Christ ALPHA 1-2 LDplus User manual

Version 11.2006 – English
Revision 1.2
Operating Manual
Freeze Dryer
ALPHA 1-2 LDplus
Part. No. 101521

Operating Manual Freeze Dryer ALPHA 1-2 LDplus
OPERATING MANUAL
ALPHA 1- 2 LDplus
Order Number:
Serial Number:
In case of inquiries please state the above numbers.
For service:
please use online service request form:
www.martinchrist.de →[Contacts] →[Service request]
Martin Christ Gefriertrocknungsanlagen GmbH
An der Unteren Söse 50, 37520 Osterode (Germany)
Phone [phone], Fax [phone]
eMail: [email protected]

Operating Manual Freeze Dryer ALPHA 1-2 LDplus
Preface
Dear customer
Congratulations on purchasing a CHRIST freeze dryer.
The freeze dryer ALPHA1-2 LDPlus is equipped with a lot of user-
friendly options which make the operation easier for you.
The newly designed ALPHA1-2 LDPlus 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 unit
operation with the new LDplus control system (Lyo-Display-plus):
 Graphic LC display with a clear layout showing the most
important process data (ice condenser temperature,
process time, section time and vacuum)
 Comfortable and self-explaining menu guidance in
German, English, French, Spanish and Polish
 Conversion of product temperature and vacuum according
to the vapour pressure curve for ice
 RS-232 communications interface (PC) available as an
option
 Retrofitting of a vacuum control system using a pressure
control valve and a vacuum sensor head (both available as
accessories) possible
We can now offer you a freeze dryer combining functionality and
convention utilisation.
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, 37520 Osterode (Germany)
Phone [phone] / 5007-0, Fax [phone] / 5007-12
Internet: www.martinchrist.de, e-mail: [email protected]

Operating Manual Freeze Dryer ALPHA 1-2 LDplus Contents •iii
Contents
1. General Information 1
1.1. Introduction ......................................................................................................1
1.2. Applications......................................................................................................2
1.3. Technical Specifications of Freeze Dryer ALPHA 1- 2 LDplus ..........................3
1.4. Standards and Regulations..............................................................................6
1.5. Safety Instructions ...........................................................................................6
1.5.1. CAUTION! Disconnect 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. ADVICE! Transport Instructions! ........................................................7
1.6. Prohibited Freeze Drying Processes...............................................................8
2. General Information on Freeze Drying 9
2.1. General Information on Freeze Drying ............................................................9
2.2. Preparation.....................................................................................................12
2.3. Freezing.........................................................................................................12
2.4. Main Drying....................................................................................................13
2.5. Final Drying....................................................................................................17
2.6. End of Drying and Aeration............................................................................17
2.7. Defrosting.......................................................................................................18
3. Description of the Freeze Drying Processes 19
3.1. Separate Freezing and Drying Outside the Ice Condenser Chamber
(Process B) on Shelves .................................................................................19
3.2. Separate Freezing and Drying Outside the Ice Condenser Chamber
(Process B) with Sealing Device....................................................................20
3.3. Separate Freezing and Drying of Liquids in Flasks (Process B)...................21
3.4. Separate Freezing and Drying of Liquids in Ampoules (Process B)..............22
4. Installation and Commissioning of the Unit 25
4.1. Site of Installation...........................................................................................25
4.2. Mains Electricity.............................................................................................26
4.3. Fuses on Site.................................................................................................26
4.4. Checking the Earth Connection.....................................................................26
4.5. Aeration..........................................................................................................26
4.6. Condensate and Defrosting Water ................................................................26
4.7. Vacuum Pump Exhaust .................................................................................27
4.8. Initial Start-up.................................................................................................27
4.8.1. Functional Components and Control Elements................................28
4.8.2. Connection of vacuum sensor vacuum Pump, and pressure
control valve......................................................................................29
4.8.3. Switching-on.....................................................................................34
5. LDplus Control System 37
5.1. Introduction ....................................................................................................37
5.2. LDplus control panel......................................................................................37

iv •Contents Operating Manual Freeze Dryer ALPHA 1-2 LDplus
5.3. Brief Guide - Handling....................................................................................38
5.4. Visual components of the LDplus control system..........................................39
5.4.1. Main window.....................................................................................39
5.4.2. Status bar .........................................................................................39
5.4.3. Softkey function................................................................................40
5.5. Values window...............................................................................................41
5.6. Mode..............................................................................................................42
5.6.1. Starting a drying process..................................................................42
5.6.2. Changing the phase .........................................................................42
5.6.3. Timer.................................................................................................42
5.7. Main menu .....................................................................................................43
5.7.1. Change set values............................................................................43
5.7.2. Special functions ..............................................................................44
5.7.3. Process and equipment information system ....................................45
5.7.4. Options .............................................................................................45
5.7.5. Tutorial..............................................................................................46
5.8. Process and equipment information system..................................................47
5.8.1. Information status.............................................................................47
5.9. LDplus special functions................................................................................48
5.9.1. Defrost ice condenser (option) .........................................................48
5.9.2. Electrical lifting device (option).........................................................48
6. Error Correction 49
6.1. Power Failure.................................................................................................49
6.2. Insufficient Vacuum........................................................................................49
6.3. Unit does not function....................................................................................51
6.4. Insufficient Ice Condenser Temperature........................................................51
6.5. Process and Equipment Information System.................................................52
6.5.1. Error Messages ................................................................................52
7. Maintenance 55
7.1. Ice Condenser Chamber................................................................................55
7.2. Heat Exchanger .............................................................................................55
7.3. Adjustment and Maintenance of the Vacuum Sensor VSP62.......................55
7.3.1. Maintenance of the Vacuum Sensor:...............................................55
7.3.2. Replacement and adjustment...........................................................56
7.4. Rubber Valves ...............................................................................................57
7.5. Vacuum Pump ...............................................................................................57
7.6. Exhaust Filter.................................................................................................57
7.7. Cleaning.........................................................................................................58
7.7.1. Cleaning of the Freeze Dryer ...........................................................58
7.7.2. Cleaning of Accessories...................................................................58
7.7.3. Maintenance of the Aeration Valve and the Drain Valve..................58
7.7.4. Disinfection of Drying Chamber, Lid and Accessories .....................59
7.7.5. Checks by Operator..........................................................................59
8. Options 61
8.1. Process Control System LPC-32, Software...................................................61
8.2. Process Control System LPC-32, Software with PC hardware.....................61
8.3. LyoLog LL-1 (Documentation Software)........................................................61
8.4. LDplus Simulation Tool (Training Software)..................................................61
9. Enclosures 63
10. Special functions 79

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •1
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 vapour. This
happens under vacuum and the temperature in the product is
normally less than -10°C.
The aim of freeze drying is to obtain an easily water soluble
product which will have the same characteristics as the original
product after addition of water.
As the drying process takes place in frozen state at very low
temperatures it is possible to dry e. g. 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 most gentle 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.

2 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus
1.2. Applications
The freeze dryer ALPHA 1-2 LDplus is a high-performance
universal laboratory and pre-production unit for freeze drying of
solid or liquid products in ampoules, vials, glass flasks, plasma
bottles or dishes. All operations necessary for freeze drying can be
realized in one and the same unit:
• Freezing of the products (uncontrolled shelf surface
temperature)1
• 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 limit values and high final vacuum for the
removal of capillarily or molecularly bound water.
The freeze dryer ALPHA 1-2 LDplus is suitable for drying of e. g.
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.
1Normally done separately in a deep-freeze

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •3
1.3. Technical Specifications of Freeze Dryer
ALPHA 1- 2 LDplus
ALPHA 1-2 LDplus
Performance data
Ice condenser capacity max. 2.5kg
Ice condenser
performance1) max. 2kg/24h
Ice condenser
temperature1) approx. –55°C
Shelf or product
temperature during freezing
in the ice condenser
chamber
approx. –25°C
Ice condenser chamber
volume: approx. 3,5l
Max. shelf surface area
when drying outside the ice
condenser chamber
(process B):
3 shelves, Ø200
Atotal 0.092m2
spacing: up to 80mm
with accessory
no. 120893
Max. shelf surface area
when drying in glass vials
with sealing under vacuum
or nitrogen atmosphere
outside the ice condenser
chamber (process B):
2 shelves, Ø200
Atotal 0.054m2
spacing: 25-70mm
with accessory
no. 121015
Drying in round bottom
flasks. Please note that the
max. ice condenser
capacity is 2kg
(process B):
8 pieces, with
accessory no.
121450

4 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus
Physical data (without
vacuum pump):
Dimensions of the unit: width: 315mm
height: 345mm
depth: 460mm
(incl. vacuum flange
connection)
Weight: approx. 28kg
Noise emissions according
to DIN 45635: 49 dB(A)
Electromagnetic
compatibility according to
EN 55011:
class B
Filling quantities:
Refrigerant: see label on the back
of the unit
Connection requirements
with vacuum pump
0.4KVA:
Electrical connection: 230V / 50Hz (others
upon request)
Power consumption: 1,2kVA
Max. current: 5A
Fuse protection: 6,3A
Ambient temperature: +10°C to +25°C
(higher temperatures
upon request)

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •5
Equipment connections:
Vacuum connection: Small flange
connection
DN 25 KF
(ISO 28403,
DIN 2861)
Drain valve and
Aeration valve:: Hose nozzle DN10 (outside diameter
12mm)
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 litre vacuum pump oil (only in case a pump is
delivered)
• 0.5 m drain hose (silicone 9 x 12 mm)
• 1 operating manual and further detailed technical
documentation
The scope of delivery does not include:
Commissioning of the unit (inside Germany) can be
performed upon request and will be invoiced at cost.
Installation of the exhaust pipe of the vacuum pump (not
necessary when using an exhaust filter).

6 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus
1.4. Standards and Regulations
Please refer to the enclosed EU Declaration of Conformity.
1.5. Safety Instructions
1.5.1. CAUTION! Disconnect Mains Plug!
As current-carrying parts are accessible inside the unit
the mains plug must be disconnected before the side panels 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 e.g. a cooling trap for protection of the
vacuum pump (if necessary check with our service department).
Besides, the unit may be damaged by corrosion.
Special caution is necessary when using azides because a
dangerous explosive develops in combination with copper or non-
ferrous metals! It is absolutely essential to consult our service
department!
1.5.3. ADVICE! Cleaning and Maintenance of the Unit!
For infectious, toxic, pathogenic and radioactive
substances the corresponding 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 take care that limbs do not come into contact with
the condenser in the ice condenser chamber as the limbs may

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •7
become frozen to the surface. The limb can only be detached from
the surface by applying heat. Liquid should not be used.
1.5.5. ADVICE! 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 putting down the unit do not hold
the plastic control panel. Please note: When putting the unit down
on a surface there is a danger of squeezing hands or fingers.
WRONG CORRECT

8 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus
1.6. Prohibited Freeze Drying Processes
1. Operation of freeze dryer when not installed correctly.
2. Operation of freeze dryer without panels.
3. Operation of freeze dryer by non-authorised personnel.
4. Operation of freeze dryer with shelves not installed
properly.
5. Operation of freeze dryer with very corrosive
substances (e.g. hydrogen chloride). 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 must not degrade
the mechanical strength of the ice condenser chamber,
the drying chamber, the lid or the accessory
components.
6. Operation of 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 not to use poor quality goods.
Breaking glass or bursting vessels can cause
dangerous situations during freeze drying.
7. Operation of freeze dryer in locations with danger of
explosion.
8. During operation the freeze dryer must not be knocked
or moved. Leaning against or resting on the freeze
dryer is not allowed.
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 inflammable
substances.
12. Infectious, toxic, pathogenic and radioactive
substances must only be dried in suitable vessels.

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information on Freeze Drying •9
2. General Information on Freeze
Drying
2.1. General Information on Freeze Drying
Freeze drying is the most gentle 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
placed in the vacuum drying chamber for drying. The ice
condenser can also be described as a vapour 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 vapour. 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 heatable. Once the “free
water” has been removed from the product, it is also possible to
remove the marginally contained adsorptively bound water by
means of very low 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) heatable2and 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 filter bottles, etc.
• Pumps to evacuate air and water vapour
a) vacuum pump to evacuate the drying chamber
(= gas pump)
b) ice condenser with temperatures from -50°C to
-105°C (depending on type of unit) to remove the
2Heatable (controlled) shelves are only possible with an LSC control system.

10 •General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus
water vapour from the chamber
(= vapour pump)
Sublimation
The principle of sublimation is briefly explained using the phase
diagram of water (freeze drying of mainly aqueous solutions, see
vapour 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, vapour 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. 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 (vapour pressure curve above ice).

Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information on Freeze Drying •11
Conversion table "Vapor pressure above ice" (sublimation
curve)
Pressure units: 1mbar = 100Pa
1Pa = 0.01mbar
Temperature units: 273
+
=
tT
273
−
=
Tt
328.1
+
⋅
=
ttF
8.1 32
−
=F
t
t
T = thermodynamic temperatureK (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

12 •General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus
2.2. Preparation
In case the unit is equipped with a pressure control valve the
vacuum pump should be warmed up. The operation
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 freeze dryer. 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.