Mini Lyotrap - Wolf Laboratories
Contents
1. e i 3 Rubber valve a 7D oO cg d l CT Glass tube Glass flasks Ka R Ss EN f f j KE D CL Section Gasket Vacuum Hose K ne Frozen in Time Ltd oo www freezedriers com x L Drai Lablyo Mini rain valve FIT LYO 13 0 Column manifold 8 port Additionally requires 1x LU section gaskets FIT LYO 40 0 8 x Quick seal valves FIT LYO 43 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 24 4 7 6 8 port lid manifold L Section Gasket Rubber valve NE a a V VS Glass tube YN fg N J N i 4 L Section Gasket Vacuum Hose Lablyo e D EE M Mini Frozen in Time ua oo SCH N gaco SS Vacuum pump Se s ee p oo NN 9 www freezedriers com Le J IW o oJ Drain val Lablyo Mini Felt Valve FIT LYO 6 0 Additionally requires Lid manifold 8 port Acrylic drying chamber FIT LYO 01 0 2 x VU section gaskets FIT LYO 40 0 8 x Quick seal valves FIT LYO 43 0 Additionally options 6 shelf rack FIT LYO 03 0 6 x Trays 230mm FIT LYO 34 0 To use the Lid manifold as a plain lid without valves it can be turned upsid2. 3 2 6 Drying with a 48 port ampoule manifold 3 2 7 The Lablyo Mini as a standalone cold trap 4 Installation and Commissioning of the Unit 4 1 Site of installation GEET 4 3 Air ell Ee 4 4 Condensate and defrosting water 4 5 Vacuum pump exhaust oases eee cece cent eeeeeeeeaeeeeeeeeeaeeeeeeeaaes 4 6 linitial Start Up EE 4 7 Installation Of accessories esses 4 7 1 Vial closing device sss 4 7 2 48 port ampoule manttold 4 7 3 Spin fre Ze 2 ccc cece niaaa eai adii 4 7 4 Heated abelves 2 20 0 ccecececeeeee eect cece eeeeeeeeeeeeaees 4 7 5 8 port column manitold eee ee eee eens eeeees 4 7 6 8 port lid mantold cece eee eeeeeeeeeeeeeeeeees 4 7 7 6 shelf TACK TEE 4 7 8 The Lablyo Mini as a standalone cold trap Operating Manual Freeze Drier Lablyo Mini and Accessories S RI iret el D 2 Applications TEE 3 Lablyo Mini technical data 4 Safety Instructons nens 1 4 1 Disconnect the mains plug sse UE e 1 4 3 Cleaning and Maintenance 1 4 4 Freezing skin to cold eurtarcesg AAA 1 4 5 Transport instructions ccccceeecceeeeeeeeeeeeeeeeeneeaeees Page 3 5 Using the Lablyo Mini sss 28 5 1 Switching the unit on NENNEN NEEN NN 28 5 2 Starting the defrost zue NEE HENN NENNSER tene e SEENEN REENEN me Rd xa Re 28 5 3 Temperature deplay eee ee eee eeeeee eee ceeeeeeeeeeeeeeeeeees 2
3. Frozen in Time a Manufacturers of Freeze Drying Machines and Vacuum Cold traps Operating Manual Lablyo Mini Main associated accessories Acrylic drying chamber FIT LYO 01 0 6 height shelf rack FIT LYO 03 0 6 heated shelf rack FIT LYO 19 0 4 shelf vial closing device FIT LYO 22 0 8 port flask manifold FIT LYO 13 0 48 port ampoule manifold FIT LYO 25 0 Spin Freezer FIT LYO 28 0 Vacuum pump FIT LYO 59 0 Includes IQ OQ Qualification Contents General Information 1 1 1 1 1 2 Information on Freeze Drying 2 1 General Information on Freeze Drying ssssssessesssresrrssrrrerrreenen 2 2 c r 2 3 Primary drvimg nennen 2 4 Secondary drying sse 2 5 End of PIOCOSS 2 aceti tinet ied enit AER desta aped 2 6 Delfrosting erine eege NEEN ent aha id d 3 Description of the Freeze Drying Processes 3 1 Freezing the product inicie nei cine nete det intense A 3 1 1 Freezing samples inside the ice condenser 3 1 2 Freezing in aneviernalIreezer 3 1 3 Freezing with a spin freezer esee 3 1 4 Flask freezing in a glycol freezer bath 3 2 Drying the product een eee c cre erdt ed dee ee LE E p 3 2 1 Drying on plain sbelves errereen 3 2 2 Drying on heated abeves 3 2 3 Drying in a vial closing device 3 2 4 Drying in a vial closing device with heated shelves 3 2 5 Drying with a drum column or lid manifold
4. It is advisable to pre cool the shelves in order to avoid partial thawing during the evacuation Products containing solvent high salt or sugar concentrations require freezing to lower temperatures 2 3 Primary drying The Lablyo Mini is taken to its operating temperature The vacuum pump is switched on The duration of the main drying phase depends mainly on the layer thickness of the product the solid content of the product the heat supplied to the product during the drying process the vacuum pressure inside the drying chamber during the drying process With increasing pressure the rate of sublimation rises as long as it stays below the vapour pressure of the product This is because at higher pressures the heat energy reaches the sublimation front of the ice core sooner Therefore the drying period is shortened The water vapor generated during the main drying phase is not intended to be removed by the vacuum pump It is to be collected by the ice condenser The purpose of the vacuum pump is to lower the partial pressure of the non condensable gases so that the water vapor can be transported from the product to the ice condenser However small quantities of water vapor will be removed by the vacuum pump The vacuum pump is equipped with a gas ballast valve that when open removes traces of condensable vapors from the pump For this reason the gas ballast valve can be open during the main primary phase The gas ballast valve
5. These shelves are ideal for product that requires slow drying with minimal heat input or small volume drying 3 2 1 Drying on heated shelves Vials bottles trays or dishes containing frozen product are arranged on the shelves and lowered into the acrylic chamber These shelves are ideal for product that requires faster drying or higher temperatures Each shelf is has equal heat input and there is a temperature sensor sampling one shelf only Product should be loaded equally over all the shelves to allow for even drying rates There are leadthroughs in the lid for the temperature sensor and power supply The Lablyo Mini requires a separate temperature controller 3 2 3 Drying in a closing device The closing devise is a series of shelves also for use inside an acrylic chamber Trays of frozen product are loaded onto it is then lowered into the chamber When the product is dry the lids on the vials can be closed sealing in either a vacuum or a nitrogen charge To do this the handle is turned clockwise to close levels 1 and 3 and then anticlockwise to close levels 2 and 4 3 2 4 Drying in a closing device with heated shelves This combines the closing device with the heated shelves in one unit For use when extra heat is required in closable vials Operating Manual Freeze Drier Lablyo Mini and Accessories 3 2 5 Freeze drying with a column or lid manifold These manifolds use rubber valves to attach the glass fr
6. sretupezeej yu TYNE BO TO 39vid WAO L 0 8 8 LVELO XV 8918 8 LPEL0 TAL i voz ovid nvWwO30 ON QNVION3 ZH9090A AHOA Page 34 D d e H o m voesosGooos 66sos eso 5o Sooooscoooo oo09900000 MM oooscssoss xowob0o90o 5o Sonaosaooon oo00900000 A oo Seege 9096509606 er um im 3o a5oodonoodn aoccocoono N oo See Se 9665550999 M o cocooooooos ooocooccoooo Os e MM Sooaococoooo oo00992000 m ae seseseeoess ot M m oo 00000000000 5o Socoocooooo 3o 5o o gre 9 1 y n o KE So o lt p dim WWOSE Hld3 83HAVHO 5 a o e lt i ge D S oO i S e a g o 8 S 3 in S 0 ar 4 Iz 2 S d CG SU a o 3 o N o Y y Es a Lr T a 3 KH Qu in S a be me LO O1110 ve18 2 Sv Lanod NI 4l D ON LWO ON 2900 E Oz n n m En En rm E z m 3r 8 z E Y z T C o E 9 IQ OQ Qualification This Qualification Protocol is solely intended to be used with Lablyo Mini freeze driers which are new or relocated It is written to assist the end user in validation of predetermined specifications The protocol begins with planning
7. Ampoule plates E L Section Gasket Vacuum Hose Ee Labo x S Vacuum pump www freezedriers com 9 e Lablyo Mini Drain valve FIT LYO 28 0 Spin Freeze with 1 x set carrier plates Includes L section gasket Additionally options Extra Spin Freeze plates FIT LYO 31 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 22 4 7 4 Heated shelves Acrylic lid with ss iL leadthroughs jj LU Section Gasket SS Heater shelves B i j Heater F E La 5 E control ZE ai par LT a V Section oo Ct RTT Le acuum Hose Lablyo NC n A I Mini E EE Vacuum pump S vn LU o d 9 o Www freezedrlors com i l e Lablyo Mini Drain valve Heated Shelves 6 shelves temperature controlled FIT LYO 19 0 Additionally requires Acrylic drying chamber FIT LYO 01 0 2 x LU section gaskets FIT LYO 40 0 FIT LYO 34 0 6 x Trays 230mm Page 23 Operating Manual Freeze Drier Lablyo Mini and Accessories 4 7 5 8 port column manifold Column manifold
8. Below are helpful hints to be included in the organization s Maintainance preventive maintenance plan 2a Vacuum Vacuum grease should be applied to rubber Y Grease components as required In general vacuum grease should be the first step in trouble shooting vacuum leaks Thin layers of grease are adequate for all seals Only use grease specially formulated for low vacuum service Is vacuum grease readily available and documented Type of grease used 2b Vacuum The vacuum pump oil should be changed as needed Y Pump Change oil that appears cloudy or discolored At a Oil minimum oil should be changed every 1000 hours of service Has there been a preventive maintenance plan established for the vacuum pump Type of oil to be used 3 Personnel Training 3a User Training Have personnel that will use the Lablyo Mini freeze Y Related to drier been adequately trained Equipment Are personnel familiar with All the buttons and displays on the front Collector capacity limits before defrosting Defrosting and draining methods Safe handling of solvents drained The use of vacuum grease Opening closing and venting sample valves Cleaning of the freeze dryer and neutralization of acids 3b User s Are the personnel who are to use or maintain Y Manual the Lablyo Mini able to locate the User s Manual for the machine Operating Manual Freeze Drier Lablyo Mini and Accessories 9 3 Summary Lablyo Mini freezedrier IQ
9. During the drying process the resistance increases The drying curve is determined by the latent heat of sublimation and the amount of vapour transported In order to increase the specific heat conduction properties of the product and to keep the water vapour volume as low as possible it is necessary that drying takes place as close as possible to the solidification point or eutectic point Primary Drying Secondary Drying 1004 o c el s c OO mE 9 N KR a 50 5 K g g 0 m 0 10 20 24 30 Time in Hours The drying time depends heavily on the vacuum level The nearer the vacuum to the solidification point in accordance with the vapor pressure curve the shorter the drying time Operating Manual Freeze Drier Lablyo Mini and Accessories Page 12 Facts regarding ice in a vacuum 1 0 gram of ice at 1 0 mbar assumes a volume of 1 m vapor 0 1 mbar assumes a volume of 10 m vapor 0 01 mbar assumes a volume of 100 m vapor Heat supply during drying The required heat supply to the product to be dried takes place by Conduction through contact in the drying chamber Mild conduction through low pressure vapour Radiant heat energy Affects of freeze drying of a product in a dish Radiant heat Radiant heat Vaporization Product bod 4d d d dod d Tray Ee Ets BIOS dE cun oe lt Front Goat heat ransion 7 Shelf Heat transfer takes place via the heated shel
10. OQ Document Equipment Location FreeZone Ser No Model No User Protocol Revision or Date published Contact print name Title Review the Response columns for answers of NO Use the area below to describe the deficiency or unacceptable results Those deficiencies are to be followed with an instruction for Corrective Actions Once acceptable results are obtained the deficiency is accepted by signing the Corrective Action Step Deficiency followed by Corrective Action Signature Operating Manual Freeze Drier Lablyo Mini and Accessories Page 39
11. behind the unit The freeze dryer should be positioned horizontally The ambient temperature should be between approx 5 C and 30 C The refrigeration compressor of the freeze dryer is air cooled Sufficient air circulation must be ensured A distance of at least 30cm to the wall should be kept The unit should not be positioned near radiators or heat sources In the case of insufficient air circulation or too high ambient temperatures the temperature and the pressure in the refrigerating system will increase If the maximum permissible operating pressure is exceeded this may cause the refrigeration unit to switch off 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 Frozen in Time freeze dryers are units of safety class The Lablyo Mini has a three wire connection cable with a 230VAC 13 amp fused plug earth contact The freeze dryer must be on a circuit protected with a 16 Amp fuse or circuit breaker 4 3 Air admittance Drain valve The drain valve is also used for air admittance If bottles have to be sealed in nitrogen the ice condenser chamber can be purged through the drain valve Take care not to over pressure the system 4 4 Condensate and defrosting water The condensate and the defrosting water are discharged through the drain valve 4 5 Vacuum pump exhaust gases The oil mist from the vacuum pump is normally trapped i
12. fittings to the customer s requirements Operating Manual Freeze Drier Lablyo Mini and Accessories Page 27 5 Using the Lablyo Mini 5 1 Switching on the unit Switch the Lablyo Mini on at the power switch on the rear of the unit The indicator light should now be on The refrigeration will be running 5 2 Defrost If a defrost is fitted The red illuminated switch on the side activates the defrost Defrost on the Lablyo Mini will override the refrigeration Defrost should only be switched on to defrost ice and it must then be switched off However the defrost heater is self regulating and will not over heat 5 3 Temperature display The temperature displays in C this measures the wall temperature of the condenser chamber 5 4 Drain valve The drain valve should be closed whenever the vacuum pump is activated It should not be opened while the vacuum pump is still switch on The drain valve is used to drain defrosted condensate from the condenser chamber It is also used to admit air or inert gases into the condenser chamber to break the vacuum Operating Manual Freeze Drier Lablyo Mini and Accessories Page 28 6 Accessories and part numbers FIT LYO 01 0 Acrylic drying chamber 300mm OD Additionally requires 2x U section gaskets FIT LYO 40 0 Required if using with the Lablyo Mini 6 shelf rack FIT LYO 03 0 Heated shelves FIT LYO 19 0 Lid manifold FIT LYO 6 0 Closing device FIT LYO 22 0 FIT LYO 03 0
13. heat energy is taken from the warmer surrounding air When drying takes place on shelves in an acrylic chamber the heat energy source is radiation from the environment and directly by from the shelves if they are heated Primary drying removes the most of the water from the product Secondary drying removes the last traces of water means of deep vacuum The main components of a freeze dryer are e Vacuum drying chamber or manifold a plain or heated shelves for drying in dishes b shelves with sealing device for drying in vials or small bottles c rubber valves for connecting round bottom flasks bottles etc d rubber nipples for connecting ampoules e Vacuum pump to evacuate air e ce condenser with a temperature of 55 C or 85 C to condense vapour Sublimation The principle of sublimation is briefly explained using the phase diagram of solid liquid and vapour If the pressure is higher than 6 1 mbar water passes through all three phases solid liquid vapour when the temperature is lowered or raised At 6 1 mbar and 0 C all three lines meet this is called the triple point where all three phase can occur simultaneously Below this point when the pressure is lower than 6 1 mbar the ice is converted directly from a solid to a vapour on reaching the sublimation pressure curve The sublimation curve shows the vapour pressure of water as affected by temperature and pressure Operating Manual Freeze Drier Lablyo Mini and Accesso
14. on a surface not to trap fingers Operating Manual Freeze Drier Lablyo Mini and Accessories Page 7 1 5 The Lablyo Mini should not be used when 1 It is not properly installed 2 The lid or accessories are not properly installed 3 Panels are missing 4 The operator is not authorized or trained 5 Highly corrosive or solvent substances are present 6 The accessories are not designed to be used with the unit or show signs of damage Glassware can be susceptible to implosion causing potential risk during freeze drying 7 In hazardous or dangerous locations 11 The products are explosive or highly flammable 12 The products are Infectious toxic pathogenic or radioactive unless in suitable vessels and in accordance with the relevant safety data Operating Manual Freeze Drier Lablyo Mini and Accessories Page 8 2 Information on Freeze Drying 2 1 General Information on Freeze Drying Freeze drying is the gentlest process for drying products It uses the process of sublimation the direct conversion from solid to gaseous state The frozen product is dried under vacuum without thawing The condenser chamber works as a cryogenic pump as it takes large quantities of vapour and condenses it to ice The vacuum pump is only intended to remove the air from the drying chamber but not the vapor In order to start the sublimation process energy must be supplied to the product When drying takes place in glass flasks on a manifold the
15. recommend removing it for refreezing It is advisable to defrost the condenser chamber at this point If the product is considered to be still usable then it can be placed back in the freeze drier and the process can be started again 7 2 Insufficient vacuum T 1 1 Easy initial checks Check that the drain valve is closed Remove the accessory and seal the top of the condenser chamber with a blank lid and a lightly greased L section gasket If the lid now seals it indicates that there is a leak in the accessory If the lid does not seal then the drain valve vacuum hose or vacuum pump is at fault Check that the vacuum pump is running and that there is suction If there is check that the hose push on connections between Lablyo Mini and vacuum pump are tight Make sure that the drain valve is not leaking by checking for suction when it is closed If the accessory is leaking examine every port and push on fitting Lightly grease any sealing parts and press down on chamber or manifold in order to assist the sealing gaskets 7 1 2 Checks to make using a vacuum sensor The following steps require that the there is no ice or water inside the condenser chamber Dry the chamber with a cloth To test the Lablyo Mini connected to the vacuum pump and put a blank lid and seal on the mouth of the chamber It will not achieve the same level of vacuum as a direct reading off the pump but it should probably be lower than 0 1 mbar The next thing to do wou
16. unit width 524 mm height 400 mm depth 515 mm Weight approx 48 kg Noise emissions according to DIN 45635 54 dB A Chamber Dimensions 200mm x 350mm Electromagnetic compatibility according class B to EN 55011 Refrigerant R507 0 65KG Voltage 240V 50Hz 220V 60Hz special order Main fuse rating 13 Amp Ambient temperature 5 C to 30 C Equipment connections Vacuum connection 19mm nozzle Drain valve 1 4 BSP ball valve Electrical connection IEC connection Operating Manual Freeze Drier Lablyo Mini and Accessories Page 6 1 4 Safety instructions 1 4 1 Disconnect the mains plug before removing panels The mains plug must be disconnected before the panels are removed or any maintenance work is undertaken 1 4 2 Solvents Acidic or high solvent concentration products should not be dried because of corrosion risk and damage to the vacuum pump 1 4 3 Cleaning and Maintenance of the Unit For infectious toxic pathogenic and radioactive substances the danger information of the associated safety regulations must be observed 1 4 4 Freezing of skin to surfaces Make sure skin does not come into contact with freezing surfaces Skin can only be detached from the surface by applying heat Do not use liquid 1 4 5 Transporting The Lablyo Mini should be carried by two people and care must be taken when placing the unit down
17. 6 shelf rack for acrylic chamber aluminum Additionally requires Acrylic drying chamber FIT LYO 01 0 2x LU section gaskets FIT LYO 40 0 FIT LYO 6 0 Lid manifold 8 port Additionally requires Acrylic drying chamber FIT LYO 01 0 2 x LU section gaskets FIT LYO 40 0 8 x Quick seal valves FIT LYO 43 0 FIT LYO 9 0 Cold trap lid with hose for solvent recovery or vacuum pump protection Additionally requires 1x LU section gaskets FIT LYO 40 0 FIT LYO 12 0 Lid for drying chamber plain 320mm diameter x 20mm thick Additionally requires Acrylic drying chamber FIT LYO 01 0 2 x LU section gaskets FIT LYO 40 0 FIT LYO 13 0 Column manifold 8 port Additionally requires 1x L section gaskets FIT LYO 40 0 8 x Quick seal valves FIT LYO 43 0 FIT LYO 16 0 Column manifold 16 port Additionally requires 1x LU section gaskets FIT LYO 40 0 16 x Quick seal valves FIT LYO 43 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 29 FIT LYO 19 0 Heated Shelves 6 shelves temperature controlled Additionally requires Acrylic drying chamber FIT LYO 01 0 2 x LU section gaskets FIT LYO 40 0 FIT LYO 22 0 Vial Closing Device Additionally requires Acrylic drying chamber FIT LYO 01 0 2 x LU section gaskets FIT LYO 40 0 FIT LYO 25 0 Lid with ampoule manifold 48 port Additionally requires 1x UL section gasket FIT LYO 40 0 FIT LYO 28 0 Spin Freeze with 1 x set carrier plates Additionally options 1 x Extra Sp
18. 8 5 4 EIERE 28 6 Accessories and part numbers eects 29 7 Troubleshooting FA Power TT 31 7 2 INSUFFICIENT vacu Missiaen iiaeia aieiai 31 7 3 Unit does not work 0 eee cee eeeeeeeceee cee eeeeeeeeesaeaaeaeecaeeeeeeeeeeeeeeeseseensacaeeeeeeeeees 33 7 4 Insufficient ice condenser Temperature 31 8 Maintenance 8 1 Ice condenser chamber 32 8 2 Heat exchange EE 32 8 3 R bb r EE 32 NET EE 32 8 5 EXMA UST EE 32 SENEGAL C 33 8 6 1 Cleaning the freeze dryer ssssssssssesseeessessssersssrrssrnsstrnsrnnernnernnnne 33 8 6 2 Cleaning the accessories ssssssssssseeeeen 33 8 6 3 Maintenance of the drain vahye 33 8 6 4 Disinfecting the drying chamber the lid and the accessories 33 8 7 Checks by the operator eene nnne nennen 33 8 8 Layout and Dimensions n emen 34 9 IQ OQ Qualification 9 1 Installation Oualhticaton enne 35 9 2 Operational Qualification sss enne 37 9 3 SUMMEANY Seed euo te eda uod gud Uni Mex Geesse desen 39 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 4 1 General Information 1 1 Introduction What is freeze drying lyophilisation Freeze drying means Removal of water from frozen material The drying process takes place by direct conversion from ice to vapour This process is called sublimation Sublimation happens under vacuum when the temperature in the product is less than 10 C The aim of freeze drying is to obtain a re
19. adily water soluble product which has the same characteristics as the original product after the addition of water As the drying process takes place in the frozen state at low temperatures it is possible to dry proteins which will not denature Most of the other chemical compounds will also remain unchanged Freeze drying products of biological origin such as tissues tissue extracts bacteria vaccines and sera transforms them into a dry product During this process enzymatic bacterial and chemical changes are largely avoided Freeze drying is the gentlest process for preserving the biological properties of sensitive tissue and tissue components Freeze drying can also be used for dry some inorganic products 1 2 Applications The Lablyo Mini is a laboratory and pre production machine for the freeze drying of products in ampoules vials glass flasks bottles or dishes The initial freezing of the products will require a spin freezer flask freezing bath laboratory freezer or in some cases the pre freezing of the products can be done in the Lablyo Mini chamber The appropriate accessories are required for freeze drying can be made with the use of the Operating Manual Freeze Drier Lablyo Mini and Accessories Page 5 Lablyo Mini 1 3 Technical data of freeze dryer Performance data 55 C Ice condenser capacity 3 kg max Ice condenser performance 2 kg per 24 hour maximum Physical data Dimensions of the
20. ber hose and clamps provided Vacuum Is the vacuum pump plugged into the rear of the freeze Y Pump dryer and the pump s power switch turned to the ON 2e Electrical position Vacuum The vacuum pump s ballast should remain closed Is Y Ballast the pump s ballast closed Electrical Plug the freeze dryer into a dedicated electrical outlet Y Connection Has the electrical service been verified to be adequate in size and voltage The ID plate on the rear of the freeze dryer has the electrical requirements 2e Electrical Has the ground on the electrical service been verified Y Grounding Operating Manual Freeze Drier Lablyo Mini and Accessories Page 36 9 2 Operational Qualification Step Description Specification or Acceptance Criteria Result 1 Freeze Drier 1a Refrigeration With the freeze dryer system at ambient temperature turn the Main Power Switch ON Does the refrigeration system start Record the time it started Y N Vacuum Pump Make sure all vacuum fittings and seals are in place Start the Vacuum Pump Record the time it started Refrigeration Effectiveness Does the condenser chamber temperature reach 47 C in less than 40 minutes With the system under vacuum and 21 C ambient temperature NOTE Freeze Dryers are tested to 55 C or in the factory Conditions may vary in the field resulting in warmer acceptance temperatures Verify Dis
21. e down Operating Manual Freeze Drier Lablyo Mini and Accessories Page 25 4 7 7 6 shelf rack Acrylic lid Acrylic Chamb 7 Section Gasket crylic Chamber Shelves LU Section Gasket Vacuum bl 0 Hose Mini Pius us eoi P Je Vacuum pump m 71 Er www freezedriers com Y FIT LYO 03 0 6 shelf rack for acrylic chamber aluminum Additionally requires Acrylic drying chamber FIT LYO 01 0 2x LU section gaskets FIT LYO 40 0 Lid for drying chamber FIT LYO 12 0 Additionally options Lid manifold 8 port FIT LYO 6 0 4 x Trays 220mm FIT LYO 34 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 26 4 7 8 The Lablyo Mini as a standalone cold trap INZ Cold Trap lid for solvent wenn CL Section Gasket Vacuum Hose o N o j bs Es Frozen in Time Lu SU www freezedriers com Le J Kc Lablyo Mini Drain valve FIT LYO 9 0 Cold trap lid with hose for solvent recovery or vacuum pump protection Additionally requires 1x LU section gaskets FIT LYO 40 0 Lid can be made to order with any
22. eeze drying flasks The flasks are frozen first and then can be added or removed from the manifold while the refrigeration and vacuum pump are running When adding a flask to a manifold that is under vacuum it is important to close the valves on the other flasks that are in use Open the valve to the newly introduced flask and after a few minutes the rest of the valves can be reopened 3 2 6 Freeze drying with a 48 port ampoule manifold The 48 port ampoule manifold requires that all 48 ports are used at once Ampoules from the spin freeze are a push on seal to the rubber nipples When the frozen the ampoules are attached then will freeze dry from the vacuum and the ambient heat Once the product is dry the ampoules can be removed and sealed The ampoules are usually hermetically sealed using a flame to melt the glass tube while it is being twisted 3 2 7 The Lablyo Mini as a standalone cold trap The Lablyo Mini can be equipped with an adaptor lid to act as a cold trap for vacuum pump protection It will trap water vapour or any other condensable that would contaminate the vacuum pump oil It can also be used for vacuum distillation so the condensable product can be collected Operating Manual Freeze Drier Lablyo Mini and Accessories Page 17 4 Installation and Commissioning of the Unit 4 1 Site of installation In order to ensure the air circulation of the heat exchanger do not place any paper cloths or similar items
23. evious drying processes deposit on it the freeze dryer may not achieve correct vacuum levels Therefore take care that no product or other residues will get into the valve 8 6 4 Disinfecting the drying chamber the lid and the accessories Check compatibility with the lid and the drying chamber The freeze dryers and the accessories are made of different materials A possible incompatibility must be considered For autoclaving the temperature stability of the individual materials must be taken into consideration Please consult us if in doubt If dangerous materials are used the freeze dryer and the accessories must be disinfected 8 7 Checks by the operator The operator has to ensure that the important parts of the freeze dryer that are necessary for Sea 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 PAT test must be carried out annually Operating Manual Freeze Drier Lablyo Mini and Accessories Page 33 i 8 v QONV8 3ONVHTTOL WW NI SNOISN3WIG NOLLDH JdIH3HS Med TVIHLSDONI QVOH 9HOA SUSUNLOVANNVW 3NIHOVIW NIAYA 323383 G11 AWIL NI N3ZOH4 IV 18S jnoKo1 um oK qo3 um og ava HO tii 3 1 Zi vO TI3NNOO d FO so o s3ovis wwo3a nomeu A NOlLdIMOS3Q ONIMVMO SEN Nya szo roi saovid 1VAI030 Z wio
24. he freeze dryer And have the means to be powered by a IEC connection An oil mist eliminator exhaust filter is recommended Accessories Freeze drying chambers or manifolds are not included with the freeze dryer Has an appropriate accessory been purchased to complete the required freeze drying process Y JIN N A Operating Manual Freeze Drier Lablyo Mini and Accessories Page 35 2 Prior to operation 2a Damage Have the delivered products been inspected fo any Y Claims signs of damage that may have occurred while in transit Keep packaging materials until inspection is complete WARNING Do not attempt to pull a vacuum ona freeze dryer with any damage to any of the accessories manifolds chambers etc Implosion and potential for injury can occur If damaged contact Frozen in Time 01347 878158 or the distributer from whom it was purchased 2b Handling Has the Safety Officer or equivalent reviewed the safe Y Solvents handling and disposal of solvents trapped as well as N A used vacuum pump oil 2c Manifold Place the desired drying chamber or manifold on to the Y Installation top of the Lablyo Mini condenser chamber flange N A Do you have the correct number and size of L section gaskets to make the vacuum seal 2d Vacuum Install the vacuum pump per the Users Manual Is the Y Pump pump attached to the vacuum port at the top of the Installation chamber with the correct rub
25. in Freeze plates FIT LYO 31 0 FIT LYO 34 0 Trays 230mm for vials or tray drying x1 Additional option for the 6 shelf rack FIT LYO 03 0 Heated shelves FIT LYO 19 0 Closing device FIT LYO 22 0 FIT LYO 37 0 Vacuum hose 1m for vacuum pump Additional option for the Vacuum Pump FIT LYO 59 0 FIT LYO 40 0 LU section gaskets for accessories Additional option for the Column manifold 8 port FIT LYO 13 0 Column manifold 16 port FIT LYO 16 0 Lid manifold 8 port FIT LYO 25 0 Acrylic drying chamber FIT LYO 01 0 Lid for drying chamber FIT LYO 12 0 FIT LYO 43 0 Quick seal valves Additional option for the Column manifold 8 port FIT LYO 13 0 Column manifold 16 port FIT LYO 16 0 Lid manifold 8 port FIT LYO 16 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 30 7 Troubleshooting 7 1 Power failure 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 the product was in when the power failure occurred If power returns within a few minutes then it is unlikely that any damage will have occurred It is important to distinguish between the primary drying phase and the secondary drying phase The product is in the secondary drying phase if the residual moisture has reached approximately 5 96 Below this value the product is generally not damaged by a power failure If the product is in the primary drying phase we
26. ir admittance The product is dry when it at or above ambient temperature while under the secondary drying vacuum level The condenser temperature will also be lower than when under load The vacuum pump can be switched off and the condenser chamber drain valve can be opened as an air admittance valve This valve can be used to purge the unit with nitrogen or another inert gas instead of using air Then the unit is switched off and the product is removed 2 6 Defrosting Defrosting of the ice condenser is carried out by switching off the refrigeration and switching on the red defrost button To let the water out the open the drain valve and allow to drain into an appropriate container The defrost is self regulating and will not overheat Operating Manual Freeze Drier Lablyo Mini and Accessories Page 14 3 Description of the Freeze Drying Processes 3 1 Freezing the product There are 4 ways to freeze the product when using the Lablyo Mini 1 The condenser chamber 2 A laboratory freezer preferably 40 C 3 The Spin freezer 4 Flask freezing in a glycol bath 3 1 1 Freezing inside the ice condenser chamber Possible water residue is removed from the ice condenser chamber To do this open the drain valve so that water residue can drain off Then the ice 2 conaenser chamber should be wiped out if necessary This i will minimize the risk of trays freezing to the chamber The refrigeration unit is then switch on and allowed to go down
27. is not required for secondary drying and closing it will help achieve a lower level of vacuum During primary drying the moisture is removed by sublimation and during final drying the bound moisture is removed by desorption The recommended vacuum pump should reach with open gas ballast valve a vacuum level lower than the relevant water vapour pressure Operating Manual Freeze Drier Lablyo Mini and Accessories Page 11 The residual moisture of the dried product depends mainly on The temperature of the dried product during the final drying process The final vacuum reached during the final drying process The end of the primary drying phase is reached when the product temperature is nearly the same as the shelf temperature temperature difference between shelf and product approximately 3 to 5 C Once the primary drying is completed the secondary drying will remove the bound water from the product The following diagram shows the drying process for a product containing approximately 10 96 solid matter During the first quarter of the primary drying phase 50 of the water content is condensed During the next quarter of the primary drying phase 5096 of the remaining water content is condensed This continues until the drying curve approaches the time axis asymptotically This typical drying curve is due to the fact that the area of sublimation recedes into the product and the remaining water vapour must pass through the already dried layers
28. ld be to fit the accessory if it is a manifold with rubber valves then these should all be closed If it is a 48 port manifold then all 48 ports need to blanked off or fit with ampoules All accessories with acrylic chambers need to be assembled complete To check the vacuum pump directly it is necessary to use a separate vacuum sensor Make sure that the vacuum pump is warm and there should be a vacuum reading of 0 04 mbar or less 7 3 Unit does not work If the indicator light does not work and the refrigeration system is not running after the mains switch has been activated the following tests must be performed Check that the Lablyo Mini is plugged in Check the breakers or fuses for the circuit Check the plug fuse 7 4 Insufficient ice condenser temperature The refrigeration will stop if the ambient temperature is too high or the airflow is restricted to the heat exchanger Once the permissible operating conditions are reached again the refrigeration unit is switched on automatically via the motor protection switch or via the pressure switch The minimum ice condenser temperature of approximately 55 C or 85 C is reached when the ice condenser is not under load Sufficient air circulation is very important Do not place any objects behind the unit Operating Manual Freeze Drier Lablyo Mini and Accessories Page 31 8 Maintenance 8 1 lce condenser chamber Before each start up ensure that all water residues have been re
29. moved 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 8 2 Heat exchanger The refrigeration heat exchanger is used to cool the refrigerant compressed by the refrigeration unit The heat exchanger is located at the back of the unit and should be checked for dust or dirt residues every few months It must be cleaned whenever necessary The heat exchanger can be cleaned best by brushing by using a vacuum cleaner from the outside or by using compressed air from inside of the unit Excessive build up on the heat exchanger leads to a decrease in performance and may cause a failure of the unit 8 3 Rubber valves and seals Special attention must be paid to the rubber valves If the valves are stiff they must be dismantled cleaned slightly greased with vacuum grease and reassembled 8 4 Vacuum pump For the maintenance of the vacuum pump please refer to the separate operating manual Additionally we would like to emphasize the following points The oil level of the vacuum pump must be regularly checked at the sight glass in case of continuous operation at least once a day Top up oil to the required level via the oil inlet Due to possible operation with gas ballast oil consumption cannot be avoided For topping up see the operating manual of the pump The oil change should always be carried out with warm pump 8 5 Exhaust fil
30. n an exhaust filter If this is not the case the oil mist has to be discharged A hose can be connected to the exhaust flange of the vacuum that leads into the open air or a vent During installation of the pipe special care must be taken that condensate cannot flow back into the pump Operating Manual Freeze Drier Lablyo Mini and Accessories Page 18 4 6 Initial start up Prior to start up make sure that the freeze dryer has been properly set up and installed Vacuum pump E oo o C Acrylic lid e Acwlieich T b 7 Section Gasket crylic Chamber Shelves L Section Gasket Vacuum b lyo Hose Mini Frozen in Time ua lt gt M N e www freezedriers com Installation of the vacuum pump The vacuum pump can be powered through the Lablyo Mini via the IEC socket on the left hand side Make sure that the vacuum exhaust gases are filtered or carried off Operating Manual Freeze Drier Lablyo Mini and Accessories Page 19 4 7 Installation of accessories 4 7 1 Vial closing device _7 Operating handle YX Sep N P ef r
31. played Temperature The temperature indicated on the LCD display is measured on the collector coil There is a mobile probe that hangs free inside as well The values were calibrated at the factory by correlating its reading with that of a reference gauge attached to a sensors Does the display correlate to the reference Gauge 20C Ref Instrument If the temperature does not correlate contact Frozen in Time 01347 878158 N A Vacuum Leaks Verify that the system is leak free by continuously running the vacuum pump with the refrigeration system ON The rate the freeze dryer without samples achieves a low level of vacuum less than 13 Pa it is dependent upon many factors Inside volume amp surface area of the system Cleanliness or cleaners used on interior Condition amp size of the vacuum pump Period of time the parts have been exposed to environmental conditions Based on the freeze dryer s displayed vacuum level the freeze dryer should reach its lowest level in less than 18 hours If not refer to Vacuum Troubleshooting Guide in the User s Manual Does the system reach a displayed vacuum level of less than 6Pa in 18 hours Defrost With the refrigeration switched OFF press the defrost button ON Does the condenser chamber become warm to the touch N A Operating Manual Freeze Drier Lablyo Mini and Accessories Page 37 2 Routine
32. r LC Section Gasket Acrylic Chamber m T nennnnrinnnnn Qlosing device Vials 1 JnnmnnnHbnnnnn mnnnnnnhnnnnn NI li Vial Trays nnnnnnnhnnnnn L Section Gasket z Vacuum Hose L ab yo S a A Frozen in Time Lu oooo 00000000000000000 Vacuum pump Bf o oo www freezedriers com e 0000000000000 Lablyo Mini Drain valve FIT LYO 22 0 Vial Closing Device Additionally requires Acrylic drying chamber 2 x VU section gaskets 4 x Trays 230mm FIT LYO 01 0 FIT LYO 40 0 FIT LYO 34 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 20 4 7 2 48 port ampoule manifold Ampoules 48 port manifold Ki Push on ampoules nipples LU Section Gasket 4 L Section Gasket Labo v Mint Frozen in Time Ltd 00000000000 Vacuum Hose 00000000000000000 00000000000000000 00000000000 www freezedriers com i SC i Lablyo Mini Drain valve FIT LYO 25 0 Lid with ampoule manifold 48 port Additionally requires 1x LU section gasket FIT LYO 40 0 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 21 4 7 3 Spin freezer _ Acrylic chamber _ Ampoules Motor controler _
33. ries Page 9 Phase diagram for solid liquid and vapour 1000 LIQUID 100 10 zs A E g Su n an VAPOUR 0 001 0 0001 0 00001 100 80 C 60 C 40 C 20 C 0c 20 C 40 C 60 C 80 C 100 C 0 C 10 C Frozen in Time Ltd 20 C 30 C N Sublimation Curve 40 C 50 C 60 C g g 70 o Qa 5 80 C He 90 C 100 C 865 4 3 2 1865 4 3 2 1865 4 3 2 1865 4 3 2 1865 4 3 2 1i 10 0 1 0 0 1 0 01 0 001 Pressure mbar Operating Manual Freeze Drier Lablyo Mini and Accessories Page 10 2 2 Freezing Small product quantities can be frozen directly inside the ice condenser chamber of the Lablyo Mini Larger quantities are pre frozen in a deepfreeze This the usual option for product to be freeze dried in trays or vials Deep fill depths should be avoided by using wider containers filled to a shallower depth in order to maximize surface area Liquids to be dried in narrow ampoules should be frozen in a spin freezer this causes the product to freeze in a thin section up the wall of the tube Liquid to be dried in flasks should be rotated in a freezer bath This causes the frozen material to form a thin layer lining the flask These procedures will help minimize the drying time
34. ter 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 Operating Manual Freeze Drier Lablyo Mini and Accessories Page 32 8 6 Cleaning 8 6 1 Cleaning the freeze dryer Use soapy water or other water soluble mild cleaning agents to clean the freeze dryer Avoid corrosive and aggressive substances Do not use alkaline solutions or solvents or agents with abrasive particles Remove product residues from the ice condenser chamber using a cloth It is recommended to open the lid of the condenser chamber when the freeze dryer is not in use so that moisture can evaporate If there is the risk of toxic radioactive or pathogenic contamination special safety measures must be considered and adhered to 8 6 2 Cleaning the accessories When cleaning accessories special safety measures must be taken as these are measures to ensure operational safety and reliability Cleaning of accessories should be carried away from the freeze dryer once a week or preferably after every use Aluminium accessories are particularly prone to corrosion If there is the risk of toxic radioactive or pathogenic contamination special safety measures must be considered and adhered to 8 6 3 Maintenance of the air admittance drain valve Special attention must be paid to the air admittance drain valve If residues from pr
35. the site for the piece of equipment and therefore is of value prior to receipt of delivery The use of this document does not replace the need for the Lablyo Mini User s Manual and is in this case attached Information within the User s Manual is required to complete this IQ OQ Protocol If the manual has been misplaced copies can be obtained from the manufacturer or down loaded from their website www freezedriers com 9 1 Installation Qualification Description Specification or Acceptance Criteria Result Step 1 Site Planning 1a Space Requirements Refer to 1 3 Technical data of freeze dryer Check in the User s Manual for dimensions of the model you have chosen Has adequate floor or counter space been provided for placement of the equipment A minimum of 100mm is required between the back of a freeze dryer and the wall and between the sides and the walls for proper airflow through the refrigeration system Electrical Service Refer to the User s Manual for electrical requirements Are services available for the equipment to be connected to an electrical circuit of adequate size and the proper voltage Vacuum Pump Refer to the User s Manual Have accommodations been made to provide a suitable vacuum pump It must be capable of at least 100 Liters min With an inlet fitting suitable for a 34 inch ID vacuum hose on one end and a KF25 on the other It must have the same voltage rating as t
36. to operating temperature The trays can then be lowered into the condenser chamber to freeze With vials several layers of trays can be stacked into the chamber at once A blank lid can be placed on the top of the chamber to keep warm air and moisture from entering while the product is freezing The same principle can be used for tray drying although more care is needed when stacking the trays 3 1 2 Freezing in an external freezer The product is prepared in vials or trays and then placed in a 40 C freezer until it is completely frozen 3 1 3 The Spin freezer The spin freezer prevents foaming when vacuum freezing is used It does this by using centrifugal force The long thin ampoules sit at an angle with the tops facing in slightly towards the centre The vials are left to spin on d an adjustable timer while the vacuum is applied The centrifugal force will stop the product from overflowing and a long thin tapered layer will freeze up the side of the slanting ampoule maximizing the surface area 3 1 4 Flask freezing in a glycol bath The flasks should only be partly filled then rotated in the freezing glycol so a thin layer freezes evenly around the inside of the flask to maximize the surface area Operating Manual Freeze Drier Lablyo Mini and Accessories Page 15 3 2 1 Drying on plain shelves Vials bottles trays or dishes containing frozen product are arranged on the shelves and lowered into the acrylic chamber
37. ves by direct contact with the bottom of the tray At the beginning of sublimation the transfer of heat is very effective from the wall of the tray to the frozen product However soon an area develops which is ice free porous dried and has an insulating effect between the wall of the tray and the product This slows down the heat energy transfer available to the ice core The porous dried layer enables the passage of vapour from the ice core If it is restricted the temperature will increase and ice core will thaw rather than sublimate This applies especially to inhomogeneous products and to great layer thicknesses During this drying phase it is important to regulate the heat supply and control temperature and pressure precisely Operating Manual Freeze Drier Lablyo Mini and Accessories Page 13 2 4 Secondary drying The final pressure in the drying chamber depends on the ice condenser temperature according to the vapor 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 01 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 12 mbar The final pressure measured when there is no product in the unit and its corresponding ice temperature is determined by the warmest ice surface in the condenser chamber 2 5 End of drying and a
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