Fisher ALPHA 1-2 LDplus User manual

edition 12.2005-english
Operating Manual
Freeze Dryer
ALPHA 1-2 LDplus
Best.-Nr. 101521

OPERATING MANUAL
ALPHA 1- 2 LDplus
Order Number:
Serial Number:
In case of inquiries please state the above numbers.
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)
¾Comfortable and self-explaining menu guidance in German,
English and French
¾Conversion of product temperature and vacuum according to
the vapour pressure curve for ice
¾RS-232 communications interface (PC) available as an option
¾Retrofitting 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.
Operating Manual Freeze Dryer ALPHA 1-2 LDplus

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
Operating Manual Freeze Dryer ALPHA 1-2 LDplus Contents •iii

4.8.2. Connection of Vacuum Pump and Installation of Accessory
Components...................................................................................................29
4.8.3. Switching-on.....................................................................................34
5. LDplus Control System 35
5.1. Introduction........................................................................................35
5.2. LDplus Control Panel.........................................................................35
5.3. Brief Guide - Handling........................................................................36
5.4. Visual Components of the LDplus Control System............................37
5.4.1. Main window.....................................................................................37
5.4.2. Status bar .........................................................................................37
5.4.3. Softkey function................................................................................38
5.5. Values Window..................................................................................39
5.6. Mode..................................................................................................40
5.6.1. Starting a drying process..................................................................40
5.6.2. Changing the phase .........................................................................40
5.6.3. Timer.................................................................................................41
5.7. Main Menu.........................................................................................41
5.7.1. Change set values............................................................................41
5.7.2. Special functions ..............................................................................43
5.7.3. Process and Equipment Information System...................................43
5.7.4. Options .............................................................................................43
5.7.5. Tutorial..............................................................................................45
5.8. Process and Equipment Information System.....................................45
5.8.1. Information status.............................................................................46
5.9. LDplus Special Functions ..................................................................46
5.9.1. Defrost ice condenser (option) .........................................................46
5.9.2. Electrical lifting device (option).........................................................47
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............56
7.3.1. Maintenance of the Vacuum Sensor:...............................................56
7.3.2. Replacement and adjustment...........................................................56
7.4. Rubber Valves ...................................................................................57
7.5. Vacuum Pump ...................................................................................58
7.6. Exhaust Filter.....................................................................................58
7.7. Cleaning.............................................................................................58
7.7.1. Cleaning of the Freeze Dryer ...........................................................58
7.7.2. Cleaning of Accessories...................................................................59
7.7.3. Maintenance of the Aeration Valve and the Drain Valve..................59
7.7.4. Disinfection of Drying Chamber, Lid and Accessories .....................59
iv •Contents Operating Manual Freeze Dryer ALPHA 1-2 LDplus

7.7.5. Checks by Operator..........................................................................60
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 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 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.
Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •1

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
2 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus

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
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
Physical data (without
vacuum pump):
Dimensions of the unit: width: 315mm
height: 345mm
depth: 460mm
(incl. vacuum flange
connection)
Weight: approx. 28kg
Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •3

ALPHA 1-2 LDplus
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 / 50-60Hz
(others upon
request)
Power consumption: 1,2kVA
Max. current: 5A
Fuse protection: 6A
Ambient temperature: Climate category:
SN
+10°C to +32°C
(higher
temperatures upon
request)
Equipment connections:
Vacuum connection: Small flange
connection
DN 25 KF
(ISO 28403,
DIN 2861)
4 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus

ALPHA 1-2 LDplus
Drain valve: Hose nozzle DN10
(outside diameter
12mm)
Aeration valve: Hose nozzle DN4
(outside diameter
8mm)
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).
Operating Manual Freeze Dryer ALPHA 1-2 LDplus 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 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
6 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus

the ice condenser chamber as the limbs may 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
Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information •7

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. 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.
8 •General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus

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)
2Heatable (controlled) shelves are only possible with an LSC control system.
Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information on Freeze Drying •9

b) ice condenser with temperatures from -50°C to
-105°C (depending on type of unit) to remove the
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).
10 •General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus

Conversion table "Vapour pressure above ice"
(sublimation curve) 1 mbar = 102 Pa = 1hPa
°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 1-2 LDplus 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 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.
12 •General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus

Freezing inside the unit is not necessary if the product is pre-frozen or
stored in e. g. a deep-freeze. In this case, especially when freeze
drying small quantities, it is advisable to pre-cool the shelves in order
to avoid partial thawing during the evacuation.
Possible water residue must be removed from the ice condenser
chamber. The drain valve is 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.
Warning:
Acidic products or products with a high solvent concentration cannot
be dried without special safety measures and devices e.g. an
additional LN2cooling 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).
Operating Manual Freeze Dryer ALPHA 1-2 LDplus General Information on Freeze Drying •13