Linkam Scientific Instruments FDCS196 Page 40 User Manual Download

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Linkam Scientific Instruments Ltd

Tel: +44(0)1737 363 476

Fax: +44(0)1737 363 480

Email:

[email protected]

Unit 8 Epsom Downs Metro Centre

Waterfield, Tadworth, Surrey, KT20 5LR, UK

www.linkam.co.uk

Version: 1.01.012010

Summary of Contents for FDCS196

Page 1: ...FDCS196 Freeze Drying Cryo Stage Linkam Scientific Instruments USER GUIDE ...

Page 2: ...Stainless Steel Vacuum Tube Connection 13 FDCS196 Pro System Setup 14 Edwards Vacuum Pump Setup 14 MV196 Motorised Valve System Setup 14 Mounting the MV196 14 Sample Preparation and Loading 15 Sample Loading Using G16 3 Sample Holder 15 Sample Loading Using FDCS196 CC Crucible Carrier and Quartz Crucible 18 Cooling Connections 21 Using The FDCS196 System 22 Programming Temperature 22 Using Linksys...

Page 3: ...t with us to Activate your warranty and technical support Access the online setup videos Permanently unlock the Linksys32 software if purchased If you have purchased Linksys32 software please install the software first This pro cess will guide to register all of your products See Linksys32 manual for further installation instructions A CD with a setup videos is supplied with your system ...

Page 4: ...ignated service facility The warranty shall not apply to defects resulting from interfacing unauthorized modification or misuse operation outside of the environmental specifications for the product or improper site preparation or maintenance Technical Support Any technical questions or queries should be addressed to the Technical Support Department at the ad dress shown on the back of this manual ...

Page 5: ... Support 8 The equipment is not intended to be used outdoors 9 Each product is equipped with a 3 wire grounded earth mains plug or a free end 3 wire mains lead The plug only fits into a grounded type outlet The free end mains lead should be connected to a correctly grounded 3 wire mains outlet Do not defeat the purpose of the grounded earth type plug Free end mains leads are colour coded as follow...

Page 6: ...ole 1 3mm Weight 0 6Kg FDCS196 System The system consists of a FDCS196 stage a T95 LinkPad System Controller LNP95 liquid nitro gen cooling pump system Pirani vacuum gauge and Linksys32 software The FDCS196 Pro System has an additional 1 5L Edwards Vacuum Pump and MV196 motorised vacuum valve control System Linksys32 System control software and digital video capture can be added as an option to co...

Page 7: ...ample chamber 6 X Sample manipulator 7 Door locking thumbscrew 8 Liquid nitrogen cooling connector 9 Heating element wire 10 Stainless steel cooling tube 11 Vacuum port 12 Sample holder ramp 13 Y Sample manipulator 14 Stage lid 15 Lid insert 16 Glass window 0 3mm thick 17 Tube Clip Holder and tubing for Nitrogen de fogging stage window 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 ...

Page 8: ...ng screws ensure that the aperture is in the centre of the field of view For other types microscope s substage see the included diagram for fitting instruction Setting up the Condenser for Koehler Illumination Place a small sample on a cover slip and place onto the surface of the silver block Use the 10X lens to focus on the sample Now close down the microscope field diaphragm and adjust the con d...

Page 9: ...ezers The System is supplied with a Vacuum Tweezers Kit which consists of a Vacuum Pump 1 and tweezers 2 Connect the tubing at the end of the tweezers to the Regulator Valve 3 connection Use the dial on the valve to adjust the vacuum for the tweezers Use a finger to block the hole of the tweezers to pick up a sample cover slip with the suction cup Release the finger to drop the sample cover slip 1...

Page 10: ... Connect the Stage Cable to the Lemo Connector on the FDCS196 stage and connect the other end to the Stage Connection Socket 1 Connect the cable from the Pirani Gauge to the Slot 4 labelled VAC 2 If you have got the Pro System with MV196 Motorised Vacuum Valve System connect the cable from the MV196 Motorised Valve to Slot 1 labelled MOT VAC 3 1 T95 back panel 2 3 ...

Page 11: ...ng Keep the screws safe by screwing them into the holes on the back panel as shown by the arrows The screws must be replaced back into the transit holes on the base when shipping back to Linkam for service or repair Back Panel Cable Connection Connect the Instrument Bus Cable 3 between the LNP95 and T95 as shown Note either of the purple coloured Instrument Bus Sockets on the LNP95 can be used LNP...

Page 12: ... before loading in between the Pirani Gauge 2 and the Stage Vacuum Connector 3 Ensure that the O ring is correctly seated in the gauge and vacuum connector before tightening the Clamping Bracket 4 screw 5 Connect the Pirani Cable with the LAN type connector 5 to the Pirani and the other end of the cable to the back of the T95 Slot 4 labelled VAC see page 9 1 2 3 4 5 5 ...

Page 13: ...n the Flexible Stainless Steel Vacuum Tube 2 and the stage Vacuum Connector 3 Ensure that the O ring is correctly seated in the Steel Vacuum Tube and vacuum connector before tightening the Clamping Bracket 4 screw 5 Connect the other end of the Flexible Stainless Steel Vacuum Tube to a Vacuum Pump Note the FDCS196 is only tested with a vacuum of 10 3 mBar Do not use a vacuum lower than this Vacuum...

Page 14: ...Mounting the MV196 The MV196 has an vacuum flange just like the vacuum ports on the sides of the FDCS196 Stage Use a small amount of vacuum grease to coat a thin layer on the surface where the O ring will sit Coat the surfaces of the T piece with vacuum grease as well The valve has two ports there is one in line and one protruding perpendicularly out of the side of this valve The side port 5 is fo...

Page 15: ...r A Freeze Drying Sample is prepared using a G16 3 Sample Holder 1 To load the G16 3 into the FDCS stage open the door of the stage by unscrewing the door thumb screw The G16 3 slides into the brass housing located just inside the door The Sample Holder Ramp 2 will guide the G16 3 up on to the silver block Close the door and tighten the thumbscrew to seal the stage Adjust the XY manipulators so th...

Page 16: ...l seal be tween block and crucible Using either the dropper or micropipette place a tiny drop of oil on the silver block Be careful not to place the oil over the aperture hole of the silver block Use the supplied Vacuum Tweezers or a pair of tweezers place a clean W16Q 16 x 0 3mm Quartz Sample Window directly on top of the oil inside the G16 3 Sampler Holder Adjust the XY manipulators by a few tur...

Page 17: ...air of tweezers place a clean W13G 13 x 0 17mm Glass Sample Window on top of the sample ensuring it touches the Shim Spacer Use the XY manipulators to move the Sample Holder so the edge of the sample sits across the aperture hole of the silver block This makes visual location of the sample easier once analysis starts ...

Page 18: ...as two spring clips to hold the crucible flat against the silver block This is to ensure good thermal contact To load the quartz crucible into the carrier lift the two spring clips about 2mm upward and slide the crucible in to the holder Release the two spring clips to hold the Crucible in place Use a pair of tweezers to place a Shim Spacer inside the Quartz Crucible 1 2 ...

Page 19: ...e it touches the Shim Spacer Before loading the Crucible Carrier the silver block must be prepared with silicon oil to provide a good thermal contact between the crucible and the silver block when the stage is under a vacuum Using either the dropper or micropipette place a tiny drop of oil on the silver block Be careful not to place the oil over the aperture hole of the silver block ...

Page 20: ...des the crucible up on to the block With one hand push the FDCS CC and with the other hand lift the edge of the crucible up the ramp and over the drop of oil When the drop of oil is roughly in the centre of the crucible gently lower the crucible on the block Now close the door of the stage and screw in the door locking screw This screw only needs to be finger tight Adjust the XY manipulators by a ...

Page 21: ...sliding it on and push until it comes to a stop It does not need to go all the way to the base of the connector The thicker silicon tube from the LNP95 cooling pump ends in a white PTFE connector 2 this is pushed over the end of the other stainless steel connector as seen in the image The smaller tube from the outlet on the LNP95 should be placed in position on the top of the lid using the Tube Cl...

Page 22: ...e will display a live vacuum read ing shown in the Main Vacuum Window 2 To set a vacuum turn on the Vacuum Pump and type in a vacuum value value dependent on unit chosen in the Set point s box 3 Click the Close Valve icon 4 and the motorised valve will automatically adjust itself to achieve the set vacu um value Note a graphical indicator of the valve position between the Close and Open position c...

Page 23: ... 2 to go to the Setup Tab page Touch the Vacuum Tab 3 to display the Vacuum Setup menu Touch either the mBar or kPa check box to select the vacuum unit Touch the Confirm icon 4 to go back to the main screen If you have the FDCS196 Pro System with the MV196 Motorised Valve connected there is an extra column labelled Vac mBar kPa displayed in the main screen 5 This option is available for you to pro...

Page 24: ...The MV196 is only designed to hold a controlled vacuum between 100mbar to 0 1mbar Any values outside this range may not be accu rate Note touch the Cancel button to go back to the main screen without changing the vacuum value Note Current is the current programmed rate Note Range is the maximum and minimum vacuum value that can be program for the selected vacuum unit mBar or kPa 2 Atmos in this mo...

Page 25: ...um When a Profile is running the following display in the main screen will help you to visualise the programmed vacuum setting in the Ramp 1 The programmed vacuum value will be shown 4 if the Vaccum is set to Auto 2 The word Atmos 5 will be shown if the Vauum is set to Atmos mode 3 The word Max 6 will be shown if the Vacu um is set to Max mode Note when a Profile is running and there is no Vacuum ...

Page 26: ...ed between the stage and connector The Gas Connector is self closing it is open when the Gas Insert is pushed into the Gas Connector To close the connector the Gas Insert is removed To use the Gas Insert connect one end to a tube 3mm inner diameter 6mm outer diameter and push the other end into the Gas Connector You should hear a click when the two parts are connected properly To remove the Gas In...

Page 27: ...he carrier lift the two spring clips about 2mm upward and slide the crucible in to the holder Release the two spring clips to hold the Crucible in place Load the sample into the quartz crucible Use as little sample as possible to ensure a small thermal load and therefore better temperature sensitivity Microscope objectives require a flat surface to give maximum field of view Place a 13mm coverslip...

Page 28: ...rewing the thumbscrew and carefully push the FDCS CC and crucible into the XY slide mechanism The crucible will be guided to the surface of the silver block by the Sample Holder Ramp Close the door and tighten the thumbscrew to seal the stage 1 ...

Page 29: ...ide of this white connector is the Gas Purging Tube 3 There is a valve opening Insert connector 4 inserted into the end of this tube During the purging procedure insert this connector into the Gas Purge Valve 5 on the side of the stage to open it The Gas Purge Valve 5 is opened when the Gas Insert 6 is pushed firmly into the connector a click is heard when the two parts are connected properly To r...

Page 30: ... to the LNP Screen Menu Touch Man 2 to switch the LNP95 to manual mode The word auto is changed to speed to indicate the LNP95 is functioning in manual mode Using the Keypad type in 100 max pump speed and touch the Enter button 4 to start the LNP95 at the programmed speed 5 Filling the Liquid Nitrogen Dewar Please follow your health and safety manual for directions on how to handle liquid nitrogen...

Page 31: ...Chamber use a finger on the right hand to block the gas outlet for a few seconds to allow pressure build then release the gas Do this for a few minutes to purge the stage 7 Look at the change of reflection in the stage window as the stage is pressurised and released to check that the stage is properly sealed If there is no change there may be a leak due to incorrect placing of the silicon o rings ...

Page 32: ...et a gas flow rate of 1 5L min 5 With the gas flowing through the Sample Chamber block the gas outlet for a few sec onds and releasing the gas outlet valve with a finger Do this for a few minutes to purge the stage Reduce the gas flow rate to 20cc min to continu ously purge the stage or remove the two Gas Inserts to keep the chamber under closed inert atmosphere Note Helium gas is not recommended ...

Page 33: ...slips are held firmly then turn the assembly over and screw down the Lid Insert until it is felt to come to a stop Note W22G0 3 22mm diameter and 0 3mm thick glass window must be used for when the stage is to be used under vacuum Note you can use the W22G 22 x 0 17mm window if the stage is used without a vacuum Bottom Window Assembly Use two narrow spacing pins of Window Tool 2 to align it to the ...

Page 34: ...n 7503 FDCS Kit Full Replacement Spares Kit WG Water Gas Valve Insert x2 WVC Water Gas Valve Connector x2 SSR Silicon Rings for Lid and Base Set of 4 RI17 Stainless Steel Ring Set THC Tube Clip Holder for Nitrogen de fogging stage lid tube ORTHMS Set of O Rings for THMS Stage Body and Lid THMS Q 15mm diameter Quartz Crucible for FDCS CC FDCS CC Crucible Carrier with Spring Clips for FDCS196 G16 3 ...

Page 35: ...or W16G x4 W13G 13mm diameter Glass Sample Window 0 17mm thick Box of 100 THMS Q 15mm diameter Quartz Crucible for FDCS CC Part No Part Name Part Description 9584 FDCSB Spare Pure Silver Heating Element incl Platinum Temperature Sensor Part No Part Name Part Description 18006 VP E2M1 5 Edwards Vacuum Pump including EMF3 Mist Filter Part No Part Name Part Description 7505 VacC K Spare Vacuum Connec...

Page 36: ...ked If any damage has occurred to any of these items then it will be necessary to replace them If no damage is found check that the silver block is not constricted This can be checked simply by blowing through one of the steel cooling tubes using a compressed air line 2 Stage will not cool down to 196 C Check that the stage lid is not touching the silver block when screwed down Check that the silv...

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