L S 4 0 / 6 0 F R E E Z E D R Y E R LS40/60 Freeze Dryer Instruction Manual Severn Science Limited 4 Short Way Thornbury Bristol BS35 3UL Info@severnscience.co.
L S 4 0 / 6 0 F R E E Z E D R Y E R CONTENTS 1.0 INTRODUCTION 1.1 Scope 1.2 General safety 1.3 General description 1.3.1 Freeze Drying – Basic Principles 1.3.2 The Condenser Unit 1.3.3 The Drying Chamber 1.3.4 Control System 2.0 TECHNICAL DATA 3.0 INSTALLATION 3.1 Unpack and inspect 3.2 Equipment Placement 3.3 Preparation of Vacuum Pump 3.3.1 Check Pump Oil Level 3.3.2 Vacuum Pump Settings 3.3.3 Pump Exhaust Connection 3.4 Preparation of Refrigeration System 3.
L S 4 0 / 6 0 F R E E Z E D R Y E R 4.6 Running a Freeze Drying Cycle 4.6.1 Run a program Now 4.6.2 Run a program from a Point 4.6.3 Scheduling a Program 4.6.4 End of Program Sequence (EPS) 4.7 Program Monitoring 4.7.1 Monitor Facility 4.7.2 Pre-Plot Facility 4.7.3 Trends 4.8 Holding a Program 4.9 Aborting a Program 4.10 Stoppering 4.11 Removing Product 4.12 Condenser Defrost 5.0 CREATING / EDITING A PROGRAM 5.1 Save / Save As 5.2 Inserting a Segment 5.
L S 4 0 / 6 0 F R E E Z E D R Y E R 8.0 ALARMS 8.1 Alarm Acknowledgment 8.2 Alarm History 8.3 8.4 Alarm Note Alarm History Archive 9.0 MAINTENANCE 9.1 Maintenance Plan 9.2 9.3 9.4 9.5 9.6 9.7 9.8 9.
L S 4 0 / 6 0 F R E E Z E D R Y E R Declaration of Conformity Manufacturer’s Name: Severn Science Ltd Manufacturer’s Address: 5 Short Way Thornbury, Bristol BS35 3UL England Model / Serial No: Date of Issue: Severn Science Limited hereby declares that the above product conforms with the essential protection requirements of: Low Voltage Directive 73/23/EEC amended by 93/68/EEC. EMC Directive 89/336/EEC as amended by 92/31/EEC.
L S 4 0 / 6 0 F R E E Z E D R Y E R 1.0 INTRODUCTION 1.1 SCOPE This manual provides installation and operation instructions for the LYOSCIENCE LS40 and LS60 freeze dryers. The manual and all accompanying documentation must be read before operating the equipment. Important safety information is highlighted as WARNING and CAUTION instructions; you must obey these instructions. The use of WARNINGS and CAUTIONS are defined in the general safety section.
L S 4 0 / 6 0 1.2 F R E E Z E D R Y E R GENERAL SAFETY WARNING: Warnings are given where failure to observe the instruction could result in injury or death to persons. CAUTION: Cautions are given where failure to observe the instruction could damage to the equipment, associated equipment or process. Refer to the accompanying manufacturers’ instruction manuals for the technical data on individual components. See Appendix 1 for list of Instruction Manuals.
L S 4 0 / 6 0 F R E E Z E D R Y E R 1.3.2 THE CONDENSER UNIT The condenser unit consist of a cylindrical chamber (290 X 620 mm) with an inlet port situated near the front of the chamber and a 25 mm outlet port positioned at the rear of the chamber. The chamber walls are cooled directly by an integral CFC free refrigeration system mounted in the base of the unit.
L S 4 0 / 6 0 F R E E Z E D R Y E R a common manifold and liquid re circulating pump. Sensors in the fluid circuit provide feedback for closed loop temperature control. Temperature control is achieved by modulating the flow of heated and cooled fluid with the use of solenoid operated isolation valves in the fluid circuit. The shelves are mechanically linked to an electrically actuated ram with variable torque drive.
L S 4 0 / 6 0 F R E E Z E D R Y E R Vacuum Pump 1. Type 2. Nominal Pumping speed 3. Pump down time (to 0.
L S 4 0 / 6 0 F R E E Z E D R Y E R additional air flow / air conditioning to ensure that the temperature at the inlet to the refrigeration heat exchangers is kept below 30oC. Please consult with Severn Science for further details. After placement, remove all panels to carry out initial inspection (see sections 3.3 and 3.4). The panels are fitted with lockable latches.
L S 4 0 / 6 0 F R E E Z E D R Y E R 3.4 PREPARATION OF REFRIGERATION SYSTEM The refrigeration plant in both condenser and drying units should be examined before use. First check that the refrigeration gas lines are not contaminated with moisture by examining the colour coded indicators (only applicable for LS40 models). If the indicators are yellow, do not use the equipment and contact Severn Science immediately. The cooling circuit in the drying unit uses a heat transfer fluid (silicone oil).
L S 4 0 / 6 0 F R E E Z E D R Y E R Locked level: This is the default level from power up and hence no password is required. At this level, the user can monitor the current status of the freeze dryer through a limited number of screens, but does not have the ability to make any parameter changes. The locked level is accessed by pressing the HOME button.
L S 4 0 / 6 0 F R E E Z E D R Y E R The new user can then log on using the new password at the designated security level. Note: The id is not user adjustable. Table 3. Additional id and Password codes id OP1 OP2 OP3 OP4 OP5 SUP1 SUP2 SUP3 SUP4 SUP5 Password OP1 OP2 OP3 OP4 OP5 SUP1 SUP2 SUP3 SUP4 SUP5 Access Level Operator Operator Operator Operator Operator Supervisor Supervisor Supervisor Supervisor Supervisor 4.
L S 4 0 / 6 0 F R E E Z E D R Y E R 4.4 SWITCH ON SHELF REFRIGERATION Security level : Operator or supervisor Cooling of the shelves in the drying chamber is provided by a separate refrigeration system. To turn the shelf refrigeration system on, follow the instructions below: a) From the Home screen press the field showing Refrigeration off on the right hand side of the screen (DRYING CHAMBER). From the options press ‘REFRIGERATION ON’. b) Press the green RETURN button.
L S 4 0 / 6 0 F R E E Z E D R Y E R Table 4: Vial Capacity and Inter-shelf Distances Vial Diameter (mm) 13.5 22.0 25.0 30.0 30.5 36.5 43.0 Vial Capacity 4 shelf 5 Shelf 3744 4680 1408 1765 1064 1330 768 960 720 900 3 shelf 2808 1056 798 576 540 351 264 Per Shelf 936 353 266 192 180 117 88 Number of Shelves Maximum working height (mm) Minimum working height (mm) 2 137 87 3 95 38 4 66 24 5 49 15 4.
L S 4 0 / 6 0 F R E E Z E D R Y E R c) Press the PROGRAMS button. The Load/Save Program screen will be displayed. d) Press the file name field . A list of program names will appear in the Options Menu (see figure 2 (c) ). From the list, press the name of the program to be loaded. Note: When the equipment is first delivered there will only be one program template called Prog 1. Once loaded this can be edited as required (see section 5). e) Press the green RETURN key.
L S 4 0 / 6 0 F R E E Z E D R Y E R f) Press the LOAD button. At this stage, the Programmer menu screen will appear. The program name and status will be displayed in the program panel in the top left hand corner of the screen. g) Press the RUN FROM button. A screen headed with the name of the program is loaded. The total running time for the program selected is displayed.
L S 4 0 / 6 0 F R E E Z E D R Y E R i) Press the ACCEPT button. The program will automatically start at the date and time shown in green at the top of the screen. 4.6.4 END OF PROGRAM SEQUENCE (EPS) The EPS function allows the user to select a method to complete the cycle after the initial freeze drying program is complete. EPS functions include automatic end point determination (EPD), secondary drying, backfill and stoppering. The functions are optional and can be activated manually if required.
L S 4 0 / 6 0 F R E E Z E D R Y E R CAUTION: When using the stoppering facility (automatic or manual), the stoppering jacks provided must be used. Instructions to set up the stoppering jacks are described in figure 4. Failure to do so may result in damage to the vial samples. 4.7 PROGRAM MONITORING The program monitoring function allows the operator to review program status in real time. This can be viewed as a list or graphically using the monitor and Pre-Plot facilities. 4.7.
L S 4 0 / 6 0 F R E E Z E D R Y E R function of time (‘X’ axis). Actual and set point data is colour coded as per the legends displayed on the right hand side of the screen. To review historical data and to zoom in on different parts of the graph, press the OPTIONS printed key (see figure 2(a) ) followed by the VIEW button. Pan and Zoom controls then appear on the major axes (see figure 5). A cursor (dotted vertical line) will also appear on the right hand side of the screen.
L S 4 0 / 6 0 F R E E Z E D R Y E R Press the ABORT button. The program will abort and the program panel will change to white and read ‘IDLE’. The program can then be run again from the start or a new program loaded (see section 4.6). 4.10 STOPPERING Stoppering can be pre programmed via the EPS facility (see section 4.6.4). Alternatively, shelves can be moved up and down by pressing the arrowed buttons located on the control panel and holding until the required shelf position is achieved.
L S 4 0 / 6 0 F R E E Z E D R Y E R 4.12 CONDENSER DEFROST Security level : Operator or Supervisor To turn the condenser off, press the field labelled ‘CONDENSER RUNNING’ from the Home screen. Select ‘CONDENSER DEFROST’ from the Options Menu followed by the green RETURN button. Note: a) When CONDENSER DEFROST is selected the air admittance valve will open, the vacuum pump and refrigeration system will switch off and the defrost heater will activate.
L S 4 0 / 6 0 F R E E Z E D R Y E R To configure the segment headings follow the instructions below: a) Press the segment heading that must be modified. A box displaying data about the segment will appear. To change the segment name press the segment field. Use the keyboard to input the required name (see figure 2(e) ). Press the green RETURN key. The Editor screen reappears, showing the new segment name.
L S 4 0 / 6 0 F R E E Z E D R Y E R 5.1 SAVE / SAVE AS To save the updated program under the same file name after editing is complete, or to save the program as a new file name, follow the procedure below. To insert or delete segments prior to saving, see sections 5.2 and 5.3 respectively. a) From the Editor screen, press the OPTIONS button on the printed keypad (see figure 2(a) ). b) To save the edited program under the same file name press the SAVE button.
L S 4 0 / 6 0 F R E E Z E D R Y E R 5.4 AMENDING THE END-OF–PROGRAM SEQUENCE (EPS) To amend the set points in the end-of-program sequence, first select the EPS screen. a) Automatic EPD. To amend the pressure rise limit, press the field labelled ‘mbarl/s’. Enter the required rate (in scientific notation) on the numeric keypad and press the green RETURN button. To amend the drying time programmed for EPD, press the field labelled ‘hrs’.
L S 4 0 / 6 0 F R E E Z E D R Y E R 6.1 CHANGING LOGGING CONFIGURATION Several data logging functions (e.g., archive interval, file type/name) are factory set. However, the logging configuration can be changed if necessary, as follows: a) Press the MENU printed key. b) Press the LOGGING button. The Logging Menu will appear. c) Press the SETUP button. The Logging Setup screen will be displayed, giving a summary of the logging configuration.
L S 4 0 / 6 0 F R E E Z E D R Y E R From this screen, pressure and temperature set points and the positions of system valves can be changed by pressing the appropriate field and either selecting an option from the menu or inputting the required value on the keypad. In both cases, press the green RETURN button to accept any selection. Note: Some of the above functions can also be manually controlled from the Home screen (see section 4).
L S 4 0 / 6 0 F R E E Z E D R Y E R CODE DESCRIPTION CAUSE FAIL-DRY APG Failure of drying chamber pirani gauge APGX1 calibration out of limits/ filament failure FAIL-COND APG Failure of condenser chamber pirani gauge APGX2 calibration out of limits / filament failure. FAIL-HI PRESS Evacuation time in chamber out of limits Vacuum pump or vacuum valve failure, system leak. FAILCONDTEMP Condenser temperature high Condenser refrigeration fail. High load.
L S 4 0 / 6 0 F R E E Z E D R Y E R The note is then added to the alarm history, where it is displayed along with its time of entry. 8.4 ALARM HISTORY ARCHIVE Security level: Operator or Supervisor The Archive facility permits the current alarm history to be saved in ASCII format to floppy disc.
L S 4 0 / 6 0 F R E E Z E D R Y E R Table 7: Maintenance Plan OPERATION Check the vacuum pump oil level Change the oil mist filter element Inspect the oil drain kit Change the vacuum pump oil Service the vacuum pump Check condition of door seals FREQUENCY Weekly REFER TO SECTION 9.2 6 Monthly 9.3 Monthly 6 monthly 9.4 9.5 Yearly 9.6 Weekly 9.7 Monitor the drying Weekly chamber silicon fluid level Check cleanliness of both Monthly refrigeration systems heat exchangers 9.8 9.9 9.
L S 4 0 / 6 0 F R E E Z E D R Y E R pump out of the framework. Inspect and clean the vacuum pump inlet filter, gas ballast control, oil sight glass and motor fan cover, as described in the pump instruction manual. When refitting, ensure that all fittings are correctly reconnected to the vacuum pump. 9.7 DOOR SEALS Routinely inspect the door seals fitted to the drying and condenser chamber.
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 1.
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 2(a). Controller Layout 0/0 TEST PROG IDLE ???? HOME 12:52:29 TEMP. -80.0 C 19/05/01 TEMP. -60.0 C PRESS. 1.0E-02 mbar PRESS. 7.0E-01mbar CONDENSER RUNNING REFRIGERATION ON DRAIN OPEN VENT OPEN STATUS Printed keypad EPS Options key SETPOINT -60 C CYCLE STATUS FINISHED Floppy disk drive (1.44Mb disk required) Menu key Flip-front protective cover Figure 2(b).
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 2(c). Drop down menu (option list) Selecting certain fields will reveal a drop down menu with an options list. 0/0 TEST PROG Options menu IDLE ???? CONDENSER 12:52:29 RUNNING HOME CONDENSER RUNNING TEMP. -80.0 C Select option Press to accept option CONDENSER DEFROST 19/05/01 TEMP. -60.0 C PRESS. 1.0E-02 mbar PRESS. 7.0E-01mbar CONDENSER RUNNING REFRIGERATION ON DRAIN OPEN VENT OPEN STATUS SETPOINT -60 C CYCLE STATUS FINISHED EPS Figure 2(d).
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 2(e). Keyboard Selecting certain fields reveals a keyboard for text entry 0/0 TEST PROG IDLE ???? HOME 12:52:29 PASSWORD 19/05/01 Q W E R T Y TEMP U . I-60.0 O PC D Fmbar J K7.0E-01mbar L ; A S1.0E-02 G HPRESS. PRESS. CONDENSER RUNNING Z X C V B REFRIGERATION N M , ON TEMP. -80.
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 3. Status screen The status screen provides a summery of the present condition of the freeze dryer functions. Note: Any conditions highlighted in RED will prevent an automatic program cycle from running.
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 4. Stoppering Jacks Height adjustable shaft 19mm jack base Lock nut 49mm jack base Vial height 32mm – 42mm 42mm – 52mm 52mm – 62mm 62mm – 72mm 62mm – 82mm 70mm – 90mm Jack base required 19mm 19mm 19mm 49mm 49mm 49mm Cap screw shaft length required 20mm 30mm 40mm 20mm 30mm 40mm Mechanical stoppering jacks must be used when stoppering glass vials.
L S 4 0 / 6 0 F R E E Z E D R Y E R Figure 5. The pre-plot facility 0/0 TEST PROG IDLE ???? PROG 1 12:52:29 Condenser temperature trend Shelf temperature trend 19/05/01 CONDENSER TEMP 7.5 deg C TEMP. -80.0 C TEMP. -60.0 C SHELF PRESS. 1.0E-02 mbar PRESS. 7.0E-01mbar TEMP 0.
L S 4 0 / 6 0 F R E E Z E D R Y E R Appendix 1: Manufacturers Literature a) T800/T2900 Visual Supervisor (Eurotherm Controls) b) 2500 PID controller (Eurotherm Controls) c) 605 series drive unit (Eurotherm Controls) d) Cascade refrigeration system (Ernest West & Beynons) e) RV12 rotary pump (BOC Edwards) f) EMF adjustable gas ballast oil drain kit (BOC Edwards) g) EMF10 Oil mist filter (BOC Edwards) h) Active pirani gauge (BOC Edwards) i) Screw jack assembly (Precision Actuation Systems) j) Induction mo
L S 4 0 / 6 0 F R E E Z E D R Y E R Appendix 2: List of Drawings Electrical circuit diagram, 7705 rev A Publication reference 1HZ204-1 41
