, the measurement can be
deactivated by selecting “OFF“ as the set value.
62 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Test time
During the test, the ice condenser is separated from the drying
chamber. The pressure increase is analyzed after the test time.
If the pressure increase has to be measured during the execution
of the program, the corresponding option checkbox must be
selected.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 63
Current error/message code Total number of
errors and messages
Description
Error/message status
Code 03
Safety pressure was fall below and exceeded again
during the drying process.
The error message is displayed if the pressure has fallen below
the preset safety pressure and has then exceeded it. Please check
whether the preset value for the safety pressure is too low or the
preset value for the quantity of the sample to be dried or the shelf
temperature are too high. In this case, the temperature of the ice
condenser may rise too high because of the high load.
Code 20
Alarm Lyo Control Rx
LyoRx value is out of range. Shelf heating is turned off.
Code 21
Product to wet. Section was extended
64 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
This error message is displayed if the program fails to perform two
successful pressure increase measurements in a row at the end of
a section. The section is extended.
Code 22
Note: dT Freezing/Drying
Producttemp.1 ist out of limit at section end.
See also chapter 5.5.7 “Delta t freezing/drying”
Code 24
Maintenance interval reached. Perform maintenance
or contact local service.
See also section 5.7.5 “Maintenance of the freeze dryer”
Code 25
Shelf temperature has not been reached at section
end.
Only in the programmer module! This message is displayed if the
shelf temperature differs in an inadmissible way from the set value
for the shelf temperature at the end of a section.
Code 26
Program finished.
Only in the programmer module! The program run has been
completed.
Code 29
Maintenance of the vaccum pump is necessary.
Please maintenance the vacuum pump and reset the
working hour meter.
It is possible to set a maintenance interval for the vacuum pump
under OPTIONS Æ Misc. Æ Vacuum Pump (see “Options”).
The message is displayed in the process and equipment
information system when maintenance is due. The message has
to be confirmed. You should now perform the required
maintenance and then reset the operating hour counter under
OPTIONS Æ Misc. Æ Vacuum Pump.
Code 43
Water in ice condenser chamber
There is still water in the ice condenser chamber.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 65
5.7. Options
The OPTIONS menu is used to enter elementary configurations of
the control system.
5.7.1. Info
Select the menu item Info to open the process and equipment
information system. Saved messages or errors can be read here.
66 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Fig. 45 Dialog box for setting the contrast
5.7.3. Language
To set a language, select OPTIONS Æ Language. Turn the turn
& push button to select the corresponding flag and confirm it
with . Afterwards the mimic diagram is shown using the new
language.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 67
Set the current values for day, month and year und confirm these
settings with .
Fig. 48 Dialog box showing the maintenance intervals of the freeze dryer
68 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.7.6. Maintenance intervals of the vacuum pump
The maintenance intervals of the vacuum pump can be defined
and reset under OPTIONS Æ Misc. Æ Vacuum Pump.
The following maintenance intervals can be selected: 100, 200,
300, 400, 500, 1000, 2000, 3000, 4000 hours. If the interval is set
to ∞ hours, the system will never display any maintenance
messages.
Fig. 49 Dialog box showing the maintenance intervals of the vacuum pump
5.7.7. Process
This dialog box can be opened under OPTIONS Æ Misc. Æ
Process. It is used to preset the type of process (see chapter 3).
The mimic diagram of the unit changes accordingly. If process B is
selected, the phase Manual freezing is no longer available
since the product is frozen outside the unit (e.g. in a deep-freeze).
The phase Manual cooling IC + warm-up VP is still
available in process B since it is used mainly to warm-up the
vacuum pump and to precool the ice condenser.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 69
Fig. 51 Mimic diagram process A
5.7.8. Unlocking
This dialog box can be opened under OPTIONS Æ Misc. Æ
Unlock. A six-digit keyword has to be entered.
5.7.9. Security
The menu item OPTIONS Æ Misc. Æ Security is used to
define a four-digit user code to protect the program data against
unauthorized access. First, a dialog box opens. It is used to enter
the current user code. A new code can only be defined after this
current code has been entered correctly. The new code is valid for
all program data!
In the supply state, the user code is "ØØØØ".
70 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Fig. 54 Dialog box for entering the old user code
Fig. 55 Dialog box for the entering the new user code
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC LSC Control System • 71
Two calibrations are possible: the calibration of the IO sensor card
and the calibration of external measuring modules (Pirani and Lyo
Control).
LSC Sensor IO
The LSC sensor IO card processes analog measuring signals
such that they can be processed by the control system in the form
of digital signals. The calibration is performed once at the factory.
PT 100 temperature sensors
In order to adjust the PT100 sensors of the freeze dryer, the "LSC
Temperature Adjustment Tool" (part no. 135504) is required.
72 • LSC Control System Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
6. Troubleshooting
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Troubleshooting • 73
Please proceed in the same way in case of a leak in the aeration
valve.
Check the lid seal for dirt or damage. If necessary, it must be
cleaned or replaced.
Ensure that the entire surface of the ground-in stopper of the
attachable drying chamber is greased with vacuum grease.
When using drying chambers with several connections for rubber
valves, the valves should be removed and the connections should
be sealed with rubber stoppers. To check the valves, they are
connected one after the other and tested under vacuum.
Check the vacuum sensor for soiling, e.g. water residues.
The vacuum sensor has a limited life time due to its design
principle. Vacuum sensors are available as spare parts (VSP62,
part no. 125468).
Check the vacuum display with a suitable testing unit (if available).
In order to locate a possible leak, we recommend that the vacuum
measuring sensor is directly connected to the inlet side of the
vacuum pump. If the warm vacuum pump reaches a final pressure
of at least 0.011 mbar, the vacuum pump and the measuring
system can be considered as being in working order. There is
probably a leak in the unit if the insufficient vacuum is not caused
by an insufficient ice condenser temperature.
Check the oil level in the vacuum pump, change the oil if it is
contaminated and carry out pressure test.
If the above-mentioned steps show no result, the next step is to
check all of the small flange connections (see chapter 4.8.2) and
especially the position of the centering rings. It is usually not
necessary to grease the sealing rings with high-vacuum grease.
The vacuum pump does not switch on:
The vacuum pump is equipped with a protective switch for the
drive motor.
(Please refer to the separate operating manual of the vacuum
pump.)
General information:
The vacuum checks should be carried out when the ice condenser
is deep-frozen.
74 • Troubleshooting Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Check the internal fuse 202F3.
Internal fuses
The internal fuses 202F1, 202F2 und 202F3 are located behind
the left side panel. Switch the unit off and disconnect the mains
plug. Remove the left side panel of the unit.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Troubleshooting • 75
The refrigeration unit is automatically switched off in these cases.
Once the permissible operating conditions are reached again (after
a few minutes), the refrigeration unit is switched on automatically
via the motor protection switch or via the pressure switch.
Important errors are indicated by the process and equipment
information system.
The minimum ice condenser temperature of approx. -55°C or -
85°C is reached when the ice condenser is not loaded and the ice
condenser chamber is evacuated.
Sufficient air circulation is very important. Do not place any objects
behind the unit!
Code 01
Vacuum of 6.11 mbar has not been reached within
15 minutes. Vacuum pump was switched off. Vacuum
leakage or pump defective.
This error occurs when the pressure in the ice condenser chamber
has not reached 6.11 mbar after 15 minutes of operation with open
pressure control valve. There must be a vacuum leak in the
system. The pump is switched off to avoid it pumping against the
atmospheric pressure. The cause may be a vacuum leak (aeration
valve or drain valve not closed, lid or drying chamber not mounted
in a vacuum-tight way, missing ground-in stopper in the lid or in
the drying chamber) or a defect of the vacuum pump (check
whether the mains switch of the vacuum pump is switched on).
The pressure control valve is closed and the vacuum pump is
switched off. Please eliminate the error and confirm the message
afterwards.
Code 02
Safety pressure has not been reached within 20
minutes.
This error occurs when the preset safety pressure is not reached
within 20 minutes after the start of the vacuum pump (with open
pressure control valve). Please check whether the value set for the
safety pressure is too low.
Code 03
See chapter 5.6.1.
76 • Troubleshooting Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Code 04
Excess temperature “ice condenser”. Temperature
“ice condenser” is 65°C or more! Freeze Dryer was
switched into Standby.
This error occurs when the temperature of the ice condenser
exceeds +65°C. At the same time, all active units are switched off,
i.e. the system is automatically switched to standby mode. The
error message may occur when the temperature of the ice
condenser exceeds +65°C when defrosting the system. The
refrigeration unit is switched off in order to avoid an operation or a
start at too high temperatures. The unit cannot be reactivated until
the ice condenser temperature is lower than +65°C and after
confirmation of the error message.
Code 21
See chapter 5.6.1.
Code 22
See chapter 5.6.1.
Code 23
AC power failure
A power failure is detected if the voltage supply is interrupted
under operating conditions (running mode). The process is
resumed when the voltage supply is available again.
Code 24
See chapter 5.6.1.
Code 25
See chapter 5.6.1.
Code 26
See chapter 5.6.1.
Code 27
Note: Invalid Control System
Please contact our service department!
Code 28
Note: Invalid System Module
Please contact our service department!
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Troubleshooting • 77
Code 29
See chapter 5.6.1.
Code 30
Note: Error in configuration memory. Please
verify user defined parameters and check the
back-up battery.
This error message is displayed when the system is switched on
and the buffer battery power for the settings and the real-time
clock is too low. Please replace the buffer battery. Then it is
necessary to reset the clock (see chapter 5.7.4). The settings
(setpoints, etc.) - except for the modifications made in the last
operating phase - are automatically reloaded from the second
read-only memory so that they are available even after a failure of
the buffer battery. Nevertheless, it is recommended to check the
settings.
Code 31
Note: Error in configuration memory. Factory
settings were loaded! Please check the back-up
battery.
Please contact our service department!
Code 32
Overpressure refrigerator RM1.
Overpressure in the refrigeration unit RM1, released via the
pressure switch. Please check the ambient temperature, the air
circulation of the heat exchanger of the refrigeration unit and the
load of the unit.
Code 33
Overpressure refrigerator RM2.
Overpressure in the refrigeration unit RM2, released via the
pressure switch. Please check the ambient temperature, the air
circulation of the heat exchanger of the refrigeration unit and the
load of the unit.
Code 34
Overpressure refrigerator RM3.
Overpressure in the refrigeration unit RM3, released via the
pressure switch. Please check the ambient temperature, the air
circulation of the heat exchanger of the refrigeration unit and the
load of the unit.
78 • Troubleshooting Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Code 36
AC power failure L2
Power failure in phase L2. Please check the on-site fuses.
Code 37
AC power failure L3
Power failure in phase L3. Please check the on-site fuses.
Code 38
Excess temperature liquid for temperature control
shelves
The temperature-control liquid has exceeded the upper limit. The
heating unit for the temperature-control liquid is switched off. The
heating unit is not reactivated until the temperature-control liquid
has fallen below a lower limit. The limits are set in the thermostat.
Code 39
Level liquid for temperature control fall below
There is not enough temperature-control liquid in the brine
compensation reservoir.
Code 40
Temperature sensor “ice condenser” defective or
not connected.
This error occurs when the temperature sensor is not connected
properly or if it is damaged. Please contact our service
department.
Code 41
No valid vacuum value measured. Probe not
connected or probe and/or measuring electronics
defective.
This error occurs when the heating wire of the vacuum sensor is
damaged, the electronic measuring value device is defective or the
vacuum sensor is not connected properly.
Code 43
See chapter 5.6.1.
Code 44
Temperature sensor shelf heating defective
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Troubleshooting • 79
This error message is displayed, if the temperature sensor is either
not connected or defective. Please call customer service.
80 • Troubleshooting Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
7. Maintenance
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Maintenance • 81
A freeze dryer should be aerated and the dry product should be
removed at the end of the drying process. Then the system should
be defrosted with warm water (+50°C max.) while the drain valve
is open. Then the drying chamber has to be wiped dry.
Do not simply let the freeze dryer stand at room temperature for a
long period of time since this is the time during which the tungsten
wire reacts with the surrounding atmosphere!
In addition, it is recommended to evacuate the unit for approx. 30
minutes with an open gas ballast valve after defrosting and drying
in order to remove any residues which might react with the
tungsten wire.
Buttons with
protective caps for
calibrating the
vacuum sensor
82 • Maintenance Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Calibration to a specific zero reference value:
To perform the calibration, the actual pressure must be lower than
1.0x10-2 mbar. After pressing of the button labeled “set”, the actual
vacuum field of the LSC control system shows a value
corresponding to the zero adjustment value currently set (factory
setting 0.0010 mbar). The button labeled “adj” can now be used to
increment this value up to a maximum of 1.0x10-2 mbar. As of this
value, the output starts again at 0.0010mbar. When the zero
calibration value is adapted to the applied zero reference value,
the new zero reference value will be saved automatically after 5
seconds if no key is pressed and the calibration will be performed.
If from now on the “adj” button is pressed at zero pressure, the
system will be calibrated to the set zero calibration value.
If “set” is entered without any other key depression, the zero
calibration value will be shown in a purely informative manner for 5
seconds, but no calibration will be performed.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Maintenance • 83
7.6. Exhaust filter
If the unit is equipped with an exhaust filter (necessary if the
exhaust gases cannot be extracted into the open air or into a
vent), take care that the condensate in the filter does not rise too
high. The condensate is drained using a waste oil drain screw at
the filter.
(Please refer to the separate operating manual!)
7.7. Cleaning
84 • Maintenance Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
If there is the risk of toxic, radioactive or pathogenic
contamination, special safety measures must be considered
and adhered to.
Aluminium accessories are particularly prone to corrosion. A
neutral cleaning agent with a pH-value between 6 and 8 should be
used for such parts. Alkaline cleaning agents (pH > 8) must be
avoided. This increases the service life and considerably reduces
the susceptibility to corrosion.
Careful maintenance by the user increases the service life and
prevents premature failure of accessories. Damage caused by
insufficient care does not constitute a warranty claim.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Maintenance • 85
7.7.5. Checks by the operator
The operator has to ensure that the important parts of the freeze
dryer that are necessary for safety are not damaged.
86 • Maintenance Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
8. Options
8.7. Lyocontrol
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Options • 87
8.8. Electrical lifting device
Only for ALPHA 1-4/2-4 LSC GAMMA 1-16 LSC / 2-16 LSC and
DELTA 1-24 LSC / 2-24 LSC ALPHA 1-4/2-4 LDplus BETA 1-8/2-
8LDplus
8.10. IQ / OQ
88 • Options Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
9. Enclosures
Return declaration
Declaration of contamination
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Enclosures • 89
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Enclosures • 91
92 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Enclosures • 93
94 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
96 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
98 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
100 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
10. Special functions
serielle Schnittstelle Vakuummesssonde
Serial interface of vacuum measuring sensor
Interface sérielle du capteur de vide
Netzabsicherung
Ablassventil Wärmetauscher der Kälteanlage Mains fuse
Drain valve Heat exchanger of refrigeration unit Fusible
Vanne de vidange Echangeur thermique du groupe frigorifique
Netzkabel
Eiskondensatorkammer Anschluss Spannungsversorgung Drucksteuer- und Absperrventil Mains cable
Ice condenser chamber Power supply connection of pressure control and stop valve Cordon d'alimentation
Piège Connexion de l’alimentation électrique de la vanne régulatrice de pression et de la vanne d'arrêt
Aufstellplan
Layout / Plan d’arrangement