Operating Manual Freeze Dryer ALPHA 1-4 LSC Part. No. 102041 ALPHA 2-4 LSC Part. No. 102042 Version 09.
OPERATING MANUAL ALPHA 1-4 LSC / ALPHA 2-4 LSC Order Number: Serial Number: In case of inquiries please state the above numbers. For service please contact: MARTIN CHRIST Gefriertrocknungsanlagen GmbH An der unteren Söse 50, D-37520 Osterode Phone +49 (0) 5522 / 5007-25, Fax +49 (0) 5522 / 5007-12 eMail: service@martinchrist.
Preface Dear customer Congratulations on purchasing a CHRIST freeze dryer. The freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC is equipped with a lot of user-friendly options which make the operation easier for you. The newly designed ALPHA 1-4 LSC / ALPHA 2-4 LSC 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. 1.6. 2. 3. 3.2. 3.3. 3.4. 3.5. 19 Freezing and drying inside the ice condenser chamber (process A) on a temperature-controlled shelf...............................................19 Separate freezing and drying outside the ice condenser chamber (process B) on temperature-controlled shelves .............................................20 Separate freezing and drying outside the ice condenser chamber (process B) with sealing device ..............
5. LSC Control System 5.1. 5.2. 5.3. 5.4. 5.5. 5.6. 5.7. 5.8. 6. 7. 7.4. 73 Power failure ..................................................................................................73 Insufficient vacuum ........................................................................................73 Unit does not work .........................................................................................74 Heating unit is not activated...........................................................
7.5. 7.6. 7.7. 8. Vacuum pump ................................................................................................83 Exhaust filter ..................................................................................................84 Cleaning .........................................................................................................84 7.7.1. Cleaning the freeze dryer .................................................................84 7.7.2. Cleaning the accessories ...............
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 vapor. This happens under vacuum and the temperature in the product is normally less than -10°C. The aim of freeze drying is to obtain a readily water-soluble product which has the same characteristics as the original product after addition of water.
1.2. Areas of application The freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC is a highperformance 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 data of freeze dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Performance data ALPHA 1-4 LSC ALPHA 2-4 LSC Ice condenser capacity: 4 kg max. 4 kg max. Ice condenser performance1): 4 kg/24 h max. 4 kg/24 h max. Ice condenser temperature1): approx. –55°C approx. –85°C Possible shelf temperatures when freezing and drying inside the ice condenser chamber (process A) 1): approx. -25 °C to +99°C approx.
Performance data ALPHA 1-4 LSC ALPHA 2-4 LSC Drying in round-bottom flasks; please notice that the max. ice condenser capacity is 4 kg (process B): 12 pieces or 24 pieces 12 pieces or 24 pieces Dimensions of the unit: width: 390 mm height: 415 mm depth: 555 mm (incl. vacuum flange connection) width: 390 mm height: 415 mm depth: 555 mm (incl. vacuum flange connection) Weight: approx. 48 kg approx.
Performance data ALPHA 1-4 LSC ALPHA 2-4 LSC Main fuse rating: 10.0 A 12.0 A Ambient temperature1): +10°C to +25°C (higher temperatures upon request) +10°C to +25°C (higher temperatures upon request) Vacuum connection: Small flange connection DN 25KF (ISO 28403, DIN 2861) Small flange connection DN 25KF (ISO 28403, DIN 2861) Drain valve: Hose nozzle DN10 (outside diameter 12 mm) Hose nozzle DN10 (outside diameter 12 mm) Aeration valve: Hose nozzle DN4 (outside diameter 8 mm) max. 0.
1.4. Standards and regulations Please refer to the enclosed EU Declaration of Conformity. 1.5. Safety instructions 1.5.1. CAUTION! Disconnect the mains plug! As current-carrying parts are accessible inside the unit the mains plug must be disconnected before the side panels or the rear panel 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.
1.5.5. NOTE! 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 setting up the unit, do not hold the unit at the plastic control panel. When putting the unit down on a surface, there is a danger of squeezing hands or fingers.
1.6. Prohibited freeze drying processes 1. Operation of the freeze dryer when it is not properly installed. 2. Operation of the freeze dryer without panels. 3. Operation of the freeze dryer by non-authorized personnel. 4. Operation of the freeze dryer when the shelves are not properly installed. 5. Operation of the freeze dryer with highly 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 gentlest 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 dried under vacuum without thawing. The ice condenser can also be described as a vapor pump as the moisture which evaporates under vacuum during drying freezes onto the ice condenser.
Sublimation The principle of sublimation is briefly explained using the phase diagram of water (freeze drying of mainly aqueous solutions, see vapor 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 6.11 mbar the melting pressure curve, vapor pressure curve and sublimation pressure curve meet in one point called triple point.
Conversion table "Vapor pressure above ice" (sublimation curve) Pressure units: 1mbar = 100Pa 1Pa = 0.01mbar Temperature units: T = t + 273 t = T − 273 t F = 1.8 ⋅ t + 32 t − 32 t= F 1 .8 T = thermodynamic temperature K (Kelvin) t = temperature in degree Celsius °C tF = temperature in degree Fahrenheit °F °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.
2.2. Preparation In case the unit is equipped with a pressure control valve the vacuum pump should be warmed up. The operating 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 prefrozen 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 and the aeration valve are closed.
Warning: Acidic products or products with a high solvent concentration cannot be dried without special safety measures and devices, such as an additional LN2 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).
During the main drying phase the moisture is removed by sublimation, during final drying the bound moisture is removed by desorption. This small quantity of water vapor 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). In general, operation with closed gas ballast valve is not necessary.
The drying time depends heavily on the drying vacuum. The nearer the vacuum to the solidification point in accordance with the vapor pressure curve above ice, the shorter the drying time. Interesting correlations: 1.0 gram of ice at 1.0 mbar assumes a volume of 1 m³ vapor 0.1 mbar assumes a volume of 10 m³ vapor 0.
Heat transfer takes place via the heated shelves by direct contact with the bottom of the vessel and/or by convection via the shelf and vessel or product. 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.
2.6. End of drying and aeration A rough indication of the end of drying is the vacuum and the ice condenser temperature. The ice condenser is no longer loaded and reaches the final temperature of approx. -55°C to -85°C. The pressure in the drying chamber decreases according to the ice condenser temperature. The end of the drying process is reached when the temperature of the product and that of the shelves are about 15 to 20°C.
3. Description of the Freeze Drying Processes 3.1. Freezing and drying inside the ice condenser chamber (process A) on a temperaturecontrolled shelf First, 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. The refrigeration unit and the vacuum pump are activated via the control system to pre-cool the ice condenser and to warm up the vacuum pump.
In order to seal the bottles, the shelf must be completely filled. For small quantities, at least three spacers must be distributed evenly on each shelf (according to the height of the bottles with inserted rubber stoppers). Suitable spacers are available upon request. 3.2. Separate freezing and drying outside the ice condenser chamber (process B) on temperature-controlled shelves The product can also be dried outside the ice condenser chamber. In this case, the product has to be frozen first, e.g.
To control the shelf temperature, one shelf with a measuring sensor has to be connected. The plug of the shelf with the measuring sensor has to be connected to the socket of the vacuum-tight electrical leadthrough.
3.3. Separate freezing and drying outside the ice condenser chamber (process B) with sealing device 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. The refrigeration unit and the vacuum pump are activated via the control system to pre-cool the ice condenser and to warm up the vacuum pump. The valve is closed during the warm-up of the vacuum pump.
3.4. Separate freezing and drying of liquids in flasks (process B) 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. The refrigeration unit and the vacuum pump are activated via the control system to pre-cool the ice condenser and to warm up the vacuum pump. The valve is closed during the warm-up of the vacuum pump.
Using a distributor, a maximum of 15 ampoules can be simultaneously frozen in the cooling bath and connected to the manifold. 3.5. Separate freezing and drying of liquids in ampoules (process B) The refrigeration unit and the vacuum pump are activated via the control system to pre-cool the ice condenser and to warm up the vacuum pump. The valve is closed during the warm-up of the vacuum pump.
4. Installation and Commissioning of the Unit 4.1. Site of installation ATTENTION! In order to ensure the air circulation of the heat exchanger, do not place any paper, cloths or similar items behind the unit. The freeze dryer should be positioned horizontally. The ambient temperature should be between approx. +10°C and +25°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 power The operating voltage on the name plate must correspond to the local supply voltage. CHRIST freeze dryers are units of safety class I. The units ALPHA 1-4 LSC / ALPHA 2-4 LSC are equipped with a three-wire connection cable with a 230VAC safety plug with ground contact. 4.3. Fuses on site The freeze dryer must be protected with a 16 AG fuse. 4.4.
4.7. Vacuum pump exhaust gases During the main drying phase, the separate vacuum pump must be operated with open gas ballast valve. The oil mist that is produced is normally trapped in an exhaust filter. If this is not the case, the oil mist has to be discharged. A ½" hose can be connected to the exhaust flange of the vacuum pump RZ-2 or RC-5 and a ¾" hose can be 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.
4.8. Initial start-up ATTENTION! Prior to start-up, make sure that the freeze dryer has been properly set up and installed (see section 4.1 “Site of installation” and the following points). 4.8.1. Functional components and control elements Aeration valve Drying chamber Ø300 Ice condenser chamber Ice condenser Control system LSC Mains switch Additional interface connection (option, sep.
4.8.2. Vacuum sensor, vacuum pump and pressure control valve connection Connection diagram Process A (single-chamber system): Freezing and gentle drying of low-freezing and thermolabile substances on cooled shelves inside the ice condenser chamber (see figure 1). Typical drying vessels:: • Dishes • Injection vials (can be sealed under vacuum) Process B (double-chamber system): Separate freezing (e.g.
The accessory components are connected to the ALPHA 1-4 LSC / ALPHA 2-4 LSC freeze dryer according to the connection diagram. Please observe the following: Centering rings and clamping rings with wing nuts are used as connecting elements (small flange connections in accordance with ISO 28403 and DIN 2861, see also the following instructions).
Installation of the VSP62 vacuum sensor The vacuum sensor has to be connected to the vacuum connection at the back of the unit in an upright position using a centering ring and a clamping ring. The sensor connecting cable has to be connected to the corresponding socket at the back of the unit. After power-on, the vacuum sensor needs a few minutes to reach its operating temperature.
Installation of the vacuum pump The vacuum pump has to be connected to the unit and to the socket at the back panel of the unit. Make sure that the vacuum exhaust gases are filtered or carried off.
4.8.3. Installation of accessory components Further accessories (e.g. shelves, connections for round-bottom flasks) are added in accordance with the scope of supply. The drying chamber or a lid is placed on top of the ice condenser chamber.
Process B 34 • Installation and Commissioning of the Unit Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Process B Drying chamber Ø457 Rubber valve Connection piece for rubber valve to extend the drying chamber, 18 pieces max. Distributor Drying vessel, e.g. ampoule 5 shelves max., Ø375 heated Drying vessel, e.g. round bottom flask Drying vessel, e.g.
Process B Ground-in stopper Drying chamber Ø300mm Rack with 10 shelves max.
Process A Sealing device Acrylic lid Shelf Ø200 Drying vessel, e.g. injection bottle ALPHA 1-4 LSC ALPHA 2-4 LSC 4.8.4. Preparations for freeze-drying Close the aeration valve and the drain valve on the left side of the unit. If rubber valves are included in the system (located at the drying chamber), they have to be closed. 4.8.5. Power-on Press the mains switch on the right side of the unit to switch the unit on. At first, the LSC control system performs a self-test. This may take several seconds.
5. LSC Control System 5.1. Introduction LSC (Lyo Screen Control) stands for a graphical user interface that is used to control freeze drying processes. The operation of the unit is very easy and self-explaining with the “turn & push” button. Most of the process data are displayed either in a detailed table or in a clear flow diagram. 5.1.1. LSC control panel Fig. 1 1. 2. 3. 4. 5. 6. 7.
5.1.2. Brief description of operation The LSC control system is operated via the central turn & push button and four function keys at both sides of the control panel . The turn & push button is the main element for operating the control system. Turning the turn & push button positions the focus on the desired function in the menu or in the window. Pressing the turn & push button activates the selected function. Parameters (set values, etc.) are entered in the same way.
5.2. Visual components of the LSC control system The LC display is divided into the three following areas: Fig. 2 5.2.1. • Menu bar • Window area • Status bar Presentation on the LC display Menu bar The menu bar includes 5 menu tabs: VALUES, MANUAL, PROGRAM, OPTIONS, ? (Help). These menu tabs offer all configurations, parameters and operation modes of the unit. The focus can be positioned on the desired tab by turning the turn & push button to the left or to the right. Fig.
Press the button Fig. 4 to confirm the selected menu. Selected focus in the menu bar The system opens a pop-up menu or a new window. Fig. 5 5.2.2. Presentation of a pop-up menu Window area The main window covers the whole window area. Pop-up menus or dialog boxes are shown in front of the main window so that the main window is always in the background. Settings can only be modified in the active window in the foreground.
5.2.3. Pop-up menus There are two different types of pop-up menus: Pop-up menus that are opened by selecting one of the main menu tabs (first-level pop-up) and second-level pop-ups that are opened by selecting a menu item from a first-level pop-up menu. The main menu tab is also used to close the menu of a first-level pop-up. Close menu Symbol for a second-level pop-up Fig.
equipment information system is an exception since this dialog box is opened automatically by the system. Fig. 8 Dialog box The following control elements are included in the dialog boxes: 5.2.3.2. • Button: Buttons are used to confirm or to close a window. • Scrollbar: The scrollbar is used to enter higher-order parameters. • Radio button: A radio button is used to select a certain configuration. • Parameter field: All other fields that can be focused are used to enter parameters, e.g.
The lower part of the window shows an animated mimic diagram with active components (symbols). The active components of the unit are the ice condenser, the vacuum pump, valves, the electrical heating unit for shelves and the fan in the ice condenser chamber. The symbols are shown completely filled-up during operation. Anfang ALPHA1-4/2-4LSC Fig. 10 Mimic diagram of ALPHA 1-4 LSC / ALPHA 2-4 LSC Example for active components: Fig. 11 Ice condenser and fan for ice condenser chamber are not active Fig.
Values window The values window compares set values and actual values of the running process in a clear manner. Fig. 14 Values window The display of the actual values offers a special feature: The operator can select six actual values and assign them to the different display positions. In order to assign these six values select the menu VALUES Æ Display configuration. Fig.
The following actual values can be selected via the sub-scrollbar: - Time h:min (current time) - Tot. h:min (total process time) - Sec. h:min (time of process phase) - Vacuum mbar (actual vacuum value) - Condens.°C (ice condenser temperature) - Shelf °C (shelf temperature) - Product °C (product temperature) - Lyo Rx % (optional) - Lyo Prod.°C (optional) In case a position should not present an actual value, select --blank-- from the sub-scrollbar.
5.3. Function keys Function key “Standby” The function key “Standby” is used to switch off all aggregates. This function is always available (from every opened window). Usually, the drying process is finished with the “Standby” function before starting the manual aeration. Function key “Run” The freeze drying process is started with the “Run” key. In the manual mode, aggregates are switched on depending on the selected phase.
Fig. 18 Dialog box “Device locked!“ The control panel can be unlocked by pressing the function key again for 2 seconds. Function key “°C≙mbar” This function key can be used to convert the temperature of the ice condenser chamber or the vacuum in the drying chamber according to the vapor pressure curve above ice by means of a table.
switch manually to the next phase without setting the unit to the standby mode. When all desired phases are finished – usually after the final drying phase – the process is finished by pressing the function key “Standby” . In the manual mode, the duration of the different phases is determined by the operator. It is not timercontrolled.
Fig. 21 Dialog box for the input of set values in the manual mode To enter set values, select the corresponding nominal value set (phase) from the scrollbar. To do so, focus the scrollbar with and confirm the selection with . The scrollbar is now in the selection mode, i.e. the desired nominal value set can be selected with . The corresponding current set values of this phase are shown. Press the confirmation key to exit the selection mode. Fig.
5.4.3. Set values for manual main drying and final drying Fig. 25 Nominal value set for main drying and final drying The set values “vacuum” and “safety pressure” are locked against each other. In this way the input of inadmissible nominal values is prevented. (Only a certain safety pressure can be selected. The corresponding temperature of the ice pressure curve of this pressure must be at least 5K higher than the one of the set value for the vacuum.) Valid range of values: Shelf: -100°C ..
automatically after the set defrosting time (see VALUES Æ Set Values for Manual Mode). It is not possible to start the defrosting phase during an active phase (freezing, main drying, final drying). The unit has to be in the standby mode. During the defrosting process, it is not possible to select any of the other phases (freezing, main drying, final drying). In this case it is also necessary to switch the unit to the standby mode first. In addition, it is important that the chamber is completely vented, i.
Pressure difference = actual vacuum value at the beginning of the measurement - current actual vacuum value Open intermediate valve Fig.28 Close intermediate valve Intermediate valve between the drying chamber and the ice condenser Press to finish the pressure increase measurement. The values for the pressure difference and the measuring time are frozen. They are indicators for the current amount of water vapor and thus for the residual moisture content of the product.
5.5. Programmer module (optional) 5.5.1. General information The programmer module PGM-30 is used for a timer-controlled pre-programmed process (freeze-drying program). A freeze-drying program is divided into several sections. Every section of the program has set values for the phase, the section time, the shelf temperature, the vacuum, the safety pressure and dT freezing/drying. The PGM-30 can store up to 30 individual programs. Up to 32 sections can be assigned to each program.
warm-up phase. As a result, the pressure inside the chamber is not affected. Fig. 31 The programmer module shifts the warm-up phase into the freezing phase so that it takes place prior to the first drying section The programmer module data “set values”, “actual values” and “status” are shown at the usual locations in the values window, in the mimic diagram and in the status line. Fig. 32 Pop-up window of the programmer module The programmer module can be activated by selecting the Program menu.
5.5.2. Creating a new Program In order to create a new program, select a free location under Program Æ New. Free program locations are marked by < --->. After the selection of a program location, the program editing mode is activated. As a program base, the standard program named “Christ” is created. The standard program can be customized by changing set values or by deleting or adding sections. The date of creation of the program is set to the current date.
entered. The user code is defined under OPTIONS Æ Misc. Æ Security. Fig. 35 Dialog box for entering the user code The programmer module always shows 3 sections in order to make the connection with the previous and the section clear. The first section is always defined as “loading”. In this section, the start conditions of the program are defined. All other sections will be executed one after another.
exit the editing frame, select the top focus position (section number). Inserting a section This button inserts a new section at the section position in the editing frame. The set values are copied from the selected section. A maximum of 32 sections can be defined. Deleting a section This button deletes a section at the section position in the editing frame. A program consists of at least 3 sections. Additional set values 5.5.3.1. • Warm-up vacuum pump Defines the time for the warm-up of the vacuum pump.
Fig. 37 General program information 5.5.4. Loading a program Select the program under PROGRAM Æ Load. A dialog box opens showing general program information. The start section and the time for starting the section can be set as desired. to load the program. The dialog box is closed and Press the status bar is updated. Press the function key “Run” to start the program. Fig. 38 Dialog box “Load program“ Fig.
5.5.5. Copying a program Select the program to be copied (source program location) under PPROGRAM Æ Copy. Only program locations that actually contain a program can be copied. If a program location is free, the selection will be ignored. If all 32 program locations already contain a program, the selection will be ignored, too. After the selection of the program, a dialog box opens showing general program information. The LSC control system suggests a free program location as the target program location.
5.5.7. Delta t freezing/drying Preselection of the maximum admissible difference between the shelf temperature and the product temperature at the end of a section. The unit only switches to the next process phase if the actual difference is below the set value. If, for example, the shelf temperature during the freezing process is set to -40°C and a product temperature of at least -30°C has to be ensured before the “main drying” process can start, the admissible difference is +10K.
Test time During the test, the ice condenser is separated from the drying chamber. The pressure increase is analyzed after the test time. If the pressure increase has to be measured during the execution of the program, the corresponding option checkbox must be selected. Fig.42 Parameters for the pressure increase measurement 5.6. Process and equipment information system The process and equipment information system shows and saves malfunctions and messages.
Current error/message code Total number of errors and messages Description Error/message status Confirm Close the process and equipment information system Fig. 43: Dialog box for the process and equipment information system The following messages are displayed in the process and equipment information system: 5.6.1. Process messages For messages referring to hardware errors please see chapter 6.7.1. Code 03 Safety pressure was fall below and exceeded again during the drying process.
This error message is displayed if the program fails to perform two successful pressure increase measurements in a row at the end of a section. The section is extended. Code 22 Note: dT Freezing/Drying Producttemp.1 ist out of limit at section end. See also chapter 5.5.7 “Delta t freezing/drying” Code 24 Maintenance interval reached. Perform maintenance or contact local service. See also section 5.7.5 “Maintenance of the freeze dryer” Code 25 Shelf temperature has not been reached at section end.
5.7. Options The OPTIONS menu is used to enter elementary configurations of the control system. Fig. 44 Options menu 5.7.1. Info Select the menu item Info to open the process and equipment information system. Saved messages or errors can be read here. 5.7.2. Display contrast The contrast of the LC display has to be modified depending on the lighting conditions and the visual angle. Open the corresponding dialog box under OPTIONS Æ Contrast. Position and , i.e.
Fig. 45 Dialog box for setting the contrast 5.7.3. Language To set a language, select OPTIONS Æ Language. Turn the turn & push button to select the corresponding flag and confirm it with . Afterwards the mimic diagram is shown using the new language. Fig. 46 Dialog box for selecting the language 5.7.4. Changing the date and time The LSC control system is equipped with a built-in clock with a buffer battery. The clock has to be reset after a failure of this buffer battery.
Set the current values for day, month and year und confirm these settings with . To set the time, proceed as follows: Set the current values for hour and the next minute. When the minute changes, confirm the new setting with . The counter of the seconds will be reset to zero. Example: The current time is 10:23:15 [hour:min:sec]. Hence the time to be set is 10:24 [hour:min]. Confirm the new setting by pressing when the minute changes to 10:24:00 [hour:min:sec]. Fig. 47 Dialog box for date and time 5.7.5.
5.7.6. Maintenance intervals of the vacuum pump The maintenance intervals of the vacuum pump can be defined and reset under OPTIONS Æ Misc. Æ Vacuum Pump. The following maintenance intervals can be selected: 100, 200, 300, 400, 500, 1000, 2000, 3000, 4000 hours. If the interval is set to ∞ hours, the system will never display any maintenance messages. Fig. 49 Dialog box showing the maintenance intervals of the vacuum pump 5.7.7. Process This dialog box can be opened under OPTIONS Æ Misc. Æ Process.
Fig. 51 Mimic diagram process A Fig. 52 Mimic diagram process B 5.7.8. Unlocking This dialog box can be opened under OPTIONS Æ Misc. Æ Unlock. A six-digit keyword has to be entered. Fig. 53 Dialog box for unlocking There will be a long sound signal (about 1 s) in case an invalid keyword is entered. If the keyword is accepted, there will be a short sound signal. 5.7.9. Security The menu item OPTIONS Æ Misc.
Fig. 54 Dialog box for entering the old user code There will be a long sound signal (about 1 s) if a wrong user code is entered. If the user code is accepted, there will be a short sound signal. Fig. 55 Dialog box for the entering the new user code 5.7.10. System calibration A dialog box showing all the values that are necessary for a calibration can be opened under OPTIONS Æ Misc. Æ Calibration. Fig.
Two calibrations are possible: the calibration of the IO sensor card and the calibration of external measuring modules (Pirani and Lyo Control). LSC Sensor IO The LSC sensor IO card processes analog measuring signals such that they can be processed by the control system in the form of digital signals. The calibration is performed once at the factory. PT 100 temperature sensors In order to adjust the PT100 sensors of the freeze dryer, the "LSC Temperature Adjustment Tool" (part no. 135504) is required. 5.8.
6. Troubleshooting 6.1. Power failure The control system continues with the process after a power failure. The pre-selected conditions remain saved even during an automatic process. In the event of a power failure in the drying phase, the batch may become unusable. Whether the batch can be saved or not depends on the drying phase in which the product was when the power failure occurred.
Please proceed in the same way in case of a leak in the aeration valve. Check the lid seal for dirt or damage. If necessary, it must be cleaned or replaced. Ensure that the entire surface of the ground-in stopper of the attachable drying chamber is greased with vacuum grease. When using drying chambers with several connections for rubber valves, the valves should be removed and the connections should be sealed with rubber stoppers.
Check the internal fuse 202F3. 6.4. Heating unit is not activated Please note that during the main drying phase and during the final drying phase the heating unit is not activated until the preset safety pressure is reached. If the heating unit is not activated even though the pressure is below the safety pressure, please check the fuse 202F1. 6.5. Fan (ice condenser chamber) is not activated Check the precision connection in the ice condenser chamber. Check the internal fuse 202F2.
The refrigeration unit is automatically switched off in these cases. Once the permissible operating conditions are reached again (after a few minutes), the refrigeration unit is switched on automatically via the motor protection switch or via the pressure switch. Important errors are indicated by the process and equipment information system. The minimum ice condenser temperature of approx. -55°C or 85°C is reached when the ice condenser is not loaded and the ice condenser chamber is evacuated.
Code 04 Excess temperature “ice condenser”. Temperature “ice condenser” is 65°C or more! Freeze Dryer was switched into Standby. This error occurs when the temperature of the ice condenser exceeds +65°C. At the same time, all active units are switched off, i.e. the system is automatically switched to standby mode. The error message may occur when the temperature of the ice condenser exceeds +65°C when defrosting the system.
Code 29 See chapter 5.6.1. Code 30 Note: Error in configuration memory. Please verify user defined parameters and check the back-up battery. This error message is displayed when the system is switched on and the buffer battery power for the settings and the real-time clock is too low. Please replace the buffer battery. Then it is necessary to reset the clock (see chapter 5.7.4). The settings (setpoints, etc.
Code 36 AC power failure L2 Power failure in phase L2. Please check the on-site fuses. Code 37 AC power failure L3 Power failure in phase L3. Please check the on-site fuses. Code 38 Excess temperature liquid for temperature control shelves The temperature-control liquid has exceeded the upper limit. The heating unit for the temperature-control liquid is switched off. The heating unit is not reactivated until the temperature-control liquid has fallen below a lower limit.
This error message is displayed, if the temperature sensor is either not connected or defective. Please call customer service.
7. Maintenance 7.1. Ice condenser chamber Before each start-up, ensure that all water residues have been removed from the ice condenser chamber. If necessary, wipe the ice condenser chamber dry. Before every drying process it is recommended to open and close the drain valve. 7.2. Heat exchanger A laminated heat exchanger is used to cool the refrigerant compressed by the refrigeration unit.
A freeze dryer should be aerated and the dry product should be removed at the end of the drying process. Then the system should be defrosted with warm water (+50°C max.) while the drain valve is open. Then the drying chamber has to be wiped dry. Do not simply let the freeze dryer stand at room temperature for a long period of time since this is the time during which the tungsten wire reacts with the surrounding atmosphere! In addition, it is recommended to evacuate the unit for approx.
Calibration to a specific zero reference value: To perform the calibration, the actual pressure must be lower than 1.0x10-2 mbar. After pressing of the button labeled “set”, the actual vacuum field of the LSC control system shows a value corresponding to the zero adjustment value currently set (factory setting 0.0010 mbar). The button labeled “adj” can now be used to increment this value up to a maximum of 1.0x10-2 mbar. As of this value, the output starts again at 0.0010mbar.
7.6. Exhaust filter If the unit is equipped with an exhaust filter (necessary if the exhaust gases cannot be extracted into the open air or into a vent), take care that the condensate in the filter does not rise too high. The condensate is drained using a waste oil drain screw at the filter. (Please refer to the separate operating manual!) 7.7. Cleaning 7.7.1. Cleaning the freeze dryer Use soap water or other water-soluble, mild cleaning agents to clean the freeze dryer.
If there is the risk of toxic, radioactive or pathogenic contamination, special safety measures must be considered and adhered to. Aluminium accessories are particularly prone to corrosion. A neutral cleaning agent with a pH-value between 6 and 8 should be used for such parts. Alkaline cleaning agents (pH > 8) must be avoided. This increases the service life and considerably reduces the susceptibility to corrosion.
7.7.5. Checks by the operator The operator has to ensure that the important parts of the freeze dryer that are necessary 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 abrasion of material etc. Furthermore, a ground conductor check must be carried out regularly.
8. Options 8.1. Process control system LPC-32, software 8.2. Process control system LPC-32, software with PC hardware 8.3. Programmer module PGM 30 8.4. Extension unit HED-16 LSC 8.5. LyoLog LL-1 (documentation software) 8.6. Pressure increase test 8.7.
8.8. Electrical lifting device Only for ALPHA 1-4/2-4 LSC GAMMA 1-16 LSC / 2-16 LSC and DELTA 1-24 LSC / 2-24 LSC ALPHA 1-4/2-4 LDplus BETA 1-8/28LDplus 8.9. Solvent-resistant version 8.10. IQ / OQ 8.11. Cooling bath CB 18-40 8.12. Cooling bath Subject to technical changes.
9.
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Enclosures • 91
92 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC Enclosures • 93
94 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
96 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
98 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
100 • Enclosures Operating Manual Freeze Dryer ALPHA 1-4 LSC / ALPHA 2-4 LSC
10.
serielle Schnittstelle Vakuummesssonde Serial interface of vacuum measuring sensor Interface sérielle du capteur de vide Anlagensteuerung LSC Control system LSC Système de contrôle LSC Netzschalter Mains switch Commutateur d’alimentation Belüftungsventil Aeration valve Soupape de ventilation Ablassventil Drain valve Vanne de vidange Eiskondensatorkammer Ice condenser chamber Piège Eiskondensator Ice condenser Condenseur serielle Schnittstelle serial interface Interface sérielle Anschluss Spannungsvers
