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8 | Operating top-mount drying racks

Büchi Labortechnik AG

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Operation Manual Lyovapor™ L-300/L-300 Pro

8.7

Determining the number of flasks

NOTE

Do not overfill flasks

Maximum volume of the samples ≤ half of the flask volume

NOTE

The number of flasks used should be determined individually for every process.

The number of flasks used is dependent on the following factors:

The volume of the flask

The method of freezing

The concentration of the sample

The composition of the solvent

Number of flasks using water as an example

Flask volume 1000 mL

Flask volume 500 mL

Rotating freezing

Max. 22 flasks

Static freezing

Max. 36 flasks

8.8

Operating manifold valves

The lever on a manifold valve can be set to the following positions:

Position

Function

A: Lever pointing up

The connected vessel is evacuated.

B: Lever pointing down The connected vessel is vented.

Содержание Lyovapor L-300

Страница 1: ...Lyovapor L 300 L 300 Pro Operation Manual 1153869 D en...

Страница 2: ...ves the right to make changes to the manual as deemed necessary in the light of experience especially with respect to structure illustrations and technical details This manual is copyrighted Informati...

Страница 3: ...isks 12 2 5 1 Faults during operation 12 2 5 2 Glass and acrylic breakage 12 2 5 3 Low internal pressure 12 2 5 4 Cold and hot surfaces 12 2 6 Personal protective equipment 12 2 7 Modifications 13 3 P...

Страница 4: ...2 10 Fitting an air filter option 34 5 3 Commissioning the vacuum pump 35 5 4 Establishing LAN connection 35 5 4 1 Requirements for local network settings 35 5 4 2 Preparing the instrument for app us...

Страница 5: ...method Pro control panel 74 7 9 1 Preparing the instrument 74 7 9 2 Selecting a method 74 7 9 3 Starting freeze drying 75 7 9 4 Changing parameters while the process is running 76 7 9 5 Ending freeze...

Страница 6: ...Cleaning the ice condenser 103 10 Help with faults 104 10 1 Troubleshooting 104 10 2 Faults possible causes and remedies 104 10 3 Locating leaking manifold valve 105 10 4 Manually defrosting ice cond...

Страница 7: ...operating instructions follow the instructions and specifications in the documentation for the connected devices 1 2 Warning notices in this document Warning notices warn you of dangers that can occur...

Страница 8: ...that must be carried out by the user This character indicates the result of a correctly carried out instruction Mark up Explanation Window Software Windows are marked up like this Tab Tabs are marked...

Страница 9: ...the instrument for processing substances outside of research and development Production and processing of substances that can lead to spontaneous reactions such as explosives metal hydrides or solven...

Страница 10: ...us working practices Safety related incidents that occur while using the instrument should be reported to the manufacturer quality buchi com BUCHI service technicians Service technicians authorized by...

Страница 11: ...2 Location of warning signs on the product General warning Dangerous electrical voltage Flammable substances Keep at least 40 cm clearance to pre vent overheating 2 4 3 Location of warning signs on th...

Страница 12: ...ully and do not drop them u Always place the flasks in a suitable holder when they are not mounted on the Lyovapor u Always visually inspect glass and acrylic components for damage every time they are...

Страница 13: ...t safety and lead to accidents u Use only genuine BUCHI accessories spare parts and consumables u Carry out technical changes only with prior written approval from BUCHI u Only allow changes to be mad...

Страница 14: ...end product The following top mount drying racks can be used Non heatable and heatable shelves in rack Trays in rack Top mount rack with manifold valves 3 1 1 Freezing phase In the freezing phase the...

Страница 15: ...below the collapse temperature for amorphous materials in the sample Sublimation of the ice crystals progresses downwards from the surface of the product Above the sublimation boundary the product is...

Страница 16: ...L 300 L 300 Pro 6 5 8 9 4 3 2 1 7 Fig 4 Front View 1 Connections for heated shelf Lyovapor L 300 Pro only 2 Intermediate valve 3 Ice condenser 4 Optional mounting position for con trol panel 5 Ventil...

Страница 17: ...specifications 3 Connections for pressure sensors option 4 Side connections 5 Connection for fresh water 6 Connection for condensate drain hose I 7 Connection for condensate drain hose II 8 Ventilati...

Страница 18: ...Chapter 3 6 Technical data page 21 2 1 8 7 6 3 4 5 Fig 6 Side connections 1 Connection for pressure sensor option 2 Connection for pressure sensor option 3 Automatic stoppering connection 4 Connection...

Страница 19: ...4 Control panel 1 2 3 Fig 7 Control panel 1 View 2 Function buttons 3 Navigation control 3 2 5 Pro control panel 1 2 Fig 8 Pro control panel 1 Touch screen display 2 Navigation control 3 3 Type plate...

Страница 20: ...6 Power consumption maximum 7 Year of manufacture 8 Product code 9 Approvals 10 Symbol for Do not dispose of as household waste 3 4 Scope of delivery NOTE The scope of delivery depends of the configu...

Страница 21: ...he back of the instrument L xxx xxHz HT Cooling System Refrigerant Rxxx Filling xxx g Global Warming Potential GWP xx tCO2 High Side Design Pressure xxxx Low Side Design Pressure xxxx 5 3 1 2 4 6 Fig...

Страница 22: ...12 kg 24 h Lowest condenser temperature without samples 105 C 105 C Temperature divergence 3 0 C 3 0 C Condenser capacity Unlimited 2 x 1 kg Unlimited 2 x 1 kg Condenser surface area 2 x 1280 cm2 2 x...

Страница 23: ...onditions For indoor use only Max altitude above sea level 2000 m Ambient temperature 15 30 C Maximum relative humidity 80 for temperatures up to 30 C Storage temperature max 45 C 3 6 3 Materials NOTI...

Страница 24: ...al Lyovapor L 300 L 300 Pro Component Materials of construction Condensate drain valve Steel 1 4301 304 with EPDM sealings Sili con drain tubing Venting valve Brass with FKM seal Regulating valve EN 1...

Страница 25: ...whenever possible Avoid sharp movements during transit u After transporting check the instrument and all glass components for damage u Damage that has occurred in transit should be reported to the ca...

Страница 26: ...compressor Firm level surface Minimum space requirements 810 mm x 1000 mm x 1000 mm W x D x H Take into account the maximum product dimensions and weight Take into account the 1100 mm operating height...

Страница 27: ...the refrigerant compressor requires ten minutes to return to the collection tank 5 2 1 Preparing the instrument u Clean the instrument with a damp cloth before commissioning u Check all sealing surfa...

Страница 28: ...sert the power plug into the power socket 5 2 3 Fitting the fresh water connections NOTICE Risk of instrument damage from scale formation u Use distilled water u Do not connect to mains water supply N...

Страница 29: ...Fitting fill level sensor in water tank optional page 29 5 2 4 Fitting fill level sensor in water tank optional Fig 14 Fitting the fresh water level sensor u Switch the On Off master switch to Off u F...

Страница 30: ...ate drain tube u Switch the On Off master switch to Off u Fit the drain tube 4 onto the connection marked Drain 1 5 u Fix the drain tube in place with a hose clip u Fit another drain tube onto the con...

Страница 31: ...et tube Precondition R The coolant connection complies with the specified parameters See Chapter 3 6 Technical data page 21 u Make sure that the instrument is not connected to the power supply u Fit t...

Страница 32: ...sensor connection 6 and fix with the clamp 3 u Plug the connecting lead connection into the socket 10 on the pressure sensor 1 u Plug the connecting lead connection into the socket marked Vacuum Sens...

Страница 33: ...nnection complies with the specified parameters See Chapter 3 6 Technical data page 21 u Switch the On Off master switch to Off u Fit the inert gas tube 1 onto the gas connection for the pressure regu...

Страница 34: ...meters See Chapter 3 6 Technical data page 21 u Switch the On Off master switch to Off u Fit the tube 3 onto the gas connection for the pressure regulating valve 5 u Fix the tube 3 with the tube clip...

Страница 35: ...open gas ballast valve NOTE Prepare the vacuum pump according to the manufacturer s instructions See relevant documentation 1 2 Fig 21 Connections for vacuum pump 1 Vacuum pump power connection 2 Vac...

Страница 36: ...he LAN cable while the unit is connected to the BUCHI Cloud Services u Connect the unit to the LAN local area network u Restart the unit Navigation path Settings Network u Navigate to Network u Activa...

Страница 37: ...on the underside u Switch on the instrument The status bar shows the SD card symbol The following data is stored on the SD card Numbering Date Time Set pressure Current pressure in the ice condenser...

Страница 38: ...s are proceeded for several days 6 1 Layout of the control panel 4 3 2 1 6 5 Fig 22 Layout of the control panel No Description Function 1 Status bar Shows the current status of the instrument 2 Menu b...

Страница 39: ...OK Confirm Confirms an entry EDIT Edit Allows the selected item to be edited MENU Menu Allows selection of a menu from the menu bar using the navigation con trol SAVE Save Saves the setting Process c...

Страница 40: ...bar The control panel highlights the selected parameter in black u To increase or decrease the figure turn the navigation control clockwise or anti clockwise u Tap the function Save on the function b...

Страница 41: ...Explanation Mobile connection password View The control panel shows a password for entry in the BUCHI Monitor app Mobile connection QR code View The control unit shows a QR code for reading by the BU...

Страница 42: ...illumination level in 0 100 Network Enter value The following parameters can be edited Device name MAC address DHCP System IP address Subnet mask Gateway DNS server BUCHI Cloud Server IP address Dele...

Страница 43: ...e condenser 2 Expansion valve 1 Expansion valve 2 Bypass valve Safety switch for low pressure low temp Safety switch for high pressure low temp Intermediate heat exchanger temperature Safety switch fo...

Страница 44: ...essure ice condenser 1 Pressure ice condenser 2 Main valve 1 Main valve 2 Vacuum Pump Venting valve 1 Venting valve 2 Regulating valve 1 Vacuum regulation 1 Vacuum regulation 2 Regulating valve 2 Vacu...

Страница 45: ...over temperature Steam generator water level OK Water tank fill level low Waste tank full Water pump Stoppering System View The following information on the stoppering system is available Number of u...

Страница 46: ...istory The following message types are possible I Information No immediate actions by customer are needed W Warning Minor failures during operation Customer action is required E Error Major failures d...

Страница 47: ...hows the remaining time Defrosting The instrument is defrosting The status bar shows the remaining time Standby Shutting down is completed Conditioning The instrument is starting up including starting...

Страница 48: ...te Attach the sample The ice condenser is yellow The ice condenser is preparing for switch over Sample attachment is possible as long p and T settings are stable The ice condenser is red The ice conde...

Страница 49: ...ying racks page 81 u Load the top mount drying rack with frozen samples u Navigate to the Start menu via the navigation path u Enter the required settings for the process parameters u Tap the function...

Страница 50: ...ting down the instrument can damage the instrument u Shut down the instrument completely u If the shutdown was interrupted tap the function Defrost on the function bar NOTICE Do not use force to remov...

Страница 51: ...rol panel 6 Operation Manual Lyovapor L 300 L 300 Pro 51 118 6 5 6 Switching off the instrument Precondition R The instrument has been shut down See Chapter 6 5 5 Shutting down the instrument page 50...

Страница 52: ...proceeded for several days 7 1 Layout of Pro control panel 5 4 3 2 1 Fig 23 Layout of Pro control panel No Description Function 1 Status bar Shows the current status of the instrument 2 Menu bar Show...

Страница 53: ...he navigation con trol SAVE Save Saves the setting Process control function buttons Symbol Description Meaning Defrost Defrosts the ice condenser AERATE Aerate Vents the system OFF Shut down The instr...

Страница 54: ...the menu bar Navigation through the menus is by the input controls The following menus are available Menu symbol Meaning Submenu Action Start menu Process control parameters Favourites menu Bookmarks...

Страница 55: ...ites menu The Favourites menu allows you to define submenus and actions as favourites Adding a favourite u Navigate to a submenu or action u Tap the function Add to favourites on the function bar The...

Страница 56: ...the control panel The following languages are avail able English German French Italian Spanish Russian Portuguese Japa nese Chinese Indonesian Korean Temperature unit Choice of unit for indica tion of...

Страница 57: ...nal connections to the instrument Submenu End point determination Action Option Explanation Pressure rise test View Shows the current settings for the pressure rise test Pressure difference test View...

Страница 58: ...e condenser 2 Expansion valve 1 Expansion valve 2 Bypass valve Safety switch for low pressure low temp Safety switch for high pressure low temp Intermediate heat exchanger temperature Safety switch fo...

Страница 59: ...essure ice condenser 1 Pressure ice condenser 2 Main valve 1 Main valve 2 Vacuum Pump Venting valve 1 Venting valve 2 Regulating valve 1 Vacuum regulation 1 Vacuum regulation 2 Regulating valve 2 Vacu...

Страница 60: ...l OK Water tank fill level low Waste tank full Water pump Stoppering System View The following information on the stoppering system is available Number of uses Start Up Down Oil pressure Drying shelve...

Страница 61: ...istory The following message types are possible I Information No immediate actions by customer are needed W Warning Minor failures during operation Customer action is required E Error Major failures d...

Страница 62: ...s bar shows the remaining time Standby Shutting down is completed Conditioning The instrument is starting up including starting re frigerant compressors and vacuum pump Reconditioning The instrument i...

Страница 63: ...oud P Sample protection is active Reason the pressure is outside the pressure lim its T Sample protection is active Reason the temperature is outside the safe tem perature range PT Sample protection i...

Страница 64: ...are two possible ways of creating a new method Creating a new method Navigation path Method u Navigate to the Method menu via the navigation path u Tap the function New on the function bar The new met...

Страница 65: ...Sample collapse temperature The control panel shows a dialog box with a numeric input box u Enter the value in the numeric input box u Tap the function Save on the function bar The setting is saved T...

Страница 66: ...ettings for the action Steps affect a single step in each case Navigation path Method u Navigate to the Method menu via the navigation path u Tap the name of the method that you wish to edit The contr...

Страница 67: ...as required u Tap the function Save on the function bar The setting is changed Add step u Use the function Right or Left on the function bar to navigate to the position at which you wish to add a step...

Страница 68: ...on function is ac tivated Safety temp time Enter value Time as of which sample protection in inactive The value relates to the time before completion of primary drying End point defi nition More setti...

Страница 69: ...fies a temperature for the dry ing shelves Editing the settings for a phase u Tap the phase that you wish to edit The control panel highlights the selected phase in green u Tap the setting that you wi...

Страница 70: ...hapter 5 2 8 Fitting pressure sensors option page 31 R A Pirani pressure sensor Inficon PSG55x is connected to the connection Vacuum Sensor 2 See Chapter 5 2 8 Fitting pressure sensors option page 31...

Страница 71: ...l drying shelves are below the threshold The samples on a drying shelf have different drying times Take account of the different drying times in the Duration setting The temperature difference test es...

Страница 72: ...difference between the two sensor readings below which the end point is reached Term Enter value The period of time during which the difference is not to be ex ceeded If the threshold is not exceeded...

Страница 73: ...est is to be carried out Start time Enter value Sets the time from which the pressure difference test is to be performed The value relates to the time before completion of the primary drying phase or...

Страница 74: ...oning Time re quired approx 30min Navigation path Start Precondition R All commissioning operations have been completed See Chapter 5 2 Putting the instrument in operation page 27 u Navigate to the St...

Страница 75: ...mount drying rack with frozen samples u Navigate to the Start menu via the navigation path u Tap the function Start on the function bar u Make sure that the specified gas is being used u Answer YES t...

Страница 76: ...bar shows the status Aerating u Wait until the status bar shows the status Unload Load u Remove the dried preparation from the top mount drying rack 7 9 6 Shutting down the instrument NOTICE Not compl...

Страница 77: ...trument NOTICE Several conditioning of instrument in a day is damaging for cooling circuit If it is necessary wait 2 hours between each conditioning Time re quired approx 30min Navigation path Start P...

Страница 78: ...The instrument is shutting down The aeration valve and the drain valve are closed The status bar shows the remaining time 7 10 3 Editing parameters while the process is running Navigation path Start P...

Страница 79: ...line shows whether the pressure rise test has been passed or not 7 10 5 Ending freeze drying Navigation path Start Precondition R The sample is dry u Navigate to the Start menu via the navigation pat...

Страница 80: ...a the navigation path u Tap the function Shut down on the function bar The instrument is shutting down The status bar shows the remaining time and the status Shutting down After the instrument has shu...

Страница 81: ...ice condenser is clean free of dust and not scratched u Check the O ring for damage u Place the O ring into the groove on the ice condenser u Place the main plate on the ice condenser u Make sure that...

Страница 82: ...bortechnik AG 82 118 Operation Manual Lyovapor L 300 L 300 Pro u Place the intermediate plate on the main plate u Loosen all fixing screws u Align the slots for the shelves u Tighten the fixing screws...

Страница 83: ...temperature sensor electrical connector so that the marks on the connector and the heatable shelf are parallel u Press the temperature sensor electrical connector onto the connection u Locate the cyl...

Страница 84: ...s the status Stoppering u Turn the hand wheel until all samples are sealed u Confirm the verification question on the control panel 8 2 Operating manifold acrylic drying chamber heatable shelves u Mak...

Страница 85: ...that the groove on the ice condenser is clean free of dust and not scratched u Check the 300 mm dia O ring for damage u Place the 300mm dia O ring in the groove in the main plate u Place the intermed...

Страница 86: ...into the rack u Press the plug onto the shelf connection and turn the ring counterclockwise at the same time option u Turn the temperature sensor electrical connector so that the marks on the connect...

Страница 87: ...the O ring for damage u Place the O ring into the groove of the cover u Place the manifold cover on the cylinder u Carry out freeze drying 8 3 Operating manifold acrylic drying chamber non heatable s...

Страница 88: ...e main plate on the ice condenser u Make sure that the groove on the ice condenser is clean free of dust and not scratched u Check the 300 mm dia O ring for damage u Place the 300mm dia O ring in the...

Страница 89: ...300 Pro 89 118 u Locate the cylinder in the groove above the main plate u Fit manifold valve onto the connection on the top mount drying rack u Check the O ring for damage u Place the O ring into the...

Страница 90: ...of dust and not scratched u Check the O ring for damage u Place the O ring into the groove on the ice condenser u Place the main plate on the ice condenser u Make sure that the groove on the ice cond...

Страница 91: ...ual Lyovapor L 300 L 300 Pro 91 118 u Align the slots for the shelves u Tighten the fixing screws u Place the rack on the intermediate plate u Slide the shelves into the rack u Press the plug onto the...

Страница 92: ...o the connection u Locate the cylinder in the groove above the main plate u Check the O ring for damage u Place the O ring into the groove of the cover u Place the cover on the cylinder u Carry out fr...

Страница 93: ...the groove on the ice condenser is clean free of dust and not scratched u Check the 300 mm dia O ring for damage u Place the 300mm dia O ring in the groove in the main plate u Place the intermediate p...

Страница 94: ...6 Operating manifold drying rack u Make sure that the groove above the ice condenser is clean free of dust and not scratched u Check the O ring for damage u Place the O ring into the groove on the ice...

Страница 95: ...Lyovapor L 300 L 300 Pro 95 118 u Fit manifold valve onto the connection on the top mount drying rack u Place the base plate on the main plate u Place the seal on the connection u Fit the manifold dry...

Страница 96: ...ent on the following factors The volume of the flask The method of freezing The concentration of the sample The composition of the solvent Number of flasks using water as an example Flask volume 1000...

Страница 97: ...a mild detergent Daily O ring dia 300 mm u Wipe down the 300 mm O rings with a damp cloth u Check for scratches and other damage u Replace the 300 mm O ring if it is damaged Daily u Replace the 300 m...

Страница 98: ...he vacuum system Time re quired max 10 min Navigation path Configuration Servicing Vacuum test Precondition R Conditioning of the instrument has been completed R A top mount drying rack is fitted R Th...

Страница 99: ...rforming a leak test 9 3 1 Performing a leak test with a drying chamber The leak test checks the vacuum system for possible leaks Time re quired 45 min NOTE The leak test can be aborted by tapping Sto...

Страница 100: ...4L 47 2L Acrylic drying chamber with 4 drying shelves 54 1L Acrylic drying chamber with 6 drying shelves Both ice condensers 1 2 1 2 1 2 33 5L 56 3L Acrylic drying chamber with 4 drying shelves 63 2L...

Страница 101: ...chamber only Replace leaking manifold valve Locate leaking manifold valve See Chap ter 10 3 Locating leaking manifold valve page 105 9 3 2 Performing leak test with a manifold drying rack The leak te...

Страница 102: ...ng rack installed Troubleshooting after failed leak test Possible cause Action Top mount drying rack not correctly fit ted Fit the top mount drying rack correctly O rings dirty Wipe down the O ring wi...

Страница 103: ...hapter 5 2 5 Fitting the drain tubes page 29 u Pour approx 5 L of warm water into the ice condenser through the open intermediate valve u Leave it to take effect for five minutes u Navigate to the Def...

Страница 104: ...pter 10 4 Manually defrosting ice condenser page 105 u Fill up fresh water 10 2 Faults possible causes and remedies Malfunction Possible cause Remedy Instrument does not work Instrument is not connect...

Страница 105: ...art view via the navigation path u Set the vacuum to 0 5 mbar u Tap the function Start on the function bar u Turn each manifold valve individually while checking the display to see if the actual press...

Страница 106: ...ction bar u Repeat the instructions for defrosting the ice condenser until the temperature of the defrosting water matches the ambient temperature 10 5 Error messages Error message Possible cause Solu...

Страница 107: ...Final confirmation for the aera tion of the drying chamber u Confirm if aeration should be done 5242 Vacuum pump oil operating hours exceed u Change vacuum pump oil if other vacuum pump is used 5243...

Страница 108: ...ter u Initiate a shutdown Defrost the ice condenser manually 5381 Preparation of vacuum in new ice condenser cannot be done within 30 min u Use less sample u Add new sample later u Check vacuum pump p...

Страница 109: ...at the same connector position u Contact BUCHI Customer Service Defective component e g heat ing coil cable plug 5571 Sample temperature sensor is disconnected u Connect a functioning PT 1000 at the s...

Страница 110: ...rants R507 and R1150 are used in the instrument Those refrigerants are toxic and must not be allowed to enter the soil or groundwater u Dispose of the appliance properly if necessary using a professio...

Страница 111: ...h the prior written permission of BUCHI 12 1 1 Accessories Description Order no Image Pirani pressure sensor Inficon PSG 550 11062229 Capacitive pressure sensor Inficon CDG 020 D 11062230 PT1000 sampl...

Страница 112: ...der no Image SD Card 1 GB 11064730 Connection cable for vacuum pump 11064934 12 1 3 Spare parts Description Order no Image User interface 11063580 User interface Pro 11063581 O Ring 300 mm 11065367 O...

Страница 113: ...scription Order no Image Vacuum seal KF 16 11063455 Vacuum seal KF 25 11063457 Vacuum seal KF 40 11063659 O Ring Silicone 94 61 x 6 99 mm 11062420 O Ring Silicone 161 3 x 5 33 mm 11062421 Edward vacuu...

Страница 114: ...without sealing 300 mm H 50 mm 11062912 Top cover manifold PMMA with 12 valves with out sealing 300 mm W 546 mm H 127 mm 11065595 Top cover stoppering without sealing only for rack for 4 heatable shel...

Страница 115: ...nifold rack 11064953 Baseplate PMMA for manifold rack 11065733 Suction nipple For manifold application to create vacuum in sample flasks 11065819 Ampoule adapter for manifold with 19 ampoule connectio...

Страница 116: ...filter paper 11067334 Manifold flask adapter set US joint size with 12 adapters incl filter paper 11066171 Manifold flask adapter set US joint size with 6 adapters incl filter paper 11067333 Filter ro...

Страница 117: ......

Страница 118: ...We are represented by more than 100 distribution partners worldwide Find your local representative at www buchi com...

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