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Datasheet | Christ ALPHA 1-2 LDplus Technical data | Manualzz
Operating Manual
Freeze Dryer
ALPHA 1-4 LSC
Part. No. 102041
ALPHA 2-4 LSC
Part. No. 102042
Version 09.2006 - English
OPERATING MANUAL
ALPHA 1-4 LSC / ALPHA 2-4 LSC
Order Number:
Serial Number:
In case of inquiries please state the above numbers.
For service please contact:
MARTIN CHRIST Gefriertrocknungsanlagen GmbH
An der unteren Söse 50, D-37520 Osterode
Phone +49 (0) 5522 / 5007-25, Fax +49 (0) 5522 / 5007-12
eMail: [email protected]
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.
MARTIN CHRIST Gefriertrocknungsanlagen GmbH
An der unteren Söse 50, D-37520 Osterode
Phone +49 (0) 5522 / 5007-0, Fax +49 (0) 5522 / 5007-12,
Internet: www.martinchrist.de, eMail: [email protected]
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Contents
1.
General Information
1.1.
1.2.
1.3.
1.4.
1.5.
1.6.
2.
3.
3.2.
3.3.
3.4.
3.5.
19
Freezing and drying inside the ice condenser chamber
(process A) on a temperature-controlled shelf...............................................19
Separate freezing and drying outside the ice condenser chamber
(process B) on temperature-controlled shelves .............................................20
Separate freezing and drying outside the ice condenser chamber
(process B) with sealing device .....................................................................22
Separate freezing and drying of liquids in flasks (process B)........................23
Separate freezing and drying of liquids in ampoules (process B) .................24
Installation and Commissioning of the Unit
4.1.
4.2.
4.3.
4.4.
4.5.
4.6.
4.7.
4.8.
9
General Information on Freeze Drying ............................................................9
Preparation.....................................................................................................12
Freezing .........................................................................................................12
Main drying.....................................................................................................13
Final drying.....................................................................................................17
End of drying and aeration.............................................................................18
Defrosting.......................................................................................................18
Description of the Freeze Drying Processes
3.1.
4.
Introduction ......................................................................................................1
Areas of application .........................................................................................2
Technical data of freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC .................3
Standards and regulations ...............................................................................6
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
Prohibited freeze drying processes .................................................................8
General Information on Freeze Drying
2.1.
2.2.
2.3.
2.4.
2.5.
2.6.
2.7.
1
25
Site of installation...........................................................................................25
Mains power...................................................................................................26
Fuses on site..................................................................................................26
Checking the ground connection ...................................................................26
Aeration..........................................................................................................26
Condensate and defrosting water..................................................................26
Vacuum pump exhaust gases........................................................................27
Initial start-up..................................................................................................28
4.8.1. Functional components and control elements..................................28
4.8.2. Vacuum sensor, vacuum pump and pressure control valve
connection.........................................................................................29
4.8.3. Installation of accessory components ..............................................33
4.8.4. Preparations for freeze-drying ..........................................................37
4.8.5. Power-on ..........................................................................................37
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Contents • iii
5.
LSC Control System
5.1.
5.2.
5.3.
5.4.
5.5.
5.6.
5.7.
5.8.
6.
7.
7.4.
73
Power failure ..................................................................................................73
Insufficient vacuum ........................................................................................73
Unit does not work .........................................................................................74
Heating unit is not activated...........................................................................75
Fan (ice condenser chamber) is not activated...............................................75
Insufficient ice condenser temperature or shelf temperature ........................75
Process and equipment information system..................................................76
6.7.1. Error messages ................................................................................76
Maintenance
7.1.
7.2.
7.3.
iv • Contents
Introduction ....................................................................................................39
5.1.1. LSC control panel .............................................................................39
5.1.2. Brief description of operation............................................................40
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
Function keys .................................................................................................48
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
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
Process and equipment information system..................................................63
5.6.1. Process messages ...........................................................................64
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
Integrated brief description ............................................................................72
Troubleshooting
6.1.
6.2.
6.3.
6.4.
6.5.
6.6.
6.7.
39
81
Ice condenser chamber .................................................................................81
Heat exchanger..............................................................................................81
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
Rubber valves ................................................................................................83
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
7.5.
7.6.
7.7.
8.
Vacuum pump ................................................................................................83
Exhaust filter ..................................................................................................84
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
Options
8.1.
8.2.
8.3.
8.4.
8.5.
8.6.
8.7.
8.8.
8.9.
8.10.
8.11.
8.12.
87
Process control system LPC-32, software.....................................................87
Process control system LPC-32, software with PC hardware .......................87
Programmer module PGM 30 ........................................................................87
Extension unit HED-16 LSC...........................................................................87
LyoLog LL-1 (documentation software) .........................................................87
Pressure increase test ...................................................................................87
Lyocontrol.......................................................................................................87
Electrical lifting device....................................................................................88
Solvent-resistant version................................................................................88
IQ / OQ...........................................................................................................88
Cooling bath CB 18-40...................................................................................88
Cooling bath ...................................................................................................88
9.
Enclosures
10.
Special functions
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
89
105
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 highperformance 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
Performance data
ALPHA 1-4 LSC ALPHA 2-4 LSC
Ice condenser capacity:
4 kg max.
4 kg max.
Ice condenser
performance1):
4 kg/24 h max.
4 kg/24 h max.
Ice condenser
temperature1):
approx. –55°C
approx. –85°C
Possible shelf
temperatures when
freezing and drying
inside the ice condenser
chamber (process A) 1):
approx. -25 °C to
+99°C
approx. -50°C to
+99°C
Possible shelf
temperatures when
drying outside the ice
condenser chamber
(process B) 1):
room temperature
to +99°C
room temperature
to +99°C
Max. shelf surface area
when drying inside the
ice condenser chamber
(process A):
1 shelf
Ø200mm
0.031 m2
1 shelf
Ø200mm
0.031 m2
10 shelves,
Ø200mm
10 shelves
Ø200mm
0.031 m2
or
5 shelves,
Ø375mm
0.110 m2
0.031 m2
or
5 shelves,
Ø375mm
0.110 m2
4 shelves,
Ø250mm
0.045 m2
4 shelves,
Ø250mm
0.045 m2
Max. shelf surface area
when drying outside the
ice condenser chamber
(process B):
Max. shelf surface area
when drying in glass
vials with sealing under
vacuum or nitrogen
atmosphere outside the
ice condenser chamber
(process B):
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
(process B):
12 pieces or
24 pieces
12 pieces or
24 pieces
Dimensions of the unit:
width: 390 mm
height: 415 mm
depth: 555 mm
(incl. vacuum
flange connection)
width: 390 mm
height: 415 mm
depth: 555 mm
(incl. vacuum
flange connection)
Weight:
approx. 48 kg
approx. 60 kg
Noise emissions
according to DIN 45635:
54 dB(A)
54 dB(A)
Electromagnetic
compatibility according
to EN 55011:
class B
class B
see label on the
back of the unit
see label on the
back of the unit
Supply voltage:
230 V / 50 Hz
(others upon
request)
230 V / 50 Hz
(others upon
request)
Power rating:
1.6 KW
1.8 KW
Max. current
consumption:
8.0 A
11.0 A
Physical data
(without vacuum
pump):
Filling quantities:
Refrigerant:
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
Ambient temperature1):
+10°C to +25°C
(higher
temperatures
upon request)
+10°C to +25°C
(higher
temperatures
upon request)
Vacuum connection:
Small flange
connection
DN 25KF
(ISO 28403,
DIN 2861)
Small flange
connection
DN 25KF
(ISO 28403,
DIN 2861)
Drain valve:
Hose nozzle
DN10 (outside
diameter 12 mm)
Hose nozzle
DN10 (outside
diameter 12 mm)
Aeration valve:
Hose nozzle DN4
(outside diameter
8 mm) max. 0.2
bar overpressure
Hose nozzle DN4
(outside diameter
8 mm) max. 0.2
bar overpressure
Equipment
connections:
1)
All machine specifications (especially for temperatures, power
and capacity) refer to the nominal ambient temperature of 20°C
The scope of delivery includes:
•
1 tube of high-vacuum grease
•
1 liter of vacuum pump oil (only in case a pump is
included)
•
1 set of flange components and several small parts for
service and maintenance purposes
•
0.5 m drain hose (silicone 9 x 12 mm)
•
1 operating manual and further detailed technical
documentation
•
Commissioning of the unit (inside Germany)
The scope of delivery does not include:
•
Installation of the exhaust pipe of the vacuum pump
(not necessary when using an exhaust filter).
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.
1.5. Safety instructions
1.5.1.
CAUTION! Disconnect the mains plug!
As current-carrying parts are accessible inside the unit
the mains plug must be disconnected before the side panels or the
rear panel are opened or before the control panel is removed.
For maintenance work the unit must be switched off with the mains
switch.
1.5.2.
CAUTION! Solvents!
Acidic products or products with a high solvent
concentration cannot be dried without special protective measures
and devices such as, for example, cooling trap for protection of the
vacuum pump (if necessary check with our factory). The unit can
also be damaged by corrosion.
Special caution is necessary when using azides because a
dangerous explosive develops in combination with copper or nonferrous metals! It is absolutely essential to consult our factory!
1.5.3.
ADVICE! Cleaning and Maintenance of the Unit!
For infectious, toxic, pathogenic and radioactive
substances, the danger information of the associated safety
regulations must be observed.
1.5.4.
WARNING! Freezing of limbs to surfaces!
During operation of the freeze dryer, dangerous
situations in the ice condenser chamber may arise. When putting
in the shelves, make sure that no limbs come into contact with the
condenser in the ice condenser chamber as the limbs may freeze
to the surface. The limb can only be detached from the surface by
applying heat. Liquid should not be used.
6 • General Information
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
1.5.5.
NOTE! Transport instructions!
Please keep the packaging for possible subsequent
dispatch.
The freeze dryer should be carried by two persons by holding it
underneath on both sides.
WARNING! When transporting or setting up the unit, do not hold
the unit at the plastic control panel. When putting the unit down on
a surface, there is a danger of squeezing hands or fingers.
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
2.1. General Information on Freeze Drying
Freeze drying is the gentlest process for drying products. It is
based on the physical phenomenon of sublimation, i.e. the direct
conversion from solid to gaseous state. The frozen product is dried
under vacuum without thawing. The ice condenser can also be
described as a vapor pump as the moisture which evaporates
under vacuum during drying freezes onto the ice condenser.
Consequently, the vacuum pump is only intended to remove the
air from the drying chamber (=gas pump) but not the vapor. In
order to start the sublimation process, energy must be supplied to
the product. This takes place during drying in round-bottom flasks
or wide-neck filter bottles etc. due to the much warmer
environment (direct heat contact), on unheated shelves by means
of heat radiation from the environment and directly by means of
the shelves when they are heatable. Once the “free water” has
been completely removed from the product, it is also possible to
remove the last traces of water bound by adsorption by means of a
very deep vacuum. This part of the drying process is referred to as
final drying (desorption).
The main components of a freeze dryer are:
•
Vacuum drying chamber with heating device
a) heatable and unheatable shelves for drying in dishes
b) shelves with sealing device for drying in bottles
c) rubber valves for connecting round-bottom flasks,
wide-neck filter bottles, etc.
d) manifold for connecting round-bottom flasks, wide-,
neck bottles, etc.
•
Pumps to evacuate air and water vapor
a) vacuum pump to evacuate the drying chamber
(= gas pump)
b) ice condenser with temperatures from -50°C to
-105°C (depending on the type of unit) to remove the
water vapor from the chamber
(= vapor pump)
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).
Vapor pressure curve for ice and water
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
°C
mbar
°C
mbar
°C
mbar
°C
mbar
0
6.110
-20
1.030
-40
0.120
-60
0.011
-1
5.620
-21
0.940
-41
0.110
-61
0.009
-2
5.170
-22
0.850
-42
0.100
-62
0.008
-3
4.760
-23
0.770
-43
0.090
-63
0.007
-4
4.370
-24
0.700
-44
0.080
-64
0.006
-5
4.020
-25
0.630
-45
0.070
-65
0.0054
-6
3.690
-26
0.570
-46
0.060
-66
0.0047
-7
3.380
-27
0.520
-47
0.055
-67
0.0041
-8
3.010
-28
0.470
-48
0.050
-68
0.0035
-9
2.840
-29
0.420
-49
0.045
-69
0.0030
-10
2.560
-30
0.370
-50
0.040
-70
0.0026
-11
2.380
-31
0.340
-51
0.035
-71
0.0023
-11
2.170
-32
0.310
-52
0.030
-72
0.0019
-13
1.980
-33
0.280
-53
0.025
-73
0.0017
-14
1.810
-34
0.250
-54
0.024
-74
0.0014
-15
1.650
-35
0.220
-55
0.021
-75
0.0012
-16
1.510
-36
0.200
-56
0.018
-76
0.0010
-17
1.370
-37
0.180
-57
0.016
-77
-18
1.250
-38
0.160
-58
0.014
-78
-19
1.140
-39
0.140
-59
0.012
-79
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 prefrozen 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.
2.4. Main drying
The vacuum pump is switched on.
Please note:
Defrosting during the drying process is possible (visible foaming)
when drying products containing e. g. solvents or high salt
concentrations. In this case it is necessary to freeze the product at
temperatures as low as possible, e.g. in liquid nitrogen.
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).
Special precautions are necessary when using
azides because a dangerous explosive develops in
combination with copper or non-ferrous metals! It is
absolutely essential to consult our company!
As soon as sublimation of the water vapor from the frozen product
begins, heat is extracted and consequently the product continues
to cool down.
The maximum rate of sublimation is reached at the start of the
drying process.
Depending on the rate of sublimation the ice condenser
temperature and thus the pressure in the drying chamber or ice
condenser chamber rises.
The duration of the main drying phase depends mainly on:
•
the layer thickness of the product,
•
the solid content of the product,
•
the heat supplied to the product during the drying
process,
•
the pressure inside the drying chamber during the
drying process.
With increasing pressure (not vacuum!) the rate of sublimation
rises and the drying period is shortened.
The water vapor generated during the main drying phase is not
pumped off by the vacuum pump but collected by the ice
condenser.
The purpose of the vacuum pump is to lower the partial pressure
of the non-condensable gases so that the water vapor can be
transported from the product to the ice condenser.
However, small quantities of water vapor are also pumped off by
the vacuum pump. Therefore, the vacuum pump is equipped with
a gas ballast device.
If the gas ballast valve is open, the extracted condensable vapors
will be emitted via the exhaust pipe together with air.
For this reason the gas ballast valve must be open during the main
drying phase!
The gas ballast valve can only be closed for final drying since
there is not much water vapor left during this section of the drying
process.
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
Heat supply during drying
The required heat supply to the product to be dried takes place
through direct heat contact in the drying chamber, heat conduction
through gas or through radiation. Heat transfer by direct contact
and heat conduction through gas are the most usual sources of
heat in today’s freeze dryers. The constraints caused by the
former can be seen in the following diagram.
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.
2.5. Final drying
The final pressure in the drying chamber depends on the ice
condenser temperature according to the vapor pressure curve
above ice :
e. g.
1.030 mbar correspond to -20°C
0.370 mbar correspond to -30°C
0.120 mbar correspond to -40°C
0.040 mbar correspond to -50°C
0.011 mbar correspond to -60°C
The unit is in operating condition if the temperature of the ice
condenser is lower than -50°C and the pressure is lower than
0.120 mbar.
The final pressure measured by the vacuum sensor when there is
no product in the unit and its corresponding ice temperature value
is mainly determined by the warmest place of the ice on the ice
condenser chamber. Moreover, this value is affected by residues
or parts of solvents in the product with a higher vapor pressure.
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
Max. liquid height
Connection pipe for vacuum pump
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
3.1. Freezing and drying inside the ice condenser
chamber (process A) on a temperaturecontrolled shelf
First, 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.
With the sealing device (option), injection bottles can be sealed
with serrated rubber stoppers inside the ice condenser chamber
under vacuum or inert gas. To do this, the shelves are moved
against each other by a pressure plate using a spindle. (When
drying inside the ice condenser chamber, only 1 shelf can be used.
When drying outside the ice condenser chamber, a maximum of 4
shelves can be used.)
After completion of the drying process, the lever of the rotary
leadthrough is turned to the right until a resistance is felt.
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.
3.2. Separate freezing and drying outside the ice
condenser chamber (process B) on
temperature-controlled shelves
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 deepfreeze.
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.
Temperature controlled shelf with build-in
measuring sensor PT100
(4-pole precision connector)
Intermediate valve or fan
(6-pole precision connector
Shelf 2 (middle, yellow)
Temperature-controlled shelf
without built-in measuring
sensor PT100
(“banana plug”)
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.
3.5. Separate freezing and drying of liquids in
ampoules (process B)
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 manifold is equipped with blind plugs for the connection of a
maximum of 48 ampoules. The blind plugs ensure that the
manifold can be pre-evacuated.
The first hose is clamped in the middle with the supplied hose
clamp and the blind plug is removed. The vacuum of the system is
preserved.
The liquid in the ampoule is either frozen under rotation in a
cooling bath or in a deep-freeze.
If shock-freezing is required, we recommend that freezing is
carried out in liquid nitrogen or in a cooling bath.
The ampoule is then connected to the hose and the hose clamp is
removed. Thus the partial pressure in the ampoule is suddenly
decreased and partial thawing during the evacuation process is
avoided.
One ampoule after the other is connected using this method.
The ampoules are sealed in the same way. The hose of the
ampoule to be sealed is clamped and the ampoule is sealed under
vacuum using the blow lamp.
If the ampoule breaks during sealing, the vacuum in the drying
chamber is not affected since the hose is clamped with the hose
clamp.
The remaining glass of the sealed ampoule is removed and the
hose is closed with a blind plug.
In this way, one ampoule after the other can be sealed or new
ampoules can be connected.
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
4.1. Site of installation
ATTENTION! In order to ensure the air circulation of the
heat exchanger, do not place any paper, cloths or similar items
behind the unit.
The freeze dryer should be positioned horizontally. The ambient
temperature should be between approx. +10°C and +25°C.
The refrigeration compressor of the freeze dryer is air-cooled.
Sufficient air circulation must be ensured. A distance of at least 30
cm to the wall should be kept. The unit should not be positioned
near radiators or heat sources and direct insolation must be
avoided.
In case of insufficient air circulation or too high ambient
temperatures, the temperature and the pressure in the
refrigerating system will increase. If the maximum permissible
operating pressure is exceeded, this may cause a failure of the
refrigeration 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:
4.2. Mains power
The operating voltage on the name plate must correspond to the
local supply voltage.
CHRIST freeze dryers are units of safety class I. The units ALPHA
1-4 LSC / ALPHA 2-4 LSC are equipped with a three-wire
connection cable with a 230VAC safety plug with ground contact.
4.3. Fuses on site
The freeze dryer must be protected with a 16 AG fuse.
4.4. Checking the ground connection
To check the ground conductor, there is an equipotential bonding
screw at the rear panel of the freeze dryer. A ground conductor
check can be carried out using a suitable measuring instrument.
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!
4.6. Condensate and defrosting water
The condensate and the defrosting water are discharged through
the drain valve at the lower left side of the unit. Connect the
supplied hose to the hose nozzle. The condensate and the
defrosting water are collected in a vessel.
The condensate and the defrosting water can also be directly fed
into a drain using this hose provided it can flow off freely. To
achieve this, the hose must have a steady downward slope. It
must be ensured that water does not collect in any part of the
hose. The end of the hose always has to be above the level of the
liquid in the collecting vessel. Otherwise there is the risk of water
and dirt residues being sucked into the condenser chamber if there
is a negative pressure when the drain valve is opened.
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).
4.8.1.
Functional components and control elements
Aeration valve
Drying chamber
Ø300
Ice condenser chamber
Ice condenser
Control system LSC
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
Name plate
Vacuum connection
Heat exchanger of refrigeration unit
28 • Installation and Commissioning of the Unit
Equipotential bonding screw for
protective ground wire check and
central ground connection
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
Process A (single-chamber system):
Freezing and gentle drying of low-freezing and thermolabile substances
on cooled shelves inside the ice condenser chamber (see figure 1).
Typical drying vessels::
•
Dishes
•
Injection vials (can be sealed under vacuum)
Process B (double-chamber system):
Separate freezing (e.g. in a deep-freeze) and drying outside the ice
condenser chamber (see figure 2)
Typical drying vessels:
•
Dishes
•
Injection vials (can be sealed under vacuum)
•
Round-bottom flasks, wide-neck filter bottles
•
Ampoules
1 Vacuum pump
2 Ice condenser chamber
3 Ice condenser
4 Glass lid
5 Drying chamber
6 Heatable shelf
7 Vacuum sensor
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
8 Drain valve
9 Motor- driven intermediate valve
11 Pressure control valve
12 Aeration valve
13 Rubber valve
14 Thermal insulation
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).
Information concerning the connection with centering rings
and clamping rings
Small flange connections between aggregates or hose
connections that are not mounted properly are often the reason for
serious vacuum problems.
Please loosen the connection and replace the centering ring (with
sealing ring inside) centrically between the flange connections.
Seal the connection with the clamping ring by fastening the wing
nut.
Please take care that the centering ring does not slip out of place
and that is does not get tilted.
Small flange and centering ring
Mounting of the clamping ring
30 • Installation and Commissioning of the Unit
Small flange with centering ring
and small flange
Fastening of the clamping ring
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.
Vacuum sensor VSP62
Small flange connection
Vacuum sensor connector
socket
Vacuum sensor connecting
cable
Installation of the pressure control valve
If a pressure control valve is available, it has to be mounted
between the freeze dryer and the vacuum pump. Then it has to be
plugged into the power socket at the back panel of the unit.
Vacuum pump
connection
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Pay attention to the mounting direction of
the pressure control valve and of the stop valve
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
Drying chamber Ø457
Rubber valve
Connection piece for
rubber valve to extend
the drying chamber,
18 pieces max.
Distributor
Drying vessel,
e.g. ampoule
5 shelves max.,
Ø375 heated
Drying vessel,
e.g. round bottom flask
Drying vessel,
e.g. injection bottles
Product dish
Connection flange
ALPHA 1-4 LSC
ALPHA 2-4 LSC
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
ALPHA 1-4 LSC
ALPHA 2-4 LSC
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
Shelf Ø200
Drying vessel,
e.g. injection bottle
ALPHA 1-4 LSC
ALPHA 2-4 LSC
4.8.4.
Preparations for freeze-drying
Close the aeration valve and the drain valve on the left side of the
unit.
If rubber valves are included in the system (located at the drying
chamber), they have to be closed.
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.
5.1.1.
LSC control panel
Fig. 1
1.
2.
3.
4.
5.
6.
7.
¼“ VGA LC display
Turn & push button
Function key “Standby”
Function key “Run”
Function key “°C mbar”
Function key “Lock/Unlock”
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.
The following functions are assigned to the four function keys
:
Standby
Switches the unit into the standby mode, i.e. all aggregates
are switched off. This function is always available. It is
usually used after the drying process is completed and
before the manual aeration.
Run
Activates the phase that has been pre-selected in the
“Manual” menu or starts a program. Phases are changed in
the manual mode in the RUN state. This function is only
available when all menus and windows are closed.
°C mbar
The conversion table “vapor pressure above ice“ for water
is opened in another window. This function is only
available in the mimic diagram, in the values window, in the
programmer module or during the modification of a set
value.
Lock/Unlock
The function keys
and the turn & push button are
locked against unintentional operation. The locking
function is activated by pressing the key for about two
seconds. The unlocking function is activated 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:
Fig. 2
5.2.1.
•
Menu bar
•
Window area
•
Status bar
Presentation on the LC display
Menu bar
The menu bar includes 5 menu tabs: VALUES, MANUAL,
PROGRAM, OPTIONS, ? (Help). These menu tabs offer all
configurations, parameters and operation modes of the unit.
The focus can be positioned on the desired tab by turning the turn
& push button
to the left or to the right.
Fig. 3
Moving the focus in the menu bar
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
LSC Control System • 41
Press the button
Fig. 4
to confirm the selected menu.
Selected focus in the menu bar
The system opens a pop-up menu or a new window.
Fig. 5
5.2.2.
Presentation of a pop-up menu
Window area
The main window covers the whole window area. Pop-up menus
or dialog boxes are shown in front of the main window so that the
main window is always in the background. Settings can only be
modified in the active window in the foreground. This means that
when a menu is open, the actual values in the main window
cannot be modified.
Below is a description of the different window types of the LSC
control system:
1. Pop-up menus
2. Dialog boxes
3. Main windows (covering the whole window area)
a.
Mimic diagram
b.
Values window
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
Fig. 6
First-level pop-up menu
In order to close a second-level pop-up menu, select the
button which is available in all second-level menus. The secondlevel menu is closed and the system returns to the last menu item
of the first-level pop-up menu.
Second-level pop-up
First-level pop-up
Symbol for
second-level pop-up
Close second-level
pop-up
Fig. 7
5.2.3.1.
First- and second-level pop-up menus
Dialog boxes
Dialog boxes are used to input parameters and to display
additional information (e.g. vapor pressure curve above ice, set
value changes etc.). A dialog box is usually opened by selecting a
menu item or by pressing a function key. The process and
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.
Fig. 8
Dialog box
The following control elements are included in the dialog boxes:
5.2.3.2.
•
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.
Main window
Mimic diagram
The mimic diagram shows the main process values, set values
and actual values.
The set values always refer to the pre-selected or active phase
(see status bar).
Fig. 9
44 • LSC Control System
Mimic diagram
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. 10 Mimic diagram of ALPHA 1-4 LSC / ALPHA 2-4 LSC
Example for active components:
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.
Fig. 13 Opening the 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. 14 Values window
The display of the actual values offers a special feature: The
operator can select six actual values and assign them to the
different display positions. In order to assign these six values
select the menu VALUES Æ Display configuration.
Fig. 15 Dialog box for the configuration of six positions for actual values
The 6 sub-scrollbars of the multi-scrollbar reflect the positions of
the 6 actual values in the values window.
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:
-
Time h:min
(current time)
-
Tot. h:min
(total process time)
-
Sec. h:min
(time of process phase)
-
Vacuum mbar
(actual vacuum value)
-
Condens.°C
(ice condenser temperature)
-
Shelf °C
(shelf temperature)
-
Product °C
(product temperature)
-
Lyo Rx %
(optional)
-
Lyo Prod.°C
(optional)
In case a position should not present an actual value, select
--blank-- from the sub-scrollbar.
To switch from the values window to the mimic diagram select the
menu item VALUES Æ Show mimic diagram.
Fig. 16 Opening the mimic diagram
5.2.4.
Status bar
The status bar always shows the current operating mode and the
pre-selected or active phase. In the programmer mode, it also
shows the current program section and the total program sections.
Fig. 17 Status bar in the manual mode
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.
Function key “Run”
The freeze drying process is started with the “Run” key. In the
manual mode, aggregates are switched on depending on the
selected phase. If a program has been selected beforehand, it is
started in the corresponding section. Phases are changed in the
manual mode in the RUN state. The function “Run” is only
available if all menus or windows are closed, i.e. the “Run” function
can only be activated from the values window or the mimic
diagram.
Please note that the aggregates are switched on by the control
system one after the other with a short delay. Table 1 shows the
delays for the units ALPHA 1-4 LSC and ALPHA 2-4 LSC.
ALPHA 1-4
ALPHA 2-4
Time (sec.)
Aggregate
0
Refrigeration unit 1
5
Vacuum pump
10
All other aggregates
0
Refrigeration unit 1
150
Refrigeration unit 2
155
Vacuum pump
160
All other aggregates
Table 1 Delay when switching on different aggregates
Function key “Lock/Unlock”
Press this function key for 2 seconds to lock the unit against
unintentional operation. That means that all inputs made with the
turn & push button and with the three function keys
are
ignored by the control system. The following window is displayed
instead.
48 • LSC Control System
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Fig. 18 Dialog box “Device locked!“
The control panel can be unlocked by pressing the function key
again for 2 seconds.
Function key “°C≙mbar”
This function key can be used to convert the temperature of the ice
condenser chamber or the vacuum in the drying chamber
according to the vapor pressure curve above ice by means of a
table. The conversion of the vapor pressure curve is necessary for
a better orientation and a better understanding of the correlation
between pressure and sample temperature during the freeze
drying process (see chapter 2.1). Please note that the conversion
table can only be opened if the mimic diagram, a values window or
one of the set values windows is shown. With open pop-up menus
or other dialog boxes, this function key is locked.
Fig. 19 Table for vapor pressure curve above ice
5.4. Manual mode
The manual mode enables the manual control of the process
phases: Freezing, freezing + warm-up of the vacuum pump, main
drying and final drying. In the manual mode, the set values for the
different phases have to be entered before the process start. Then
the phase has to be pre-selected. Press the function key “Run”
to start the process. When a phase is finished, the user has to
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 timercontrolled.
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.
Fig. 20 Pop-up menu for manual control
Furthermore, the pop-up menu Special functions offers the
following manual operations:
5.4.1.
•
Defrosting
•
Pressure inc. measurement (pressure increase
measurement).
•
Preselection
Input of set values in the manual mode
The set values of the process are stored in a so-called nominal
value set for each phase.
The dialog box for modifying set values can be opened via the
menu VALUES Æ Set Values for Manual Mode.
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
To enter set values, select the corresponding nominal value set
(phase) from the scrollbar. To do so, focus the scrollbar with
and confirm the selection with . The scrollbar is now in the
selection mode, i.e. the desired nominal value set can be selected
with
. The corresponding current set values of this phase are
shown. Press the confirmation key to exit the selection mode.
Fig. 22 Scrollbar in the selection 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.
Fig. 23 Editing mode for set values
5.4.2.
Set values for manual freezing
Fig. 24 Nominal value set for Freezing and Freezing + Warm-Up VP
Valid range of values:
Shelf temperature: -100°C ... +100°C
Max. range of values:
Shelf temperature: -100°C ... +100°C
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.)
Valid range of values:
Shelf:
-100°C .. +100°C
Vacuum:
0.0010 mbar ... safety pressure – 5°C
Safety pressure:
vacuum + 5°C ... 6.110 mbar and Atm
Max. range of values
Shelf:
-100°C ... +100°C
Vacuum:
0.0010mbar ... 4.020 mbar
Safety pressure:
0.0023mbar ... 6.110 mbar and Atm
The correlation between the vacuum and the temperature is
shown in the conversion table “Vapor pressure curve above ice” in
chapter 2.1.
5.4.4.
Manual defrosting (option)
To defrost the ice condenser, select the phase “Defrosting”
(Manual Æ Special Functions Æ Defrosting) and press
“Run” to start the defrosting process. During the defrosting
process, the ice condenser chamber is heated electrically by a
heating collar. To finish the defrosting process, press “Standby” .
If this button is not pressed, the defrosting process will end
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".
Fig. 26 Dialog box for manual defrosting
5.4.5.
Manual pressure increase measurement (optional)
Select (MANUAL Æ Special Functions Æ Pressure inc.
measurement) to activate the manual measurement of the
pressure increase. This feature is only available in the “Run”
mode of the main drying phase or in the “Run” mode of the final
drying phase.
Fig. 27 Dialog box for the manual pressure increase measurement
Press
to start the pressure increase measurement. During
the measurement, the intermediate valve prevents the flow of
vapor from the drying chamber to the ice condenser. The pressure
difference is displayed in accordance with the vapor pressure
curve above ice.
The pressure difference is calculated as follows:
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
intermediate valve
Fig.28
Close
intermediate valve
Intermediate valve between the drying chamber and the ice condenser
Press
to finish the pressure increase measurement. The
values for the pressure difference and the measuring time are
frozen. They are indicators for the current amount of water vapor
and thus for the residual moisture content of the product.
The pressure increase measurement stops automatically when the
test time is over or when the maximum permissible pressure
increase is exceeded.
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”
Fig. 29 Preselection menu
54 • LSC Control System
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
5.5. Programmer module (optional)
5.5.1.
General information
The programmer module PGM-30 is used for a timer-controlled
pre-programmed process (freeze-drying program).
A freeze-drying program is divided into several sections. Every
section of the program has set values for the phase, the section
time, the shelf temperature, the vacuum, the safety pressure and
dT freezing/drying. The PGM-30 can store up to 30 individual
programs. Up to 32 sections can be assigned to each program. A
program has to comprise a minimum of 3 sections.
When the programmer module executes a freeze-drying program,
it executes the created sections one after the other until the last
section is completed. The defined set values for the shelf and the
vacuum are node points that are used by the programmer module
to calculate a linear function (ramp) with the corresponding
gradient. This means that the set value does not change suddenly
at the transition from one section to the next. Instead it has a
steady ramp.
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.
The first section of a program is always “loading”. In this section,
the start values for the calculation of the function and for the shelf
temperature are defined. In general, the room temperature is
stated. If the product is pre-frozen (process B, separate freezing
and drying outside the ice condenser chamber), the corresponding
product temperature should be stated. Section 2 and all other
sections can be used for freezing, main drying and final drying,
though it is not possible to switch phases. This means, for
example, that the freezing phase cannot be selected after a main
drying section.
The time for warming up the vacuum pump (warm-up phase) is
automatically determined by the programmer module during the
freezing phase. When the vacuum pump warms up, the freezing
phase (section time) is not affected. The pressure control value is
closed when the PGM-30 activates the vacuum pump during the
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
The programmer module data “set values”, “actual values” and
“status” are shown at the usual locations in the values window, in
the mimic diagram and in the status line.
Fig. 32 Pop-up window of the programmer module
The programmer module can be activated by selecting the
Program menu. This is only possible in case no program has
been loaded so far. A pop-up menu opens and can be used to
select the desired function (load, modify, copy, delete or new
program).
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).
Fig. 33 CHRIST standard program (table)
Fig. 34 CHRIST standard program (diagram)
5.5.3.
Editing a program
An existing program can be adapted to your special freeze-drying
process under PROGRAM Æ Modify. Select the program to be
modified from the program list. If the program is locked for
unauthorized persons, an additional four-digit user code has to be
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.
Fig. 35 Dialog box for entering the user code
The programmer module always shows 3 sections in order to
make the connection with the previous and the section clear. The
first section is always defined as “loading”. In this section, the start
conditions of the program are defined. All other sections will be
executed one after another. Please note that the order of phases
of a program is always “loading”, “freezing”, “main drying” and
“final drying”. It is not possible to switch phases. Example: You
cannot have the “main drying” phase before the “freezing” phase.
Fig. 36 The program editing mode
Select the PROGRAM menu to close the programmer module. This
is necessary in order to save the modifications in the program
memory.
Modifying a Program
The section to be modified has to be selected using the scrollbar.
It is then displayed in the middle (marked by an editing frame).
After exiting the scrollbar, the focus jumps to the editing frame.
Now it is possible to modify the phases and set values. In order to
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.
Additional set values
5.5.3.1.
•
Warm-up vacuum pump
Defines the time for the warm-up of the vacuum pump.
For the warm-up, the vacuum pump is switched on
automatically by the programmer module.
•
Alarm LyoControl Rx
The value “alarm LyoControl Rx” defines the minimum
permissible value of the LyoRx sensor during the drying
process. If the actual value falls below this minimum
value, the shelf heating unit will be switched off. This
prevents the product from thawing as a result of the
excessive energy supply through the shelf temperaturecontrol system. The LyoRx value is only evaluated
during the main drying phase and during the final
drying phase.
•
dt shelf
At the end of the section, the actual temperature of the
shelf is compared to the set value. If the shelf
temperature difference is beyond the permissible range
(dt shelf), the section will be extended by the PGM-30
until the difference is in the permissible range. If the set
value for "dt shelf" is set to OFF, the shelf temperature
will not be checked at the end of the section.
•
Pressure increase test during main drying
See section 5.5.8 “Pressure increase test during main
drying”
•
Pressure increase test during final drying
See section 5.5.8 “Pressure increase test during final
drying”
General program information
The dialog box “General program information“ shows the program
name and the locking state of the program.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
LSC Control System • 59
Fig. 37 General program information
5.5.4.
Loading a program
Select the program under PROGRAM Æ Load. A dialog box
opens showing general program information. The start section and
the time for starting the section can be set as desired.
to load the program. The dialog box is closed and
Press
the status bar is updated. Press the function key “Run” to start
the program.
Fig. 38 Dialog box “Load program“
Fig. 39 Status bar in the programming mode
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.
to exit the copying mode and to return to the
Select
program selection.
Fig. 40 Dialog box “Copy program“
5.5.6.
Deleting a program
Select the program to be deleted under PROGRAM Æ Delete.
Only program locations that actually contain a program and that
are not locked can be deleted. In the case of free or locked
program locations, the selection will be ignored. After the selection
to
of the program, a confirmation dialog box opens. Press
to
delete the program. The dialog box is closed. Press
return to the program selection.
Fig. 41 Dialog box “Delete program“
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.
5.5.8.
Pressure increase measurement during drying
In the program mode, the pressure increase measurement is
always performed in the last drying phase (main drying or final
drying). The next phase only starts after two successful pressure
increase measurements in a row. In case there are no two
successful measurements at the end of the section, a message is
displayed in the process and equipment information system. The
section is extended until two measurements are performed
successfully.
Adapt the following parameters for the pressure increase
measurement:
Max. Pres. Increase
The maximum admissible pressure increase for a successful
measurement. The value is converted to K in accordance with the
vapor pressure curve above ice.
Start pres. inc. test
Start of the first pressure increase measurement since the
beginning of the last drying section.
Time between tests
Time difference between two pressure increase measurements.
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.
Fig.42
Parameters for the pressure increase measurement
5.6. Process and equipment information system
The process and equipment information system shows and saves
malfunctions and messages. In this way, short-time defects or
messages occurring overnight, for example, can be recognized the
next day. Consequential malfunctions are also saved and
displayed. The process and equipment information system is
provided with a floating relay output for a central monitoring
station.
The process and equipment information system distinguishes a
message and a process or hardware error. In the event of an error
or message, the process and equipment information system
appears automatically on the screen. Simultaneously, a sound
signal is given (5 times at 16-seconds intervals) until the error
message is confirmed. In the event of process or hardware errors,
the active operating lamp “Run” or “Standby” flashes. The
information window cannot be closed until all errors and messages
have been acknowledged.
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
Confirm
Close the process and
equipment information system
Fig. 43: Dialog box for the process and equipment information system
The following messages are displayed in the process and
equipment information system:
5.6.1.
Process messages
For messages referring to hardware errors please see chapter
6.7.1.
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.
Fig. 44 Options menu
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.
5.7.2.
Display contrast
The contrast of the LC display has to be modified depending on
the lighting conditions and the visual angle. Open the
corresponding dialog box under OPTIONS Æ Contrast. Position
and , i.e. adjust the optimum
the focus on the scrollbar with
and confirm it with . The value range for the
contrast with
contrast is restricted so that even with 0 % or 100 % the content of
the LC display can still be seen from a certain visual angle.
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.
Fig. 46 Dialog box for selecting the language
5.7.4.
Changing the date and time
The LSC control system is equipped with a built-in clock with a
buffer battery. The clock has to be reset after a failure of this buffer
battery. The time can be set under OPTIONS Æ Misc. Æ
Date/Time. The date and time that are currently set are used as
set values when the window is opened.
To set the date, proceed as follows:
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
.
To set the time, proceed as follows:
Set the current values for hour and the next minute. When the
minute changes, confirm the new setting with
. The
counter of the seconds will be reset to zero.
Example:
The current time is 10:23:15 [hour:min:sec]. Hence the time to be
set is 10:24 [hour:min]. Confirm the new setting by pressing
when the minute changes to 10:24:00 [hour:min:sec].
Fig. 47 Dialog box for date and time
5.7.5.
Maintenance of the freeze dryer
Maintenance of LSC freeze dryers is due after a maximum of 3000
operating hours or after one year after the last maintenance. When
maintenance is due, message code 24 is displayed in the process
and equipment information system. After the maintenance, reset
the counter under OPTIONS Æ Misc. Æ Maintenance by
pressing the
button. The dialog box also shows the
current number of operating hours since the last maintenance and
the date of the last maintenance in the format [month.year].
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.
Fig. 50 Dialog box for selecting a process
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
LSC Control System • 69
Fig. 51 Mimic diagram process A
Fig. 52 Mimic diagram process B
5.7.8.
Unlocking
This dialog box can be opened under OPTIONS Æ Misc. Æ
Unlock. A six-digit keyword has to be entered.
Fig. 53 Dialog box for unlocking
There will be a long sound signal (about 1 s) in case an invalid
keyword is entered. If the keyword is accepted, there will be a
short sound signal.
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
There will be a long sound signal (about 1 s) if a wrong user code
is entered. If the user code is accepted, there will be a short sound
signal.
Fig. 55 Dialog box for the entering the new user code
5.7.10. System calibration
A dialog box showing all the values that are necessary for a
calibration can be opened under OPTIONS Æ Misc. Æ
Calibration.
Fig. 56 Dialog box for calibrating the system
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.
5.8. Integrated brief description
The integrated brief description does not replace a complete
operating manual, but it can give an overview about the operation,
parameterization and operating modes of the unit.
The brief description is opened by selecting ? in the menu bar.
The system then shows a list of topics. Use the buttons
and
to browse the contents page by page. Use the
button to exit the brief description and to go back to the main
window.
Fig. 57 Contents of the brief description
72 • LSC Control System
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
6. Troubleshooting
6.1. Power failure
The control system continues with the process after a power
failure. The pre-selected conditions remain saved even during an
automatic process.
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.
It is important to distinguish between the main drying phase and
the final drying phase:
The product is in the final drying phase when the residual moisture
has reached approx. 5 %. Below this value, the product is
generally not damaged by a power failure.
If the product is in the main drying phase, we recommend aerating
the unit, taking out the product and storing it in a deep-freeze. The
defrosted condensate must be drained off prior to the next start.
6.2. Insufficient vacuum
Special attention must be paid to the high-vacuum valves. The
drain valve, the aeration valve as well as the rubber valves must
be checked.
After disconnection of the mains plug, we recommend removing
the side panels of the unit, disconnecting the hose inside the unit
from the drain valve, sealing the hose end with a rubber stopper
and evacuating the unit. If the unit now reaches the necessary
operating pressure, there is a leak in the valve. This may be
caused by residues from the drying process, fluff from cleaning
cloths or wear of the O-rings of the valve.
To eliminate this problem, we recommend evacuating and aerating
the unit through the drain valve so that any particles that the unit is
evacuated and vented by means of the drain valve so that any
deposits are removed. If necessary, the O-rings must be replaced.
If the leak cannot be eliminated in this way, the drain valve must
be cleaned or replaced.
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.
6.3. Unit does not work
If the display does not work after the mains switch has been
actuated, the following tests must be performed:
Is the mains switch plugged in?
Check the on-site fuses.
Check the automatic circuit breaker 1F1 at the back panel of
the unit.
74 • Troubleshooting
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Check the internal fuse 202F3.
6.4. Heating unit is not activated
Please note that during the main drying phase and during the final
drying phase the heating unit is not activated until the preset safety
pressure is reached.
If the heating unit is not activated even though the pressure is
below the safety pressure, please check the fuse 202F1.
6.5. Fan (ice condenser chamber) is not activated
Check the precision connection in the ice condenser chamber.
Check the internal fuse 202F2.
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.
6.6. Insufficient ice condenser temperature or shelf
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.
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!
6.7. Process and equipment information system
Process messages see chapter 5.6.1.
6.7.1.
Error messages
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
7.1. Ice condenser chamber
Before each start-up, ensure that all water residues have been
removed from the ice condenser chamber. If necessary, wipe the
ice condenser chamber dry.
Before every drying process it is recommended to open and close
the drain valve.
7.2. Heat exchanger
A laminated heat exchanger is used to cool the refrigerant
compressed by the refrigeration unit. The heat exchanger is
located at the back of the unit and should be checked for dust or
dirt residues every few months. It must be cleaned whenever
necessary. The heat exchanger can be cleaned best by brushing,
by using a vacuum cleaner from the outside or by using
compressed air from inside of the unit.
Excessive soiling of the heat exchanger leads to a decrease in
performance and may cause a failure of the unit!
Please note: The unit must not be turned upside down!
7.3. Calibration and maintenance of the vacuum
sensor VSP62
7.3.1.
Maintenance of the vacuum sensor:
The service life of the tungsten wire is limited due to the chemical
reaction with the components of the surrounding gas. Tungsten
reacts with carbon and forms tungsten carbide. As a result, the
wire gets brittle and breaks. The service life of PIRANI measuring
tubes can only be increased if they do not get into contact with
carbon-containing substances.
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.
7.3.2.
Replacement and calibration
The vacuum sensor has to be replaced if “---“ is shown in the
vacuum field after the aeration of the system instead of “Atm” and
if the process and equipment information window shows error
message 41. If after the warm-up phase and the aeration of the
unit the vacuum display still does not show “Atm” but a value like
“800“, “600“ or “400“ mbar, for example, the vacuum sensor has to
be recalibrated. The warm-up phase of the vacuum measuring
sensor takes at least 5 minutes.
Calibration of the vacuum sensor:
The vacuum sensor has two calibration buttons labeled “adj“ and
“set“. The buttons are protected by protective caps. Remove the
protective caps of the buttons prior to calibrating the sensor. Use a
small pen (max. ∅ 2.5mm) to actuate the buttons. Refit the
protective caps after the calibration.
The digital recalibration to atmospheric pressure (Atm) and zero is
possible directly at the vacuum sensor using the button labeled
“adj” (adjust). The measuring transducer automatically recognizes
the calibration point. If a zero calibration has to be performed, the
actual pressure should be lower than 5.0x10-5 mbar (factory
setting). Alternatively, the sensor can also be calibrated to a
reference value (see below). We recommend a warm-up phase of
at least 5 minutes before the calibration.
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.
7.4. Rubber valves
Special attention must be paid to the rubber valves. If the valves
are stiff, they must be dismantled, cleaned, slightly greased with
vacuum grease and reassembled.
7.5. Vacuum pump
For the maintenance of the vacuum pump, please refer to the
separate operating manual.
Additionally, we would like to emphasize the following points:
The oil level of the vacuum pump must be regularly checked at the
sight glass (in case of continuous operation at least once a week).
Top up oil to the required level via the oil inlet. Due to the
continuous operation with gas ballast, oil consumption cannot be
avoided. For topping-up see the operating manual of the pump.
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.
The first oil change must be carried out after approx. 100 operating
hours. Subsequent oil change intervals depend on the operating
conditions. In general, an oil change is necessary after approx.
500 to 1000 operating hours.
The oil change should always be carried out with warm pump.
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
7.7.1.
Cleaning the freeze dryer
Use soap water or other water-soluble, mild cleaning agents to
clean the freeze dryer. Avoid corrosive and aggressive
substances. Do not use alkaline solutions or solvents or agents
with abrasive particles. Remove product residues from the ice
condenser chamber using a cloth. It is recommended to open the
lid of the freeze dryer or of the drying chamber when the freeze
dryer is not in use so that moisture can evaporate.
If there is the risk of toxic, radioactive or pathogenic
contamination, special safety measures must be considered
and adhered to.
7.7.2.
Cleaning the accessories
When cleaning accessories, special safety measures must be
taken as these are measures to ensure operational safety and
reliability.
Chemical reactions as well as stress corrosion (combination of
changing pressure and chemical reaction) can affect or destroy the
structure of metals and plastic parts. Hardly detectable cracks on
the surface will expand and weaken the material without any
visible signs. When a visible damage of the surface, a crack, a
mark or any other change, also corrosion, is detected, the part
(shelf, vessel, drying chamber etc.) must be replaced immediately
for safety reasons.
Fans, lid seals, vessels, racks, drying chambers and shelves must
be cleaned regularly in order to avoid damage.
Cleaning of accessories should be carried out away from the
freeze dryer once a week or preferably after every use.
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.
7.7.3.
Maintenance of the aeration valve and the drain valve
Special attention must be paid to the aeration valve and the drain
valve. If residues from previous drying processes deposit on them,
the freeze dryer may malfunction. Therefore, take care that no
product or other residues will get into the pipe to the aeration valve
and to the drain valve.
7.7.4.
Disinfecting the drying chamber, the lid and the
accessories
All usual disinfectants like, for example, INCIDUR, Melisiptol,
Sagrotan, Buraton or Terralin (available through your local
laboratory supplier) can be used.
ATTENTION! Check compatibility with the lid and the drying
chamber. See also the enclosure “Chemical behavior of
PLEXIGLAS® (acrylic glass)”.
The freeze dryers and the accessories are made of different
materials. A possible incompatibility must be considered. For
autoclaving, the temperature stability of the individual materials
must be taken into consideration. Please consult us if in doubt. If
dangerous materials are used, the freeze dryer and the
accessories must be disinfected.
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.
This especially refers to:
•
Lid or drying chamber
•
Seals
•
Oil level of vacuum pump
•
Accessories, especially changes like corrosion, wear
and abrasion of material etc.
Furthermore, a ground conductor check must be carried out
regularly.
86 • Maintenance
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
8. Options
8.1. Process control system LPC-32, software
8.2. Process control system LPC-32, software with
PC hardware
8.3. Programmer module PGM 30
8.4. Extension unit HED-16 LSC
8.5. LyoLog LL-1 (documentation software)
8.6. Pressure increase test
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 1-8/28LDplus
8.9. Solvent-resistant version
8.10. IQ / OQ
8.11. Cooling bath CB 18-40
8.12. Cooling bath
Subject to technical changes.
88 • Options
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
9. Enclosures
Declaration of conformity ALPHA 1-4 / ALPHA 2-4 LSC
Operating manual of the vacuum pump (only in case of delivery)
Operating manual of the exhaust filter (only in case of delivery)
Brochure "Freeze Dryer for advanced process" (LSC Control
System
Accessories catalogue "The Accessories for Freeze Drying"
Chemical Behaviour ®Plexiglas
(material of the drying chamber and the lid)
Disinfection spray INCIDUR
(Material of all parts getting in contact with the different media)
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
Anlagensteuerung LSC
Control system LSC
Système de contrôle LSC
Netzschalter
Mains switch
Commutateur d’alimentation
Belüftungsventil
Aeration valve
Soupape de ventilation
Ablassventil
Drain valve
Vanne de vidange
Eiskondensatorkammer
Ice condenser chamber
Piège
Eiskondensator
Ice condenser
Condenseur
serielle Schnittstelle
serial interface
Interface sérielle
Anschluss Spannungsversorgung Vakuumpumpe
Vacuum pump power supply connection
Connexion de l’alimentation électrique de la pompe à vide
Vakuumanschluss
Vacuum connection
Connexion de vide
Anschluss Vakuummesssonde
Vacuum measuring sensor connection
Connexion du capteur de vide
Wärmetauscher der Kälteanlage
Heat exchanger of refrigeration unit
Echangeur thermique du groupe frigorifique
Anschluss Spannungsversorgung Drucksteuer- und Absperrventil
Power supply connection of pressure control and stop valve
Connexion de l’alimentation électrique de la vanne régulatrice de pression et de la vanne d'arrêt
Netzabsicherung
Mains fuse
Fusible
Netzkabel
Mains cable
Cordon d'alimentation
Potentialausgleichsschraube für Schutzleiterprüfung und zentraler Erdungsanschluss
Equipotential bonding screw for protective ground wire check and central ground connection
Vis d'équilibrage de potentiel pour le contrôle du conducteur de protection et pour la connexion centrale de terre.
Aufstellplan
Layout / Plan d’arrangement

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