Fisher ALPHA 1-2 LDplus Operating Manual

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

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Summary of Contents for Fisher ALPHA 1-2 LDplus

  • Page 1 Operating Manual Freeze Dryer ALPHA 1-2 LDplus Best.-Nr. 101521 edition 12.2005-english...
  • Page 2 OPERATING MANUAL ALPHA 1- 2 LD plus Order Number: Serial Number: In case of inquiries please state the above numbers. Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 3 (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...
  • Page 4: Table Of Contents

    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 Contents • iii Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 5 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...
  • Page 6 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 Enclosures Special functions Contents • v Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 8: General Information

    Lyophilisation is also the best method when drying inorganic products – e.g. nanoscale dispersions – the particle surfaces of which should remain unchanged. General Information • 1 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 9: Applications

    Normally done separately in a deep-freeze 2 • General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 10: Technical Specifications Of Freeze Dryer Alpha 1-2 Ld

    121450 is 2kg (process B): Physical data (without vacuum pump): Dimensions of the unit: width: 315mm height: 345mm depth: 460mm (incl. vacuum flange connection) Weight: approx. 28kg General Information • 3 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 11 Max. current: Fuse protection: Climate category: Ambient temperature: +10°C to +32°C (higher temperatures upon request) Equipment connections: Small flange Vacuum connection: connection DN 25 KF (ISO 28403, DIN 2861) 4 • General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 12 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). General Information • 5 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 13: Standards And Regulations

    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...
  • Page 14: Advice! Transport Instructions

    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 General Information • 7 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 15: Prohibited Freeze Drying Processes

    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...
  • Page 16: General Information On Freeze Drying

    Pumps to evacuate air and water vapour a) vacuum pump to evacuate the drying chamber (= gas pump) Heatable (controlled) shelves are only possible with an LSC control system. General Information on Freeze Drying • 9 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 17 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...
  • Page 18 0.0019 1.980 0.280 0.025 0.0017 1.810 0.250 0.024 0.0014 1.650 0.220 0.021 0.0012 1.510 0.200 0.018 0.0010 1.370 0.180 0.016 1.250 0.160 0.014 1.140 0.140 0.012 General Information on Freeze Drying • 11 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 19: Preparation

    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...
  • Page 20: Main Drying

    LN 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). General Information on Freeze Drying • 13 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 21 This small quantity of water vapour 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). 14 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 22 (eutectic point). General Information on Freeze Drying • 15 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 23 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. 16 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 24: Final Drying

    “flood” the unit with nitrogen or another inert gas instead of using air. CAUTION! Maximum overpressure 0.2 bar! Then the unit is switched off and the product is removed. General Information on Freeze Drying • 17 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 25: Defrosting

    To do this, a hose is put onto the nozzle. The condensate and the defrosting water are collected in a vessel. Pipe connection for vacuum pump (behind baffle plate) 18 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 26: Description Of The Freeze Drying Processes

    The valve is closed during warming-up of the pump. In case the unit is not equipped with an electromagnetic pressure control valve we recommend to use a Description of the Freeze Drying Processes • 19 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 27: Separate Freezing And Drying Outside The Ice Condenser Chamber (Process B) With Sealing Device

    The threaded rod is screwed into the lower shelf until its slotted head is on the same height as the rack (upper edge). 20 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 28: Separate Freezing And Drying Of Liquids In Flasks (Process B)

    The ground-in surfaces have to be cleaned and greased before every further mounting of accessories. Before the drying process can start it is necessary to check that all valves are closed. Description of the Freeze Drying Processes • 21 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 29: Separate Freezing And Drying Of Liquids In Ampoules (Process B)

    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. 22 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 30 The remaining glass from the 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. Description of the Freeze Drying Processes • 23 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 32: Installation And Commissioning Of The Unit

    This may cause an exceeding of the admissible operation pressure and thus a breakdown of the freezing unit. Installation and Commissioning of the Unit • 25 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 33: Mains Electricity

    The drain valve is also used to vent the unit when a freeze drying process has been completed. 26 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 34: Vacuum Pump Exhaust

    4.8. Initial Start-up CAUTION! Ensure that the freeze dryer is correctly mounted and installed before initial start-up (see point 4.1 Site of Installation and following points). Installation and Commissioning of the Unit • 27 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 35: Functional Components And Control Elements

    (option, sep. accessories Heat exchanger of the refrigeration unit Potential equalising screw for protective ground wire check and Mains connection and central earth connection mains fuse protection 28 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 36: Connection Of Vacuum Pump And Installation Of Accessory Components

    Centring rings and clamping flanges with wing nuts are used as connecting elements (small-flange connection according to ISO 28403 or DIN 2861, see the following instructions). Installation and Commissioning of the Unit • 29 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 37 Please take care that the centring ring does not get out of place and does not tilt. 30 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 38 In case the drying chamber is equipped with rubber valves they have to be closed. Further accessories (e.g. shelves, connections for round bottom flasks) are added accordingly. Installation and Commissioning of the Unit • 31 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 39 Example: Accessories for drying on 3 unheated shelves plus individually lockable rubber valves for round bottom flasks or wide- neck filter bottles (without vacuum pump). 32 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 40 Sealing device e.g. injection bottle with 2 shelves Ø200, unheated Drying chamber Drying vessel Ø240 e.g. injection bottle Drip tray Base plate ALPHA 1-2 LDplus Installation and Commissioning of the Unit • 33 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 41: Switching-On

    In the end, the program inquires as to whether the user wants the tutorial to be displayed again when the unit is switched on the next time. 34 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 42: Ldplus Control System

    LDplus ( L yo D isplay P lus) stands for a convenient user interface for controlling of freeze drying process. 5.2. LDplus Control Panel Illuminated LC display (240x64 pixels) Left softkey Right softkey Up key Down key LDplus Control System • 35 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 43: Brief Guide - Handling

    Inside the menu, the up key and the down key are used to shift the focus. When parameters are entered, they are used to change the value. 36 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 44: Visual Components Of The Ldplus Control System

    The freeze dryer is in standby mode. All aggregates are switched off. • The freeze dryer is in run mode. The timer is deactivated. • The freeze dryer is in run mode. The timer is activated. LDplus Control System • 37 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 45: Softkey Function

    In the screenshot, the left-hand softkey has the function Mode and the right-hand softkey the function Menu 38 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 46: Values Window

    (see the chapter "General Information on Freeze Drying"). This measuring channel can only be selected if a vacuum sensor is installed. LDplus Control System • 39 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 47: Mode

    5.6.2. Changing the phase If the unit is in run mode, you can change over to the next phase or stop the process by selecting Standby. 40 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 48: Timer

    The following section explains all menu items in detail: 5.7.1. Change set values Used to define the phases freezing, main drying and final drying. First select the phase. LDplus Control System • 41 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 49 0.0010 mbar converted into steps of 1°C according to the vapour pressure curve above ice for water. Set values for final drying are not available unless the pressure control option is installed. 42 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 50: Special Functions

    The Contrast menu is used to change the contrast of the LC display. The contrast has to be adapted to the local light conditions at the installation site of the freeze dryer. LDplus Control System • 43 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 51 Time required for defrosting the ice condenser 5.7.4.4 Service The service menu is reserved for the service engineer. This area is password-protected and not available to the user. 44 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 52: Tutorial

    & equipment information window will not be displayed until the user quits the main menu. Number of messages pending Message Information status Softkey for Softkey for acknowledging quitting the the message window LDplus Control System • 45 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 53: Information Status

    When the defrosting time is over, the defrosting process is stopped and the window is closed. You can set the time required for defrosting under Menu -> Options -> Settings -> Defrost ice condenser. 46 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 54: Electrical Lifting Device (Option)

    In order to move the drying chamber, the unit must be in standby mode and completely aerated. Use the up and down keys to move the drying chamber. LDplus Control System • 47 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 56: Error Correction

    This is caused by residue from the drying process, fluff from cleaning cloths or wear and tear of the O-rings of the valve. Error Correction • 49 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 57 The vacuum pump is equipped with a protective switch for the drive motor. (Please refer to separate operating manual). General information: The vacuum checks should be carried out when the ice condenser is deep-frozen. 50 • Error Correction Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 58: Unit Does Not Function

    -85°C is reached if the ice condenser is not loaded and the ice condenser chamber is evacuated. Sufficient air circulation is necessary. Do not deposit any objects behind the freezing unit! Error Correction • 51 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 59: Process And Equipment Information System

    The refrigerating unit is switched off in order to prevent it from being operated or started at too high temperatures. The system cannot be restarted until the ice condenser temperature is lower 52 • Error Correction Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 60 IO communication error (0x20) Error in the IO module LDplus EA Please contact our service department. Error Correction • 53 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 62: Maintenance

    Excessive dirt on the heat exchanger leads to a decrease in performance and can lead to a failure of the unit! Please note: The unit must not be turned upside down! Maintenance • 55 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 63: Adjustment And Maintenance Of The Vacuum Sensor Vsp62

    If a zero adjustment has to be performed, the actual pressure should be smaller than 5.0x10 mbar (factory setting). Alternatively, the sensor can also be adjusted to a reference value 56 • Maintenance Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 64: Rubber Valves

    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. Maintenance • 57 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 65: Vacuum Pump

    If there is the risk of toxic, radioactive or pathogenic contamination, special safety measures must be considered and adhered to. 58 • Maintenance Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 66: Cleaning Of Accessories

    “Chemical behaviour PLEXIGLAS® (acrylic glass). The freeze dryers and the accessories consist of different materials. A possible incompatibility must be considered. For autoclaving the temperature stability of the individual material must be checked. Maintenance • 59 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 67: Checks By Operator

    • 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. 60 • Maintenance Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 68: Options

    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. Options • 61 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 70: Enclosures

    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 Enclosures • 63 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 72 Enclosures • 65 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 73 66 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 74 Enclosures • 67 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 75 68 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 76 Enclosures • 69 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 77 70 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 78 Enclosures • 71 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 79 72 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 80 Enclosures • 73 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 81 74 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 82 Enclosures • 75 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 84 Enclosures • 77 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 86: Special Functions

    10. Special functions Special functions • 79 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 88 • 81 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

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