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