Gefriertrocknungsanlagen OPERATING MANUAL Freeze Dryer ALPHA 1-4 LD-2 (Best.-Nr. 101041 / 101141 / 101241) ALPHA 2-4 LD-2 (Best.-Nr.
Operating Manual ALPHA 1-4 LD-2 and ALPHA 2-4 LD 2 Order Number: Serial Number: In case of inquiries or repair please state the above numbers. For service please contact: MARTIN CHRIST Gefriertrocknungsanlagen GmbH An der unteren Sö se 50, D-37520 Osterode Tel.
Preface Dear customer, Congratulations on purchasing a CHRIST freeze dryer. The freeze dryer is equipped with user-friendly options which make the operation easier for you. The newly designed ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 is a universally usable CHRIST freeze dryer for laboratories, R&D departments and scientific institutes. The well proven range of accessories allows application oriented configuration of the equipment especially for routine use.
Contents: 1 2 ^ Page General Information 1.1 Introduction 7 1.2 Application 7 1.3 Technical specifications of freeze dryer ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 8 1.4 Standards and regulations 10 1.5 Safety instructions 10 1.6 Prohibited freeze drying processes 11 Installation and Commissioning of the Unit 2.1 Site of installation 13 2.2 Mains electricity 13 2.3 Fuses on site 13 2.4 Checking the Earth connection 13 2.5 Defrosting water 14 2.6 Vacuum pump exhaust 14 2.
3 4 5 6 Control System LD-2 24 3.1 Mains switch 25 3.2 "°C mbar" button 25 3.3 "≙ " Button 25 3.4 Connection of the vacuum measuring sensor TPR 265 26 General Information on Freeze Drying 27 4.1 Freezing 29 4.2 Main drying 30 4.3 Final drying 34 4.4 End of drying and venting 34 4.5 Defrosting 34 Description of the Freeze Drying Processes 5.1 Freezing separately and drying on shelves 35 5.2 Drying with sealing device 35 5.
8 6.7.1 Cleaning of the freeze dryer 40 6.7.2 Cleaning of accessories 40 6.7.3 Maintenance of the condensate drain valve 41 6.7.4 Disinfection of chamber and accessories 41 6.7.5 Operator checks 41 Instructions for Error Correction 7.1 Power failure 42 7.2 Insufficient vacuum 42 7.3 Unit does not function 43 7.
1 General Information 1.1 Introduction What is freeze drying? 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, when the temperature in the product is 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.
1.3 Technical Specifications of Freeze Dryer ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 Performance data: Ice condenser capacity: max. 4 kg max. 4 kg Ice condenser performance: max. 4 kg/24 h max. 4 kg/24 h Ice condenser temperature: Approx. -54°C approx. – 84°C Shelf temperature when freezing inside the ice condenser chamber: Approx. -25°C approx. – 50°C Max. shelf surface area when drying outside the ice condenser chamber: 5x shelf surface areas 360 Max.
Max. power consumption: 0,92 kVA 1,84 kVA Max. current: 4,0 A 8,0 A Safety precaution 6,3 AT 10 AT Max. ambient temperature climate category SN +10°C to +32°C (higher temperatures on request) Equipment connections: Vacuum connection: small flange connection DN 25 KF (ISO 28403, DIN 2861) Condensate drain: hose nozzle DN 10 with 0.
1.4 Standards and Regulations Please refer to the enclosed EU-Statement 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. For maintenance 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.
1.5.5 IMPORTANT! 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. RIGHT 1.6 WRONG Prohibited Freeze Drying Processes 1. Operation of freeze dryer when not installed correctly. 2.
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.
2 Installation and Commissioning of the Unit 2.1 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 positioned horizontally. The ambient temperature should be within approx. +15°C and +25°C. The refrigerator 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.
2.5 Defrosting Water The defrosting water is drained via the condensate drain valve on the left side of the unit. To drain the water place the hose supplied with the unit onto the nozzle. The defrosting water is collected in a vessel. The defrosting water can also be drained directly via this hose. The defrosting water must be able to drain freely. To achieve this the hose must have a steady downward slope. It must be ensured that water does not collect in any part of the hose.
2.7 Initial start-up CAUTION! Ensure that the freeze dryer is correctly mounted and installed before initial start-up (see point 2.1 Site and following points). 2.7.
Instructions on connecting centering rings and clamping flanges Vacuum hose Centering ring Clamping flange Vacuum release valve (separate accessory) A C Lay-out assembly of vacuum connections. Connect second flange (the centering ring must be positioned correctly!) and place clamping flange over the connection and press together. B Place centering ring on one side of small flange connection (e. g. vacuum hose). D Tighten the screw of the clamping flange by hand.
Other ordered accessories (e.g. drying chamber, shelves and connections for round bottom flasks) are added accordingly. Example: Accessory for drying on 5 unheated shelves as well as individually sealable rubber valves for round bottom flasks. Example: Accessory for drying on 2 unheated shelves with sealing device for injection vials.
Schematic diagram of accessories Drying chamber 300 with 12 connections Ground-in stopper Rubber valve Drying vessel, e.g. round bottom flasks Ampoule manifold Additional chamber 300 with 12 connections Drying vessel, e.g. ampoule 3 or 5 shelves 265, unheated Drying vessel, e.g. injection vial Product dish Drying chamber Stoppering device with 1 shelf, 250, unheated, max. 4 shelves can be used 300 Drying vessel, e.g.
Rubber valve Manifold, different versions, max. 24 rubber valves Drying vessel, e.g.. wide neck filter Drying chamber, e.g. round bottom flaks Drying vessel, e.g.
Drying chamber Rubber valve 457 Connection pipe for rubber valve, for enlarging the drying chamber max. 18 pieces Ampoule manifold Drying vessel, e.g. Ampoule Drying vessel, e.g. round bottom flasks Drying vessel, e.g.
2.7.
2.7.3 Preparing for Evacuation The drying chamber made from acrylic glass with ground-in stoppers is placed on the ice condenser chamber. The defrosting water valve at the left side of the unit and any rubber valves on the drying chamber are closed. The vacuum pump is connected to the unit and to the mains. 2.7.4 Evacuation The drying chamber is evacuated by switching on the vacuum pump. After switching on the pump it must not be possible to lift the acrylic chamber or lid anymore. 2.
2.9 Error resolution Error Measure Start of the instrument is not possible 1. Mains failure Mains plug connected? Check the fuse of the freeze dryer (Mains connection cord, fuse insert cord) respectively the fuse of the building and exchange if necessary No display Mains plug connected? Check the fuse of the freeze dryer (Mains connection cord, fuse insert cord) respectively the fuse of the building and exchange if necessary Refrigeration system does not work No vacuum 1.
3 Control System LD-2 A particular advantage of the user friendly LD control system (Lyo-display) is that all functions are explained on the control panel. - LC display showing the most important process data (temperature of ice condenser, vacuum) - Conversion of temperature and vacuum in accordance with the vapour pressure curve above ice - RS-232 communications interface (PC) is available as an option.
3.1 Mains Switch The unit is switched on by means of the mains switch on the upper right side of the unit. The LED-display lights up and the refrigerator is in operation. LC-Display Button "mbar" Button "≙ " Button "°C" 3.2 "° C mbar" Button On the freeze dryer ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 the vacuum in the drying chamber or alternatively the ice condenser temperature can be displayed. The changeover is carried out by pressing the "° C " or “ mbar” button.
3.4 Connection of the Vacuum Measuring Sensor TPR 265 Units without a vacuum measuring sensor can easily be retrofitted with the sensor TPR 265 for measuring the vacuum. To do this the plug of the measuring sensor is inserted into the socket on the back of the unit. The measuring sensor is supplied with a T-piece with small flange connections. With this T-piece the sensor is connected to the connection at the rear panel of the unit.
4 General Information on Freeze Drying Freeze drying is the most gentle process for drying biological and chemical 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 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.
Vapour pressure curve for ice and water 1mbar = 10²Pa 0 -1 -2 -3 -4 -5 -6 -7 -8 -9 -10 -11 -12 -13 -14 -15 -16 -17 -18 -19 = mbar 6,110 5,620 5,170 4,760 4,370 4,020 3,690 3,380 3,010 2,840 2,560 2,380 2,170 1,980 1,810 1,650 1,510 1,370 1,250 1,140 °C -20 -21 -22 -23 -24 -25 -26 -27 -28 -29 -30 -31 -32 -33 -34 -35 -36 -37 -38 -39 = mbar 1,030 0,940 0,850 0,770 0,700 0,630 0,570 0,520 0,470 0,420 0,370 0,340 0,310 0,280 0,250 0,220 0,200 0,180 0,160 0,140 °C -40 -41 -42 -43 -44 -45 -46 -47 -48 -49 -50
The process steps of freeze drying Prefreezing + Drying under atmosphere pressure (e.g. at - 25°C) under vacuum (e.g. at 0.1 mbar, equal to -42°C) = formation of the ice structure = keeps the water contents in the phase Additionally necessary: Energy input (= heat) but: the material remains in the solid/ice phase! (physical law: the vacuum is responsible for the product-/steam temperature) 4.
4.2 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 as low as possible, e.g. in liquid nitrogen. Warning: Acidic products or products with a high solvent concentration cannot be dried without special protective measures and devices e.g.
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! The gas ballast valve can only be closed for final drying. During the main drying phase the moisture is removed by sublimation, during final drying the bound moisture is removed by desorption.
This typical drying curve is due to the fact that the area of sublimation recedes into the product and the water vapour still to be extracted has to pass through the already dried layers. During the drying process the inner resistance increases. Thus the drying curve is primarily determined by the latent heat of sublimation and the water vapour transport speed.
Effects of freeze drying of a product in a dish Heat transfer takes place via the heated shelves1, via direct contact with the bottom of the vessel and/or via the gas between the shelves and vessel by means of convection. At the beginning of sublimation the transfer of heat is very effective from the wall of the vessel to the frozen product. However, soon an area develops which is ice free, porous and dried and has a corresponding temperature gradient between the wall of the vessel and the product.
4.3 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.
5 Description of the Freeze Drying Processes 5.1 Freezing Separately and Drying on Shelves Possible water residue is removed from the ice condenser chamber. The defrosting water valve is opened and closed again so that the water residue can be drained. The ice condenser chamber should be wiped If necessary. For pre-cooling the ice condenser the ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 is switched on. The rack is put onto the bottom plate.
5.3 Freezing Separately and Drying of Flasks Possible water residue is removed from the ice condenser chamber. The defrosting water valve is opened and closed again so that the water residue can be drained. The ice condenser chamber should be wiped if necessary. For pre-cooling the ice condenser the ALPHA 1-4 LD-2 / ALPHA 2-4 LD-2 is switched on. For drying outside of the ice condenser chamber different manifolds are available (see accessory catalogue).
If shock-freezing is required we recommend that freezing is carried out in liquid nitrogen or in a cooling bath. 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. With this procedure one ampoule after the other is connected. Sealing of the ampoule is carried out in the same way.
6 Maintenance 6.1 Vacuum Pump For maintenance of the vacuum pump please refer to the enclosed instructions. 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 instructions for the pump.
6.5 Condenser of Cooling Liquid A laminated condenser for cooling liquid is used to cool the refrigerant compressed by the refrigerator. The condenser for cooling liquid is placed at the bottom of the unit. In intervals of a few months it must be checked for dust or dirt residues and cleaned if necessary. Cleaning of the heat exchanger can be carried out best by brushing, by using a vacuum cleaner from the outside or by using compressed air from inside the unit.
"HV" Adjustment: The high-vacuum adjustment must be carried out with a two-stage slide vane rotary vacuum pump in good working order: − Mount the TPR 265 on the vacuum pump and evacuate for approx. 10 minutes. − Set the transition point in the vacuum display of ALPHA 1-4 LD-2 / ALPHA 2-4 LD2 between 0.0026 mbar and 0.0030 mbar using the potentiometer "HV" of the TPR 265. Vent the unit slowly and carry out the adjustment process once again.
Cleaning of accessories should be carried out away from the freeze dryer once a week or preferably after every use. If there is the risk of toxic, radioactive or pathogenic contamination, special safety measures must be considered and adhered to. Aluminium accessories are particularly subject to corrosion. A neutral agent with a pHvalue between 6 and 8 should be used for such parts. Alkaline agents (pH > 8) must be avoided. Thus life time is increased and corrosion is reduced considerably.
7 Error Correction 7.1 Power Failure 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. It is important to distinguish between the main drying and final drying phase: The product is in the final drying phase when the residual moisture has reached approx. 5 %. Below this value the product is generally not damaged in the event of a power failure.
When using drying chambers with 8 connections for rubber valves the valves should be taken off and the connections should be sealed with rubber stoppers. To check the valves they are connected one after the other and tested under vacuum. Check the vacuum measuring sensor for pollution such as water residue. The vacuum measuring sensor has a limited life time due to its design principle. Vacuum sensors are available as a spare part (order no. 125479).
7.4 Insufficient Ice Condenser Temperature The refrigerator is equipped with thermal motor protection. In case of excess ambient temperatures or overload the protection device is released and the refrigerator is switched off. Once the permissible operating conditions are reached again (after a few minutes), the refrigerator is automatically switched on again via the motor protection switch. The minimum ice condenser temperature of approx.
Legends referring to the following drawings ALPHA 1-4 LD und ALPHA 2-4 LD "Refrigeration System ALPHA 1-4 LD/LSC" "Refrigeration System ALPHA 2-4 LD/LSC" Nr.
Declaration of Contamination Of Freeze Dryers, Vacuum-Concentrators, Centrifuges, Accessories and Vacuum Pumps. This declaration may only be filled in and signed by authorised staff. Repair Order dtd. : Order No. : Type of unit : Serial No. : Type of unit : Serial No. : Type of unit : Serial No. : Type of unit : Serial No.
Return Declaration Following declarations are for the health and safety of our employees. Fill in the forms and attach them when returning freeze dryers, centrifuges, spare parts and accessories. Please understand that we cannot carry out any work before we have the declarations. (We recommend that you make several copies of this page.