Operating Manual Freeze Dryer ALPHA 1-2 LDplus Best.-Nr. 101521 edition 12.
OPERATING MANUAL ALPHA 1- 2 LDplus Order Number: Serial Number: In case of inquiries please state the above numbers.
Preface Dear customer Congratulations on purchasing a CHRIST freeze dryer. The freeze dryer ALPHA1-2 LDPlus is equipped with a lot of userfriendly 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.
Contents 1. General Information 1.1. 1.2. 1.3. 1.4. 1.5. Introduction ..........................................................................................1 Applications..........................................................................................2 Technical Specifications of Freeze Dryer ALPHA 1-2 LDplus................3 Standards and Regulations..................................................................6 Safety Instructions ........................................................
4.8.2. Connection of Vacuum Pump and Installation of Accessory Components...................................................................................................29 4.8.3. Switching-on .....................................................................................34 5. LDplus Control System 5.1. 5.2. 5.3. 5.4. Introduction ........................................................................................35 LDplus Control Panel ........................................................
7.7.5. 8. Checks by Operator..........................................................................60 Options 8.1. 8.2. 8.3. 8.4. 61 Process Control System LPC-32, Software .......................................61 Process Control System LPC-32, Software with PC hardware..........61 LyoLog LL-1 (Documentation Software) ............................................61 LDplus Simulation Tool (Training Software) ......................................61 9. Enclosures 63 10.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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 vapour 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.
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 vapour 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 drying time depends heavily on the drying vacuum. The nearer the vacuum is to the solidification point in accordance with the vapour pressure curve above ice, the shorter the drying time is. Interesting correlations : 1.0 gram of ice at 1.0 mbar assumes a volume of 1 m³ vapour 0.1 mbar assumes a volume of 10 m³ vapour 0.
2.5. Final Drying The final pressure in the drying chamber depends on the ice condenser temperature according to the vapour 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.
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 are drained through the drain valve at the left side of the unit. To do this, a hose is put onto the nozzle.
3. Description of the Freeze Drying Processes 3.1. Separate Freezing and Drying Outside the Ice Condenser Chamber (Process B) on Shelves It is also possible to dry the product outside the ice condenser chamber. In this case, the product has to be frozen 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.
manual stop valve. Without such a valve the vacuum pump must not be warmed up. The rack is set onto the base plate. With small samples it is recommended to pre-cool the shelves. In this way, a partial thawing during the evacuation process is avoided. When freezing and drying is performed separately outside the ice condenser chamber it is directly started with the main drying process.
Then the pressure plate is fastened with the threaded pin in such a way that it will rest on or slightly above the rubber stopper. When using two or more shelves every shelf is set directly on or with a slight distance to the rubber stoppers as it is the case for the pressure plate. Instead of the stopper the vacuum-tight rotary leadthrough is put into the standard ground socket of the drying chamber. Before inserting, the ground-in surface of the leadthrough is greased with vacuum grease.
To start the drying process, the main drying process has to be activated in the control system. The pressure control valve opens and the main drying process starts. Caution: The frozen samples can only be connected to the valves when a pressure of less than 1.030 mbar is reached. Liquids are frozen in flasks according to the shell freezing principle, manually or with a turning device. Thanks to this freezing process the layer thickness is reduced and the drying period is considerably shortened.
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 a partial thawing during the evacuation process is avoided. One ampoule after the other is connected using this method. Sealing of the ampoule is carried out 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.
4. Installation and Commissioning of the Unit 4.1. Site of Installation WARNING! Papers, cloths or similar items must not be put behind the unit as the air circulation of the heat exchanger will not work any more. The freeze dryer should be horizontally aligned. The ambient temperature should be within approx. +10°C and +32°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 following connections are required at the site: 4.2. Mains Electricity The voltage given on the name plate must correspond to the local supply voltage. CHRIST freeze dryers are units of safety class I and include a threeconductor connection cable and a shockproof plug. 4.3. Fuses on Site The freeze dryer must be protected typically with a 16 AG fuse. 4.4.
4.7. Vacuum Pump Exhaust During the main drying phase the separate vacuum pump must be operated with open gas ballast valve. The oil mist which is produced must be removed. A ½" hose can be connected to the exhaust flange of the vacuum pump RZ-2 or RC-5 and a ¾" hose is 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 care must be taken that condensate cannot flow back into the pump.
4.8.1. Functional Components and Control Elements Aeration and drain valve Ice condenser chamber Ice condenser LDplus control system Mains switch Serial interface for vacuum sensor Vacuum connection Pressure control and stop valve Vacuum pump Name plate Additional connection interface (option, sep.
4.8.2. Connection of Vacuum Pump and Installation of Accessory Components 4.8.2.1 Connection diagram ALPHA 1-2 LDplus 1 2 1 ALPHA 1-2 LDplus 2 Pressure control valve and stop valve 3 Vacuum hose 4 Vacuum pump 3 4 The accessory components are connected to the ALPHA 1-2 LDplus freeze dryer according the connection diagram shown above.
Instructions for the connection with centring rings and clamping flanges Small flange connections which are not mounted properly between the aggregates or to connect hoses are often the reason for serious vacuum problems. Please loosen the connection and replace the centring ring (with sealing ring inside) centrically between the flange connections. Seal the connection with the clamping flange by fastening the wing nut. Please take care that the centring ring does not get out of place and does not tilt.
In case a pressure control valve is available it has to be mounted between the freeze drying unit and the vacuum pump. Then it has to be plugged into the socket of the freezing unit on the rear panel of the unit. Please observe the installation direction of the pressure control and stop valve The vacuum pump is connected to the unit and plugged into the socket on the rear panel of the unit. The vacuum gases shall be filtered or drained.
Diagram of the accessories The other accessories (e.g. drying chamber, shelves, and connections for round bottom flasks) will be completed according to the scope of supply. Example: Accessories for drying on 2 unheated shelves with sealing device for injection bottles (without vacuum pump). Example: Accessories for drying on 3 unheated shelves plus individually lockable rubber valves for round bottom flasks or wideneck filter bottles (without vacuum pump).
Possible accessories for the ALPHA 1-2 LDplus: Ground-in stopper Drying chamber Ø300 with 12 connections Rubber valve Distributor Drying vessel, e.g. round bottom flask 3 shelves Ø200, unheated Drying vessel, e.g. ampoule Drying vessel, e.g. injection bottle Drying chamber Ø240 Product dish Sealing device with 2 shelves Ø200, unheated Drying vessel e.g.
4.8.3. Switching-on Press the mains switch on the right side of the unit to switch the unit on. The initialization of the LDplus control system starts. This may last for several seconds. When the unit is switched on for the first time (after delivery from the factory), the user will be guided through the LDplus control system in the form of a tutorial for a quick familiarisation with the unit. and down First select your language using the up softkey.
5. LDplus Control System 5.1. Introduction LDplus (Lyo Display Plus) stands for a convenient user interface for controlling of freeze drying process. 5.2. LDplus Control Panel 1. 3. 2. 4. 1. 2. 3. 4. 5. 5.
5.3. Brief Guide - Handling The LDplus control system is operated via four centrally located keys on the touch-sensitive control panel. The following functions are assigned to the four key 36 • LDplus Control System : • Left softkey & right softkey Softkeys are keys with dynamic functions assigned to them. The current key function is displayed next to the key. Softkeys allow the control system to be operated in a particularly easy and transparent way.
5.4. Visual Components of the LDplus Control System The LC display is divided into the three following areas: 1. Main window 2. Status bar 3. Softkey function Main window Softkey function 5.4.1. Status bar Main window The main window shows set values and actual values, menus and process-relevant information. 5.4.2. Status bar The status bar shows the current operating mode, the active phase and other relevant information. The status bar is visible at all times.
5.4.2.2 5.4.2.3 Active phase • Freezing The ice condenser is cooled. • WarmUp VP The ice condenser is cooled and the vacuum pump is activated with the pressure control valve closed. If no pressure control valve is installed, the drying chamber has to be shut off from the vacuum pump using a manual valve, for example. • Main drying The drying chamber is evacuated with the ice condenser being cooled.
5.5. Values Window The values window is displayed after the initialisation of the LDplus control system. It is divided into two areas, the left-hand values window and the right-hand values window. The left-hand and right-hand value windows are structured as follows: Measuring channel Set value Unit of the measured value Actual value The up key is used to select the measuring channel to be displayed in the left-hand values window.
5.6. Mode The mode selection can be activated by pressing the left-hand softkey in the active values window. The function Mode Mode comprises the operating mode selection and the phase selection. Freeze drying comprises the following four phases: 5.6.1. • Freezing • Warm-up vacuum pump • Main drying • Final drying Starting a drying process If the unit is in standby mode, pressing the softkey Mode leads to an inquiry concerning the phase to be used for starting the freeze drying process.
5.6.3. Timer If the timer is active for the phase (timer set value >= 1 minute), the system inquires before the selected time is over as to whether the user wants to continue with the next phase. If the last phase is active, the system inquires as to whether the process should be continued or stopped (standby). To deactivate the timer, select an infinite set value ( ). As an option, it is possible to change over to the next phase automatically when the preselected time is over.
Select the set value using the focus. Press the right-hand softkey Edit to start the editing mode. The focus is displayed in an inverted manner. You can now change the set value within a permissible range using the up and down keys. Press OK to confirm the set value or Cancel The editing mode is quit. 5.7.1.1 Set values for freezing • 5.7.1.2 to reject it. Timer Time for the freezing phase section time. You can set a time between 1 minute and 200 hours.
5.7.2. Special functions The special functions menu is used to operate special accessories (defrosting device and electrical lifting device) of the freeze dryer. If one of the options is not installed in the freeze dryer, the system displays the message Option not available. A detailed description of the special functions can be found in the chapter “LDplus Special Functions”. 5.7.3.
5.7.4.2 Language The LDplus control system can be used in the German, English or French language. 5.7.4.3 Settings The Settings menu is used to customise the operation and process management of the control system. Warm-up vacuum pump Warm-up time required by the vacuum pump. In case of doubt, please refer to the operating manual of the vacuum pump. You can set a warm-up time between 5 and 60 minutes.
5.7.5. Tutorial Starts the tutorial of the LDplus control system. 5.8. Process and Equipment Information System A detailed list of error messages can be found in the chapter "Error Correction". The process & equipment information window is displayed whenever the LDplus control system generates a new information message. In addition, the user can select Menu -> Process & Equipment Information System in the main menu to check whether messages are pending.
5.8.1. Information status Every information shown in the process & equipment information window receives a certain status. • Information present, not acknowledged • Information present, acknowledged • Information no longer present, not acknowledged Once an information is no longer present but has been acknowledged, the information will be removed from the process & equipment information window. The signal continues until all pieces of information are acknowledged.
5.9.2. Electrical lifting device (option) To move the drying chamber with the help of the electrical lifting device, open the menu Menu -> Special functions -> Electrical lifting device. In order to move the drying chamber, the unit must be in standby mode and completely aerated. Use the up Operating Manual Freeze Dryer ALPHA 1-2 LDplus and down keys to move the drying chamber.
6. Error Correction 6.1. Power Failure The control system continues the process after a power failure. The preselected conditions remain saved during the process run. The process times, the total time and the section time are reset. In the event of a power failure during the drying process the batch may become unusable. Whether the batch can be saved depends on the drying phase in which the product was when the power failure occurred.
To eliminate this fault we recommend that the unit is evacuated and vented by means of the drain valve so that any residue (e.g. collected parts) is removed. If necessary, the O-rings must be replaced. If the leakage cannot be eliminated in this way, the drain valve must be cleaned or replaced. Check the sealing of the lid for dirt or damages. If necessary, the sealing must be cleaned or replaced.
6.3. Unit does not function If the display does not work after operating the mains switch, the following must be checked: Is the mains switch plugged in? • Check the on site fuses. • Check the automatic circuit breaker 1F1 on the back of the unit. 6.4. Insufficient Ice Condenser Temperature The refrigerator is equipped with a protection device against overpressure in the refrigerating system and with a thermal motor protection.
6.5. Process and Equipment Information System 6.5.1. Error Messages Vacuum of 6.11 mbar has not been reached This error occurs in case 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 pressure control valve is closed and the vacuum pump is switched off.
than +65°C. Temperature sensor “ice condenser” defective This error occurs in case the temperature sensor is not connected properly or in case it is defective. Please contact our service department. Temperature sensor “defrosting heater” defective This error occurs in case the temperature sensor is not connected properly or in case it is defective. Please contact our service department.
7. Maintenance 7.1. Ice Condenser Chamber Before each start-up ensure that all water residue has been removed from the ice condenser chamber. If necessary, wipe the ice condenser chamber. Before every drying process it is recommended to open and close the drain valve once. 7.2. Heat Exchanger A laminated heat exchanger is used to cool the refrigerant compressed by the refrigerator. The heat exchanger is placed at the back of the unit.
7.3. Adjustment and Maintenance of the Vacuum Sensor VSP62 7.3.1. Maintenance of the Vacuum Sensor: The tungsten wire has a limited service life because it easily reacts with ambient gases. Tungsten reacts especially with carbons to build tungsten carbide. The wire becomes short and breaks. Therefore, the only possibility to enlarge the service life of PIRANI sensors is to a v o i d every contact to carbonic substances.
(see below). We recommend a warm-up phase of at least 5 minutes before the adjustment. Buttons with protective caps for adjusting the sensor 7.3.2.2 Adjustment to a specific zero reference value To perform this adjustment, the actual pressure must be lower than 1.0x10-2 mbar. After pressing of the button labelled “set”, the actual vacuum field of the LDplus control system shows a value corresponding to the zero adjustment value currently set (factory setting 0.0010 mbar).
7.5. Vacuum Pump For maintenance of the vacuum pump please refer to the separate operating manual. Additionally, we would like to emphasise the following points: The oil level of the vacuum pump must be regularly checked using the inspection 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.
7.7.2. Cleaning of Accessories When looking after accessories special safety measures must be considered as these are measures to ensure operational safety and reliability. Chemical reactions as well as stress corrosion cracking (combination of changing pressure and chemical reaction) can affect or destroy the structure of the metals and plastic parts. Hardly detectable cracks on the surface expand and weaken the material without visible signs.
Please consult us if in doubt. If dangerous materials are used, the freeze dryer and the accessories must be disinfected. 7.7.5. Checks by Operator The operator has to ensure that the important parts of the freeze dryer relevant 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 tear of material etc. Furthermore, an earth conductor check must be carried out regularly.
8. Options 8.1. Process Control System LPC-32, Software Upon request. See separate operating manual. 8.2. Process Control System LPC-32, Software with PC hardware Upon request. See separate operating manual. 8.3. LyoLog LL-1 (Documentation Software) Upon request. See separate operating manual. 8.4. LDplus Simulation Tool (Training Software) Upon request.
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