Christ ALPHA 1-2 LDplus Operating Manual
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Christ ALPHA 1-2 LDplus Operating Manual

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

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  • Page 1 Operating Manual Freeze Dryer ALPHA 1-2 LDplus Part. No. 101521 Version 11.2006 – English Revision 1.2...
  • Page 3 → [Contacts] → [Service request] www.martinchrist.de Martin Christ Gefriertrocknungsanlagen GmbH An der Unteren Söse 50, 37520 Osterode (Germany) Phone +49 (0) 5522 / 5007-8425, Fax +49 (0) 5522 / 5007-9425 eMail: service@martinchrist.de Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 5 The newly designed ALPHA1-2 LD is a universally usable Plus 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.

  • Page 7: Table Of Contents

    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 LDplus Control System 5.1. Introduction ....................37 5.2. LDplus control panel ..................37 Contents • iii Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 8 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 iv • Contents Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 9: 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 10: Applications

    Normally done separately in a deep-freeze 2 • General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 11: Technical Specifications Of Freeze Dryer Alpha 1- 2 Ld

    121015 chamber (process B): Drying in round bottom 8 pieces, with flasks. Please note that the accessory no. max. ice condenser 121450 capacity is 2kg (process B): General Information • 3 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 12 0.4KVA: Electrical connection: 230V / 50Hz (others upon request) Power consumption: 1,2kVA Max. current: Fuse protection: 6,3A +10°C to +25°C Ambient temperature: (higher temperatures upon request) 4 • General Information Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 13 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 14: Standards And Regulations

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

  • Page 15: 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 16: 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 17: General Information On Freeze Drying

    -50°C to -105°C (depending on type of unit) to remove the 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 18 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 19 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 20: 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 21: Main Drying

    In this case it is necessary to freeze the product at temperatures as low as possible, e.g. in liquid nitrogen. General Information on Freeze Drying • 13 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 22 If the gas ballast valve is open the extracted condensable vapours will be emitted via the exhaust pipe together with air. For this reason the gas ballast valve must be open during the main drying phase! 14 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 23 (eutectic point). General Information on Freeze Drying • 15 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 24 The constraints caused by the former can be seen in the following diagram. 16 • General Information on Freeze Drying Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 25: Final Drying

    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 26: 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 27: Description Of The Freeze Drying Processes

    Without such a valve the vacuum pump must not be warmed up. Description of the Freeze Drying Processes • 19 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 28: Separate Freezing And Drying Outside The Ice Condenser Chamber (Process B) With Sealing Device

    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. 20 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 29: Separate Freezing And Drying Of Liquids In Flasks (Process B)

    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. Description of the Freeze Drying Processes • 21 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 30: Separate Freezing And Drying Of Liquids In Ampoules (Process B)

    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. 22 • Description of the Freeze Drying Processes Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 31 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 33: 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 34: Mains Electricity

    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 three-conductor connection cable and a shockproof plug. 4.3. Fuses on Site The freeze dryer must be protected typically with a 16 AG fuse.

  • Page 35: 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 36: Functional Components And Control Elements

    Vacuum pump Heat exchanger of the refrigeration unit Potential equalising screw for Mains connection and protective ground wire check and mains fuse protection central earth connection 28 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 37: Connection Of Vacuum Sensor Vacuum Pump, And Pressure Control Valve

    3 Ice condenser 11 Pressure control valve 4 Glass lid 12 Aeration valve 5 Drying chamber 13 Rubber valve 6 Heatable shelf 14 Thermal insulation Installation and Commissioning of the Unit • 29 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 38 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. 30 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 39 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 40 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 41 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 42 (1) or that it can be aerated (2). As a result, it is possible to exchange vessels during the freeze-drying process. 34 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 43: 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. Installation and Commissioning of the Unit • 35 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 45: Ldplus Control System

    LDplus ( L yo D isplay P lus) stands for a convenient user interface for controlling freeze drying processes. 5.2. LDplus control panel Illuminated LC display (240x64 pixels) Left softkey Right softkey “Up” key “Down” key LDplus Control System • 37 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 46: 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. 38 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 47: Visual Components Of The Ldplus Control System

    • The freeze dryer is in the run mode. The timer is deactivated. • The freeze dryer is in the run mode. The timer is activated. LDplus Control System • 39 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 48: Softkey Function

    In the screenshot, the left-hand softkey has the function Mode and the right-hand softkey has the function Menu 40 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 49: 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 • 41 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 50: Mode

    If the last phase is active, the system inquires as to whether the process should be continued or stopped (standby). 42 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 51: Main Menu

    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. LDplus Control System • 43 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 52: Special Functions

    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”. 44 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 53: Process And Equipment Information System

    The system automatically continues with the next phase when the preselected time is over (timer active). This applies only to a phase change from: • Freezing Warm-up vacuum pump • Main drying Final drying LDplus Control System • 45 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 54: Tutorial

    The extended service menu is reserved for service engineers only. This area is password-protected and not available to the user. 5.7.5. Tutorial Starts the tutorial of the LDplus control system (only available in German, English or French). 46 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 55: Process And Equipment Information System

    The signal continues until all pieces of information are acknowledged. In order to quit the process & equipment information window, you have to acknowledge all pieces of information so that the softkey can be displayed. Back LDplus Control System • 47 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 56: Ldplus Special Functions

    In order to move the drying chamber, the unit must be in the standby mode and completely aerated. Use the “up” and “down” keys to move the drying chamber. 48 • LDplus Control System Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 57: Error Correction

    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. Error Correction • 49 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 58 The vacuum pump does not switch on: The vacuum pump is equipped with a protective switch for the drive motor. (Please refer to separate operating manual). 50 • Error Correction Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 59: 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 60: Process And Equipment Information System

    +65°C. Temperature sensor “ice condenser” defective This error occurs in case the temperature sensor is not connected properly 52 • Error Correction Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 61 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 63: Maintenance

    At the end of the drying process vent the freeze drying unit and remove the dry product. Then defrost the unit with open drain Maintenance • 55 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 64: Replacement And Adjustment

    Alternatively, the sensor can also be adjusted to a reference value (see below). We recommend a warm-up phase of at least 5 minutes before the adjustment. Buttons with protective caps for adjusting the sensor 56 • Maintenance Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 65: Rubber Valves

    The condensate is drained using a waste oil drain screw at the filter. (Please refer to separate operating manual!) Maintenance • 57 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 66: Cleaning

    Special attention must be paid to the aeration valve and the drain valve. If residues from previous drying processes deposit on them, there is the risk of faulty operation of the freeze dryer. Therefore, 58 • Maintenance Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 67: Disinfection Of Drying Chamber, Lid And Accessories

    • 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. Maintenance • 59 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 69: 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 71: 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 73 Enclosures • 65 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 74 66 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 75 Enclosures • 67 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 76 68 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 77 Enclosures • 69 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 78 70 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 79 Enclosures • 71 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 80 72 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 81 Enclosures • 73 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 82 74 • Enclosures Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 83 Enclosures • 75 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 85 Enclosures • 77 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...

  • Page 87: Special Functions

    10. Special functions Special functions • 79 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 89 • 81 Operating Manual Freeze Dryer ALPHA 1-2 LDplus...
  • Page 91 Alpha 1-2 Stü ckliste Equipment list Erlä uterung zu folgenden Zeichnungen Legends refering to the following drawings Revision: - Stand : 11.08.05 Zeichnung – Nr. Drawing – No. Kältesystem Cooling system 170089...
  • Page 92 Stü ckliste – ALPHA 1-2 Inhalt Anlage – allgemein ................... Unit general.....................3 Belü ftungssystem / Ablaufsystem ..............Aeration system / Drain system ..............4 Kältesystem 1 ....................Cooling system 1.....................5 Meßsysteme...................... Measurement system..................6 Vakuumsystem ....................Vacuum system ....................7 Page 2...

  • Page 93: A Anlage - Allgemein

    Hersteller / Typ Component Stock-No. Manufacturer / Type A-01 Trocknungskammer CHRIST Drying chamber Edelstahlrohr ∅ 12 A-05 Eiskondensator Ice condenser A-61 Ablauf Schlauchstutzen DN6 Drain A-75 Anschluß Belü ftung Luft Schlauchstutzen DN6 Connection aeration A-201 Anlagensteuerung Christ LD Controller Page 3...

  • Page 94: B Belüftungssystem / Ablaufsystem

    Stü ckliste – ALPHA 1-2 Belüftungssystem / Ablaufsystem Aeration system / Drain system Pos.-Nr. E-Nr. Komponente Lager-Nr. Hersteller / Typ Component Stock-No. Manufacturer / Type B-100 Handabsperrventil Belü ftung Christ Hand shut-off valve aeration B-106 Handabsperrventil Ablauf Christ Hand shut-off valve drain Page 4...

  • Page 95: K1 Kältesystem

    Stü ckliste – ALPHA 1-2 Kä ltesystem 1 Cooling system 1 Pos.-Nr. E-Nr. Komponente Lager-Nr. Hersteller / Typ Component Stock-No. Manufacturer / Type K1-02 Verdichter 1 572310 Danfoss SC12CLX Compressor 1 K1-10 Kondensator 572310 Danfoss Condenser Lü fter – Kondensator K1-13 Glems Fan –...

  • Page 96: M Meßsysteme

    Stü ckliste – ALPHA 1-2 Meßsysteme Measurement system Pos.-Nr. E-Nr. Komponente Lager-Nr. Hersteller / Typ Component Stock-No. Manufacturer / Type M-20 Fü hler Eiskondensator 1 239752 PT 100 Sensor ice condenser M-40 Produktfü hler 1 124802 PT 100 Product sensor 1 M-80 Vakuummeßsonde 312010...

  • Page 97: Vakuumsystem

    Stü ckliste – ALPHA 1-2 Vakuumsystem Vacuum system Pos.-Nr. E-Nr. Komponente Lager-Nr. Hersteller / Typ Component Stock-No. Manufacturer / Type V-10 Vakuumpumpe 1 610020 VacuuBrand RZ2,5 Vacuum pump V-11 Gasballastventil 1 610020 VacuuBrand Gas ballast valve Ö lablaß Vakuumpumpe 1 V-12 738000 3/8 KFE-Hahn...
  • Page 103 111A2 114A1 113A1 111A1 Keypad Di sp l ay PC-Boar d I /O PC-Boar d CO M Modu l e RS 232 . 0 RS 232 . 1 112X2 112X1 114X18 113X3 113X6 112X5 112X7 112X9 112X2 112X1 112X4 112X3 112X6 112X5 112X7...
  • Page 104 Component repor t Component name T yp Description Page Path...
  • Page 107 CERTIFICATE The Certification Body of TÜV SÜD Management Service GmbH certifies that Martin Christ Gefriertrocknungsanlagen GmbH An der Unteren Söse 50 D-37520 Osterode has established and applies a Quality Management System for Development, Production and Sales of Freeze Dryers and Rotational-Vacuum-Concentrators An audit was performed, Report No.

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