tousimis® SAMDRI®-PVT-3D
Contents
1. 8784A with every 500lbs 226 8kg LCO tanks changes The secondary 0 5m T Filter Element 8783B should be annually replaced Connecting Exhaust Hoses to SAMDRI PVT 3D 6 Attach the 6ft White COOL BLEED Exhaust Tubing provided to the COOL BLEED CO Exhaust Outlet on the left hand side of the SAMDRI PVT 3D and the 6ft Clear Exhaust Tubing to the PURGE VENT Exhaust outlet See photos below The tubing should be free of kinks which could block passage of rapidly exiting noisy CO gas or solid flakes of CO NOTE It is best to secure both the ends of the COOL BLEED and PURGE VENT Exhaust A M COOL BLEED tubing so that the ends do fa CO Exhaust not move during exhaust mad modes Be careful not to obstruct exhaust hose I D when securing PURGE VENT Exhaust Page 6 2008 tousimis Installing SAMDRI PVT 3D Samdri PVT 3D Complete Inlet Outlet Setting 1 LCO Connect Inlet EN Pas COOL BLEED CO Exhaust AUST 13 PURGE VENT Exhaust 7 Check chamber O ring and windows inspect unit to insure it is free of dust oil and moisture Chamber O ring is NOT to be greased but keep the chamber groove clean and NOTE The chamber O Ring should lie completely in its groove NEVER grease the O Ring Z J i v O Ring trc 8770 51 should iiy Bie be properly seated and dry prior to placing Chamber lid onto Process Chamber NOTE Do not expose chambe2. After all of the pressure is safely bled from high pressure line unscrew Oil Water Filter Housing by hand Position LCO Filter Element 8784A into lower Oil Water Filter Housing Let into center of lower Oil Water Filter gravity hold element in place Housing Pe if ee Carefully lower Oil Water Filter Housing Hand tighten the housing body together over replacement element 8784A firmly O Ring seats properly Open main tank valve and check for leaks 2008 tousimis Page 25 Chapter 7 LCO T Filter Element Installation 87 70 83B After all of the pressure is safely bled from high pressure line unscrew T Filter cap using wrench T Filter Gasket 8770 83D T Filter Element 8770 83B NOTE Do not over tighten T Filter Cap Hand tighten T filter cap Use wrench tighten the T filter cap firmly Open LCO tank valve and check for leaks Page 26 2008 tousimis 2008 tousimis Maintenance and Support FAQ Should the LCO tanks be secured YES It is recommended that The LCO Tanks be placed onto LCO Tank Scales tre 8770 54 and secured as per your facility safety regulations Monitor the net LCO used When you approach 50 LCO consumption it is recommended that you replace the LCO tank with a new one Always keep several spare tanks of LCO in reserve Do I need an In line regulator between the tank and the SAMDRI PVT 3D NO A regulator is
3. Chapter 5 The final dehydration step involves three conditions for the 100 dehydrating liquid 1 The dehydrating liquid should fill the vessel containing the sample in order to reduce exposure to atmospheric moisture outside the SAMDRI PVT 3D Avoid the use of powder 2 The vessel should then be tightly stoppered with the lid hand tighten type CaSO dehydrants in the ethanol We suggest the use of clean silica gel type dehydrants to avoid sample contamination from powdering CaSO 3 The 100 fluid should be obtained from a newly opened bottle of ultra pure ethanol or that it contain a dehydrant to insure no water contamination ALCOHOL IS HYGROSCOPIC crystals General Form of Phase Boundaries Pressure vs Temperature for CO Pc 1072psi Critical Point Pc Critical Pressure of CO Tc Critical Temperature of CO Page 20 2008 tousimis CHAPTER 6 Illustrations Metering Valve w Vernier Handle Setting Example The numerical markings are arbitrary numerals for the sole purpose of meter valve adjustment position reference f 1 complete counter clockwise 360 rotation from the 0 00 starting position is referred to as dre 028 aua 0 50 Setting 1 00 Setting Venting Precautions LCO Inlet COOL BLEED CO Exhaust PURGE VENT Exhaust Connect 8784 LCO FILTER ASSEMBLY DURING PURGE COLLECT WASTE ALCOHOL INTO A LCO Tank CARBOY 1 GAL MINIMUM O
4. Damage may result Use supplied 7 16 Open End Wrench to attach Exhaust Connect Line to both SAMDRI PVT 3D and Condenser SAMDRI PVT 3D uc Ca a E Er E7 _ Exhaust Insulate 8 Wire Tie M 5 Connect the white 10 length of Condenser Exhaust Tubing to the Condenser Vent Outlet and cover the Vent Outlet with the provided Vent Insulate See Step 8 9 on next page 2008 amp tousimis Page 41 Appendix C Connecting Condenser Exhaust Vent Insulate NOTE It is best to route Condenser Exhaust Tubing to facility Exhaust Conduit and attach via 1 4 male hose barb to conduit 8 Wire Tie 1 4 Male Hose Barb Connecting Condenser Drain 6 The 3 length of Clear Tygon Condenser Drain Tubing should be placed onto the condenser s drain hose barb The clear hose will allow you to visually see the alcohol draining into a carboy or Facaility s Solvent Drain Page 42 2008 tousimis Installing SAMDRI PVT 3D with SOTER Condenser SOTER Condenser Exhaust Connect Overview Exhaust Connect Power ON OFF POP Cord SAMDRI PVT 3D ower Cor Vent Outlet Attach 10 White o Exhaust Tubing to Exhaust Conduit O Alcohol Drain Valve Leave in Open Position except when relocating SOTER Condenser O Exhaust Connect Attach 3 clear Condenser drain tubing and lead to a Carboy 1 gal minimum or Solvent Drain
5. PURGE MODE 6 Keep FILL valve open To exchange all the ethanol with LCO within the chamber slowly open the PURGE VENT metering valve exhaust you can visually see movement from left to right in the chamber Make sure the liquid level in the chamber is always above the sample The FILL rate adjust should always exceed the PURGE VENT rate to insure that the sample remains covered in a liquid state Place a carboy or an Erlenmeyer Flask at the end of the clear PURGE exhaust tube to collect waste alcohol Continue in PURGE mode until all of the ethanol is exhausted To be certain that all the ethanol has been purged hold a clean piece of paper glycine paper works best about four inches from the exhaust tube and collect the solid white CO that is being emitted The solid CO will sublime and any visible wet marks on the paper indicates that there is still ethanol remaining If chamber temperature rises above 10 C during PURGE mode open the COOL VALVE this will not interfere with the PURGE mode until the chamber is cooled to 0 C then close the COOL valve and continue purging 7 After ethanol is purged close PURGE VENT metering valve Keep the FILL valve open to insure chamber is full with LCO Note that a meniscus will travel across the viewing window indicating that the chamber is full Close the FILL metering valve Turning HEAT ON OFF mdri PVT 3E Page 10 2008 tousimis Operating SAMDRI PVT
6. SAMPLE DRYING AT THE CRITICAL POINT SAMDRI ING METHOD SAMDRI ING involves immersion of the sample in an intermediate fluid ethanol and its substitution with LCO under pressure The LCO is automatically converted to its gaseous phase at the critical point in the high pressure chamber and removed at temperatures higher than 31 1 C thereby avoiding the distortion resulting from evaporation boundaries or thermal expansion Typical Paths that Critical Point Passage May Follow during Heat Phase p 14 shows the isotherm for CO including the critical isotherm at 31 1 C Superimposed is a path which an average critical drying cycle SAMDRI can follow divided here into four stages 1 the process chamber is COOLED and FILLED with LCO and maintained at 0 C 10 C 2 d the sample in the alcohol under pressure is PURGED of the alcohol with LCO until all traces of intermediate fluid alcohol are removed 3 the chamber is heated automatically to a temperature above the critical temperature of CO While the chamber volume is constant there is an accompanying rise of pressure to above the critical pressure of CO and the liquid phase is converted to the gaseous phase 4 the gaseous CO is exhausted at a temperature above 31 C from the process Page 17 Chapter 5 chamber returning the sample to conditions of room temperature and pressure The sample is now critically point dried and ready for coating metal film coa
7. transfer your sample into the process chamber Make the transfer quickly in order to avoid the samples exposure to air and moisture The chamber O Ring should lie completely in its groove NEVER grease the O Ring Place the chamber lid down over the chamber using the 3 knurl nuts tighten each by hand with equal pressure Never use channel locks or pliers for tightening the knurl nuts Always hand tight 2008 tousimis Operating SAMDRI PVT 3D COOL Valve Adjust COOL MODE 4 Open COOL valve to approximately the 0 50 position See metering valve illustration p 21 The temperature of the chamber should drop to near 0 C from room temperature in approximately 1 minute The cool rate is a function of the amount of LCO running through the COOL VALVE Usually a 0 50 setting on the COOL VALVE is satisfactory It is normal to hear the COOL Exhaust making audible noise as it exhausts from white tubing Close COOL VALVE when temperature reaches 0 C FILL Valve Adjust FILL Valve FILL MODE 5 Open FILL metering valve slowly until the chamber is full LCO will enter the process chamber mixing with the high purity alcohol A bubble meniscus will travel across the quartz viewing window indicating the chamber is full Maintain the FILL valve open to a setting of about 0 50 turns this setting could vary as per use of the metering valve 2008 tousimis Page 9 Chapter 3 PURGE VENT Valve Adjust
8. 3D 8 At this point all the metering valves should be in the CLOSE 0 00 position see page 21 Turn HEAT switch ON HEAT light will go ON As the temperature C increase so will the pressure At approximately 1 350 psi 5 20 C the pressure relief valve will begin to vent the chamber pressure The chamber s pressure will be maintained above the Never over tighten Meter critical pressure for CO 1 072 psi As the temperature passes the critical temperature for Valves when closing to 0 00 CO 31 C the heater will cut off indicated by the heat light turning OFF between 33 C position Over Tightening 39 C The temperature may coast up to 44 C this is normal Do not turn off the HEAT may damage valves switch The SAMDRI PVT 3D will automatically maintain the chamber at a temperature higher than the critical temperature 31 C of CO ue 9 At this point the SAMDRI PVT 3D is above the critical pressure 1 072 psi and tousimis oe ee eed temperature 31 C for CO It can maintain itself automatically at the tousimis equilibrium EQUILIBRIUM state indefinitely For best results we recommend that you wait 4 minutes in equilibrium before proceeding to BLEED mode 10 POWER and HEAT switches are ON FILL COOL BLEED and PURGE VENT metering valves are closed Slowly open the BLEED metering valve to the BLEED meter valve adjust position noted on the Check Out Data Sheet The initial BLEED flow rate via t
9. perfectly clear the exiting CO will be solid white even lower freezing points drop away from the top chamber window these fluids will be flushed A warming trend will be noted during the PURGE mode since the incoming fluid originates out as liquids A soft dry at room temperature The operator should occasionally check the chamber temperature and coated paper held open the COOL valve as necessary ensuring that the purging continues in the liquid state It momentarily in the is best to keep the temperature between 0 10 C during the PURGE mode exhausting stream will catch The purge time required for complete solvent exchange is not standardized but is dependent he he olid akee o upon the size density and cellular characteristics of the sample Exchange in a mono layer of CO and when shaken out ells can be completed within several minutes whereas large semipermeable structures may will show wet spots and require 15 minutes Generally 24 samples of a size 4mm x 6mm x 2mm accommodated by a indicate that there i Sample Holder tousimis catalog 8763 will require about 10 minutes these purge times are remaining alcohol to be only suggested however and should be established in each case by process operator purged CRITICAL POINT PASSAGE HEAT When all the intermediate fluid permeating the sample has been replaced by LCO purging and cooling are terminated Make sure the chamber is completely filled with LCO Return to FILL
10. Barb 30 76cm Minimum PURGE VENT COOL Meter Valve Meter Valve FILL Meter BLEED Valve Meter Valve TABLE TOP 36 92cm Minimum Width Page 39 Appendix C 3 The tousimis LCO Filter Assembly tousimis catalog 8784 is factory installed directly onto the high pressure hose See p 31 32 This helps prevent sample contamination from oil water and particulates Change the 8784A filter element with every 500lbs 226 8kg LCO tanks changes The secondary 0 5um T Filter element may be removed ultra sonicated and reinstalled every 1 year SAMDRI PVT 3D Inlet Outlet Connect 1 LCO Connect Inlet LOCO CONNECT COOL BLEED EXHAUST INLET CO2 EXHAUST CONNECT 2 COOL BLEED Exhaust Outlet Exhaust Connect to SOTER Condenser PURGE VENT Exhaust Connect Line Exhaust and Condenser Vent Insulates 4 Connect the SOTER Condenser to SAMDRI PVT 3D through Exhaust Connect see picture below 1 Exhaust Connect Line 7 0 Length Exhaust Insulate 1 75 Length 13 Vent Insulate 2 25 Length Page 40 2008 tousimis Installing SAMDRI PVT 3D with SOTER Condenser Connecting SOTER Condenser to SAMDRI PVT 3D SAMDRI PVT 3D tog NOTE MLET O 7 16 Open CEE Er NET End wrench Never over tighten 7 16 D fittings that connect e AA AN ry 4 ji Exhaust Connect Line to a both SOTER Condenser Connect and SAMDRI PVT 3D Line
11. Cords plugged into Power Strip 2008 tousimis Page 47 Appendix C Closing SAMDRI PVT 3D Process Chamber Chamber Sealing Procedure 1 Prior to placing chamber lid onto chamber be sure that o ring and surrounding chamber surface is clean and moisture free NO Grease 2 Carefully align chamber lid over chamber and carefully lower onto chamber face 3 Carefully place the 3 knurl nuts onto each appropriate chamber post and turn in a clockwise direction until flush with chamber Chamber Face Chamber O Ring seated in Chamber Gland PA 48 2008 tousimis Installing SAMDRI PVT 3D with SOTER Condenser Condenser Drain Valve Always maintain OPEN position during process run except when relocating SOTER Condenser or emptying Carboy Open Position SOTER Condenser Power Switch Turn SOTER Condenser Power Switch ON 3 5 minutes prior to process run Power Switch 2008 tousimis Page 49 ILLUSTRATION INDEX Chamber Care 23 Chamber Lamp Chamber Lamp 34 Installation 35 Removing 32 34 Flow Meter 28 General Form of Phase Boundaries Pressure vs Temperature for CO 20 Isothermal of Carbon Dioxide and an Average Drying Path of Sample in the SAMDRI PVT 3D 18 LCO Filter Assembly 24 25 LCO T Filter Element Installation 26 Purge Line Filter Replacement Instruction 36 37 SAMDRI PVT 3D 2 SAMDRI PVT 3D Chamber O Ring 7 Dryer 2 Exhaust Hose Co
12. MDRI PVT 3D with SOTER Condenser SAMDRI PVT 3D Setup Overview Remote LCD readout of LCO Tank Weight co Cylinder ON OFF Valve External tousimis Combination Filter 8784 O T Filter w 0 54m Element High Pressure Hose 5ft long other lengths available upon request O COOL BLEED CO Exhaust Tube to Hood Exhaust Conduit or Outdoors White 1 4 ID 10ft Q 120V Properly Grounded Outlet from either Wall or Transformer O Power Strip for PVT 3D and SOTER Condenser Exhaust Connect to SOTER Condenser Condenser Vent Outlet 1 4 ID to Hood Exhaust Conduit or Outdoors 10ft Condenser Drain Valve Always maintain OPEN position during process run except when relocating SOTER Condenser or emptying Carboy Condenser Clear Drain Tubing 12 1 4 ID 3ft routed to Carboy Carboy Exhaust Tube to Hood or Outdoors 15ft Tare Weight Varies Consult your LCO supplier or may be 14 stamped on tank Ceramic Heater or Heater Jacket maybe required in a 15 cold tank placement position Syphon Dip Tube LCO Tank Scale with Remote LCD Display trc 8770 54 At Room Temperature 20 C 24 C average LCO tank pressure is 800psi 5 2008 tousimis 1 a OOOO 2 EC EE lt a A o typical RULL 147 5 Ib typical LCO Tank Approximately 50 Usable for Waste Alcohol Collection 1 gal Minimum 1 4 Male Hose
13. NECT COOL BLEED EXHAUST INLET CO2 EXHAUST CONNECT oo fj a R y i LCO High Pressure COOL BLEED CO Exhaust Exhaust Connect to Hose to LCO Tank to facility exhaust SOTER Condenser SAMDRI PVT 3D with Complete Connects 1 LCO High Pressure Hose O COOL BLEED CO Exhaust Tubing 13 SOTER Condenser Vent Outlet Condenser Drain Tubing to Carboy or Facility s Solvent Drain O Exhaust Connect 2008 tousimis Page 45 Appendix C 9 Connect Condenser Drain Tubing clear to a Carboy 1 gal minimum or Facility s Solvent Drain Condenser Drain Valve should always be maintained in the OPEN position during the process run except when relocating Condenser or emptying Carboy Connect Carboy Exhaust Tubing white to Fume Hood or Outdoors See p 39 Setup Overview Connecting Power Supply 10 Make certain facility 120V Power Supply is properly grounded and plug in the Power Strip supplied Next plug in both the SOTER Condenser and SAMDRI PVT 3D Power Cords into the Power Strip Power Strip NOTE Please be certain that both SAMDRI PVT 3D and the SOTER Condenser power switches are in the OFF position before plugging their power cords into the Power Strip Power Strip PQ 46 2008 SS OUISIMIS Installing SAMDRI PVT 3D with SOTER Condenser SAMDRI PVT 3D Set Up Overview SOTER Condenser Both SOTER Condenser and SAMDRI PVT 3D Power
14. REDUCTION BLEED Mode Once the critical point has been passed with an adequate margin of safety the CO which is now in a dense vapor state is exhausted slowly from the process chamber Typical Chamber Temperature during Pressure Reduction BLEED Lu ec ZO Ww Q 2 W i TIME Minutes Typical Range of Paths that Pressure Reduction May Follow in the SAMDRI PVT 3D At 400 psi VENT mode may be activated CHAMBER PRESSURE psi TIME Minutes 2008 tousimis Page 15 Chapter 4 TYPICAL PROCESS CYCLE A typical process cycle including 7 minutes of purge time might run for about 1 2 hour as shown in the following and may use 1 5lbs 0 7kg of CO Typical Drying Cycle TYPICAL SAMDRI PVT 3D DRYING CYCLE Critical Point Passage Pressure Reduction CARE OF DRIED SAMPLES After drying care should be taken to prevent damage to the sample surfaces It is Note that the SAMDRIed recommended that the sample be attached to a tousimis 10 mm diameter or Cambridge Biological samples could 1 2 stud and as soon as possible coated with the appropriate conducting layer SAMDRI absorb certain glues DO ed biological samples are receptive to a metal coating in a vacuum and do not require any NOT USE glue to mount preparatory carbon coating If the sample cannot be further processed immediately after your sample since it will drying it should be stored in an isolated and desiccated enviro
15. RI PVT 3D Imar PV ior _ PURGE VENT Exhaust Hose F n r T 5 aegen vel P e Pa m2 i TE ONE Page 32 2008 tousimis 2008 gt tousimis Chamber Lamp installation 4 Close main LCO tank valve bleed LCO High Pressure Hose Disconnect LCO High Pressure Hose using supplied 9 16 Wrench and 1 2 Wrench from the SAMDRI PVT 3D Connect Inlet 9 16 Wrench LCO High Pressure Hose aa En pn een ann n u uaa an i or in Prg mr r TESTS r i 3 i sus ME LCO Tank with Siphon Tube 6 Unscrew the 4 black rubber legs that secure the access panel in place Page 33 Appendix A 7 Remove and set aside the access panel Note access panel orientation so that you may re install panel in the same direction upon procedure completion SAMDRI PVT 3D Chamber View Chamber Lamp Cat 8770 10 Chamber Lamp installation 9 The Chamber Lamp is mounted into a Bayonet style lamp holder Push Chamber Lamp towards the lamp housing and twist to the left to uninstall lamp As shown below 7 oN 10 Install a new Chamber Lamp Cat 8770 10 Please note that you may need to support the Chamber Lamp housing with your free hand for support 11 Re install the access panel and re connect power and all hose s prior to starting up system 2008 tousimis Page 35 APPENDIX B Purge Line Fi
16. RY AT ALL TIMES 2008 tousimis ACETONE UNT Page 23 Chapter 7 LCO Filter Assembly THE tousimis LCO FILTER ASSEMBLY 8784 O 5 Figure Shown Below Installation Instructions Tighten 1 Uncouple CGA 320 S S nut from LCO tank Close Hole if main tank valve Crack S S nut and bleed line pressure Needed Make certain there is no pressure within the high pressure hose 2 Install filter element as shown in the diagram 8784A Push element steadily into upper housing orifice until slight resistance is felt Screw housing Part B onto upper housing Part A Be sure that teflon O Ring is in place Rotate to Tight 3 The 0 5 pm T Filter Element 8770 83B is pre installed into T Filter Change LCO Filter Element 8784A with every 500 lbs of LCO consumption change T Filter Element 8770 83B every year to insure proper filtration ge Filter ement 8784A Oil Water Filter Housing LCO Tank w Siphon Tube Main LCO Tank Valve O T Filter with T Filter Element 0 5 um Gasket Teflon or Nylon 8770 83B CGA 320 S S Nipple O CGA 320 S S Coupler Nut oiwater Filter Housing w Tetion tape CAUTION USE tousimis LCO FILTER ELEMENT LCO Filter Element trc 8784A ONLY 9784 a Ne MOSS Operating pressure not to exceed 1000 psi Samdri PGA 2008 tousimis Maintenance and Support LCO Filter Element Installation 8784A
17. SAMDRI PVT 3D D O NOTE Do not over tighten fittings on either end of Exhaust Connect Check for leaks during the first run after connecting Tighten as necessary with 7 16 wrench DO NOT OVER TIGHTEN SAMDRI PVT 3D SOTER Condenser 2008 tousimis Page 43 Appendix C Connecting COOL BLEED CO Exhaust 7 Attach the 10ft White exhaust tubing provided to the COOL BLEED CO Exhaust outlet on the left hand side of the SAMDRI PVT 3D Tubing should be free of kinks which could block passage of rapidly exiting noisy gas or solid flakes of CO NOTE It is best to route COOL SAMDRI PVT 3D SAMDRI PVT 3D to facility Exhaust Conduit via 1 4 male hose barb if possible BLEED CO EXHAUST ae lay v a j 1 4 Male Hose Barb Connecting LCO High Pressure Hose 8 Attach the HIGH PRESSURE HOSE to the SAMDRI PVT 3D LCO CONNECT INLET Gently tighten the High Pressure Female Connector using the two open end wrenches provided the 9 16 onto the Hose and the 1 2 onto the Inlet Stop at the feel of first resistance re tighten if necessary should it leak 1 2 Open End 9 16 Open End rie a High Pressure SAMDRI PVT 3D ital Female Connector Ke J 1 cos Lt BLE Ua ExHa E WT x CONNIE No Teflon Tape Required PA 2008 COUN Installing SAMDRI PVT 3D with SOTER Condenser SAMDRI PVT 3D Inlet Outlet Connect View LCO2 CON
18. TABLE OF CONTENTS Chapter 1 SAMDRI PVT 3D Overview SAMDRI PVT 3D 2 SAMDRI PVT 3D Setup Overview 3 Chapter 2 Installing SAMDRI PVT 3D Preparation of Installation Site 4 Installation of the SAMDRI PVT 3D 4 Chapter 3 Operating SAMDRI PVT 3D Operating SAMDRI PVT 3D 8 Chapter 4 Operational Notes Safety Devices 12 Installation 12 Loading 12 Chamber Cooling 13 Solvent Exchange PURGE 13 Critical Point Passage HEAT 13 Pressure Reduction BLEED 15 Typical Cycle 16 Care of Dried Samples 16 Chapter 5 Theory of Critical Point Drying The SAMDRI PVT 3D 17 Preservation of Delicate Ultrastructure 17 Sample drying at the Critical Point SAMDRI ING Method 17 Transitional Fluid 18 Sample Preparation before SAMDRI ING 19 Water Exclusion 19 Chapter 6 Illustrations 21 Chapter 7 Maintenance and Support Regular Maintenance Schedule 22 Chamber Care 23 LCO2 Filter Assembly 24 LCO2 T filter Element Installation 26 FAQ 27 Optional Accessories 30 Warranty 30 Repackaging for Shipment 31 Appendix A Chamber Lamp Replacement Installation 32 B Purge Line Filter Replacement Instruction 36 C Installation of the SAMDRI PVT 3D with SOTER Condenser 38 Illustration Index 50 User s Notes 51 Check Out Data Sheet Warranty CHAPTER 1 SAMDRI PVT 3D Overview THE ADVANCED MANUAL CRITICAL POINT DRYER tousimis Catalog 8755B SAMDRI PVT 3D Page 2 2008 tousimis SAMDRI PVT 3D Setup Overview SAMDRI P
19. VT 3D Overview Remote LCD readout display of LCO Tank Weight Main ico Tank ON OFF Valve Oil Water Filter Housing of LCO2 Filter Assembly 8784 T Filter w 0 5um Element of LCO2 Filter Assembly 8784 High Pressure Hose 5ft other lengths available upon request COOL BLEED Exhaust Hose O White 1 4 ID 6ft COOL BLEED CO Exhaust Vented to either Hood Exhaust Conduit or Outdoors 120V Properly Grounded Outlet from either Wall Outlet or Transformer O PURGE VENT Exhaust Hose Clear 1 4 1D 6ft PURGE VENT Exhaust Hose routed to either an Erlenmeyer Flask a Carboy 1 gal minimum or Solvent Drain if available 11 FILL Meter Valve coor Meter Valve 13 BLEED Meter Valve 2 PURGE VENT Meter Valve power swiTcH M HEAT SWITCH Tare Weight Varies Consult your LCO supplier Usually stamped on tank Ceramic Heater or Heater Jacket maybe required in a cold tank placement position Siphon or Dip Tube 20 LCO Tank Scale trc 8770 54 At Room Temperature 20 C 24 C average LCO tank pressure is 800psi 5 2008 tousimis 1 a OOO ical NUL ay ps typical LCO Tank Approximately 50 Usable 1 4 Male Hose Barb SNS VAL AY Or 30 76cm Minimum TABLE TOP 20 51cm Minimum Width Page 3 CHAPTER 2 Installing SAMDRI PVT 3D 5 PREPARATION OF INSTALLATION SITE See A
20. again if necessary Heat is now applied to the chamber elevating the transitional fluid to above its critical temperature and pressure During the HEAT mode the CO may appear as oily currents due to the heat causing variations in LCO densities and thus the 2008 tousimis Page 13 Chapter 4 Schlieren pattern appearance The HEAT mode is thermostatically controlled to maintain a temperature at a safe margin above the critical values yet low enough that thermal destruction above 55 C of any NEVER use a LCO tank if biological sample does not occur it is kept outside in the winter Bring it to room temperature for 2 3 days before use otherwise due to low LCO tank temperature the tank will not supply the SAMDRI with LCO at the proper pressure The chamber pressure increases relative to the increase in temperature It is likely that the critical pressure will be reached before the critical temperature if the chamber was completely filled with LCO when heat was applied The APCS is factory set for 1 350 45 20 C see factory check out data sheet and will keep the chamber below 1 600 psi until the chamber temperature rises above the critical temperature Typical Paths that Critical Point Passage May Follow During Heat Mode Safety Control Rupture Disk CO Critical Pressure Lu o Q S i O N oO O Page14 2008 tousimis Operational Notes PRESSURE
21. al ultrastructure is well stabilized and free of water Most biological samples preparation could include FIXATION Fixation generally utilizes an aldehyde such as formaldehyde glutaraldehyde or acrolein to provide rapid inter and intra cellular penetration and fixation followed by osmium tetroxide for further fixation STAINING AND SPECIAL TECHNIQUES A fixative stain such as aqueous solutions of osmium tetroxide or silver is employed for SEM samples prior to dehydration and critical point drying DEHYDRATION The fixed sample is taken through a series of increasing concentrations of a liquid such as ethanol ending in a 100 ethanol of the highest possible purity tousimis CAT 5086 Transfer to room temperature before placing it in alcohol in the SAMDRI PVT 3D chamber and seal Then you may initiate the process run WATER EXCLUSION Water or oils remaining on the sample during critical point drying will not pass through the critical point with the transitional fluid since their critical pressures and temperatures are different Instead the water will evaporate from the sample surface and cause damage or the oils will cover the surface and render sputtering or shadowcasting with an electrically conducting element impossible Therefore the sample must first be completely dehydrated as mentioned above and precautions must be taken to avoid subsequent rehydration before critical point drying SAMDRI ING Page 19
22. ation with pressurized LCO as a transitional fluid The user may also find it helpful to mount the LCO cylinder on a tank scale 8770 54 to monitor transitional fluid supply by weight not pressure since only approximately 50 of the original net LCO may be used The SAMDRI PVT 3D connects to a standard 120V 50 G0Hz 15 Amp grounded outlet and can be used wherever space permits Waste alcohol can be collected into a carboy or an Erlenmeyer Flask before the venting of the CO commences The work area should be clean and dry at all times LOADING An adequate amount of intermediate fluid Ultrapure Alcohol 99 9 enough to cover the sample and holder should be poured carefully into the chamber before placing your samples into the chamber This will minimize surface evaporation of the dehydrating intermediate fluid ethanol from the sample This is done at room temperature to avoid moisture absorption from the atmospheric environment 2008 tousimis Operational Notes aug CHAMBER COOLING The tousimis cooling capability of the SAMDRI PVT 3D may be exercised at any time for it is an entirely independent operation from FILL or PURGE VENT The chamber is brought down to a temperature of approximately 0 C or below Consult Check Out Data Sheet for your unit The LCO tank should have at least 50 net weight of LCO for proper COOL operation Chamber cooling is necessary to ensure filling with the liquid phase of the trans
23. cessories p 37 Typical nominal LCO tank weights for Net 501b LCO tanks e Full tank 140 to 170 lbs Tare of tank 90 to 120 lbs e Most of the time you may use 50 of a 501b net weight CO tank e It is good practice to have spare LCO tanks stored in reserve in case a tank runs out during mid process A properly grounded 120V 50 60Hz outlet should be located within 4ft 1 2 m of set up site INSTALLATION OF THE SAMDRI PVT 3D This SAMDRI PVT 3D is supplied with the basic accessories for operation with LCO as a transitional fluid for optional accessories see p 37 1 Position a LCO tank with dip tube within 4 feet 1 2m of the PVI 3D For a longer high pressure hose length see p 37 tre 8770 HPS The LCO tank should be mounted on a 400lb 182kg capacity floor scale w remote LCD display tre 8770 54 to easily monitor LCO supply 2 No pressure gauges or regulators need be installed between the supply LCO tank and the SAMDRI PVT 3D LCO connect inlet The stainless steel sheathed high pressure hose accompanying the unit is fitted with a CGA 320 hex coupling which accepts a 3 4 plastic gasket supplied and joins the hose directly to the CGA 320 threaded male nipple at the tank top See p 31 ALL tanks are equipped with a rupture disc All LCO fittings and gasket surfaces should be kept clean and dry NEVER OVER TIGHTEN FITTINGS TUBING ATTACHED MAY BE DAMAGED 2008 tousimis Installing SA
24. he flow meter should be 8 10 SCFH Fast decompression could result in CO condensation Chamber heater will cycle ON and OFF automatically to maintain temperature above the critical temperature during BLEED Close BLEED metering valve at 400psi BLEED Valve Adjust BLEED MODE SAMDRled samples could 11 Open the PURGE VENT metering valve to at least 0 50 setting to reduce chamber be hygroscopic coating pressure to 0 psi The pressure will reach 0 psi atmospheric pressure in 2 3 minutes loosen with conducting film the 3 Chamber Knurl Nuts evenly by hand Remove your sample and store in a dry immediately will best environment i e vacuum desiccator etc for further processing preserve surfaces of interest for your studies However 12 You may begin your next process run immediately if desired even after coating with a conducting metal layer lt 13 After last process run of the day make certain the chamber is clean and O ring is in place 100A thick your sample Place lid on and tighten by hand Close the LCO main tank valve and open all valves of should be kept dry and the SAMDRI to drain them from any residual line pressure then close all the valves clean Clean the SAMDRI surfaces Turn Power OFE 2008 tousimis Page 11 CHAPTER 4 Operational Notes Methanol may also be used as an intermediate fluid Page 12 SAFETY DEVICES The SAMDRI PVT 3D sample process chamber is a h
25. igh pressure metal alloy vessel with viewing ports designed to withstand the pressures used in the critical point drying process To ensure additional operator safety the following features are incorporated e A mechanical Automatic Pressure Control System APCS which will maintain the chamber at a pressure between 1 350 psi 5 see Check Out Data Sheet for your dryer s pressure relief valve specs e A rupture disc which will be activated 2 000 psi at 20 C if the mechanical APCS should fail see factory check out data sheet for the setting s of your unit e Quartz ports which will crack along the crystal line rather than shatter should they become unduly stressed Immediately replace chamber lid if window becomes cracked e Metal alloy sintered stainless steel filters placed internally along both the inlet and exhaust paths preventing solid particles from fouling the gas lines valves fittings e An electronic heating system which is governed by two thermostats one to maintain the chamber during critical point passage at temperatures 37 C 2 C see factory check out data sheet for your unit and a second safety thermostat to shut off all heating should a failure bring the chamber temperature near 49 C 3 C e A bulb and a translucent diffuser plate below the sample chamber which illuminate chamber contents for easy viewing INSTALLATION The SAMDRI PVT 3D is supplied with all necessary internal accessories for oper
26. itional fluid LCO Cooling also insures expulsion of the gas phase ahead of the liquid phase in the pressure hose connecting the transitional fluid tank to the SAMDRI PVT 3D inlet circuit CO exiting from the COOL BLEED Exhaust hose may appear in solid flakes as it encounters the lower pressure environment A 6ft 1 4 I D white static free exhaust tubing reduces the noisy rapid expansion of the LCO exhaust This is a standard accessory SOLVENT EXCHANGE PURGE After cooling the chamber transitional fluid LCO may now be allowed to simultaneously enter and leave the chamber This process mode of incoming LCO and outgoing alcohol and SUGGESTED TEST TO CO is called PURGE Characteristics visible to the operator during the PURGE mode are as VERIFY COMPLETION follows OF PURGE Since more adiabatic e The intermediate fluid alcohol will appear as oily currents schlieren patterns cooling usually takes place within the chamber especially forwards the onset of PURGE near the exhaust orifice of e The intermediate fluid will appear as a liquid or a slurry when exiting through the ee gt 7 clear PURGE Exhaust hose Once thoroughly exchanged the chamber liquid will be will form at 79 C and Secuencia turds The Purge rate is manually adjustable with the PURGE VENT valve and should be set by such as pure ethanol have the operator to allow for a steady flushing of transitional fluid without letting the liquid level
27. laboratory and after careful reading of the MSDS 2008 tousimis LCO is shipped to your laboratory by your local distributor in steel cylinders Please note the tare weight and gross weight You can only use about 50 of the net LCO since the dip tube does not reach the bottom of the tank Advise your supplier to never wash the empty steel cylinder with water or leave it in the yard to accumulate pollutants ALWAYS KEEP SPARE FULL TANK IN RESERVE AT ROOM TEMPERATURE As you receive the LCO it is under pressure at 20 C 750 to 900 psi While CO is a respiratory stimulant humans cannot breathe air containing more than 10 carbon dioxide at this level one could faint Use the SAMDRI PVT 3D in a well ventilated room or exhaust all CO into a working hood exhaust conduit or the outdoors Please consult your laboratory regulations for exhaust requirements Usually one to two pounds of LCO are used for each process run The critical temperature and pressure of pure CO are 31 3 C 88 84 F and 72 9 atm 1072 psi respectively SAMPLE PREPARATION BEFORE SAMDRI ING It is not the intention of this manual to present an extensive review of sample preparation techniques Certain samples present special problems in preparation and it is the responsibility of the investigator to determine the best procedures in each case It is the general object of pre critical point drying preparation steps to yield a sample in which the histologic
28. lter Replacement Instruction 1 Repeat Step 1 7 of previous section Chamber Lamp Replacement Installation in order to remove access panel 2 Locate the Purge Line Filter 8770 83 as indicated below Note the Purge flow direction 0 5um Particulate Purge Line Filter 8770 83 7 6 Coupler Purge Line Filter 8770 83 Page 36 2008 tousimis Purge Line Filter Replacement Instruction gt Flow Direction Purge Line Filter 0 5 pm 8770 83 3 Disconnect Purge Line Filter by carefully holding Purge Line Filter steady with 9 16 Open end wrench while disconnecting both 7 16 couplers Carefully remove old Purge Line Filter and discard SN 7 6 Wrench 4 7 6 Wrench 9 16 Wrench 9 16 Wrench 4 Install new Purge Line Filter paying attention to flow direction Please note flow direction on the Purge Valve MUST be installed in line with flow direction indicated in previous SAMDRI PVT 3D Chamber Plumbing picture eT Hee 5 Re install access panel Re connect power and all connection hose s prior to starting up the Purge Line Filter be System replaced every 6 months with regular use Change more frequently with heavy use Please contact techsupport tousimis com with any questions 2008 tousimis Page 37 Appendix C Installing SAMDRI PVT 3D with SOTER Condenser This section is for Installing SAMDRI PVT 3D with optional SOTER Conden
29. nl Flow M AN ERLENMEYER FLASK LILY INS LALO AVES RE 6ft 180cm OR SOLVENT DRAIN measure flow at onset of BLEED mode only 6ft 180cm PURGE VENT EXHAUST HOSE CLEAR TUBING 6ft VENT TO HOOD EXHAUST CONDUIT OR OUTSIDE FLOW METER USED TO CALIBRATE FLOW AT ONSET COOL BLEED EXHAUST HOSE OF THE BLEED CYCLE SET WHITE TUBING 6ft FLOW RATE to 8 10 SCFH 2008 tousimis Page 21 CHAPTER 7 Maintenance and Support Page 22 Regular Maintenance Schedule Maintenance Activi Recommended j Manual trc Catalog D Frequency Reference Number Keep Chamber Clean and Dry Always p 23 N A 0 Replace CO tank After 50 net Contact local tank consumption supplier Replace LCO Oil Water Filter in LCO Filter Assembly 5001b LCO Use 8784A Replace T Filter Element in LCO Filter Assembly 8770 83B Chamber O Ring 3 Months 8770 51 Internal Purge Line 0 5m Filter 6 Months 8770 83 May Vary Depending on Usage 2008 tousimis Chamber Care Maintenance and Support NOTE Use Ultrapure Alcohols only i e I PA Methanol Ethanol Use minimum 99 5 purity Alcohols for best results NOTE Do not expose chamber to HF or any other Acids Do not use Acetone Please consult tousimis before using any non recommended intermediate fluids or process any non traditional CPD application material s NOTE BE SURE TO KEEP CHAMBER O RING GROVE AND FACE CLEAN AND D
30. nment After coating samples diffuse into the dried should be maintained in a dry environment to prevent changes as a result of water absorption sample or possible cracking of the coating layer Page 16 2008 tousimis CHAPTER 5 Theory of Critical Point Drying 2008 tousimis THE SAMDRI PVT 3D The tousimis SAMDRI PVT 3D is a critical point drying apparatus which through a series of stages the sample is processed by a technique which preserves and stabilizes the delicate 3 D morphology without freezing rigid chemical fixation which alters the ultra structure embedding paraffin plastics epoxies etc PRESERVATION OF DELICATE ULTRASTRUCTURE Sample Drying SAMDRI at the Critical Point In order to preserve 3 D structure one must avoid the sudden air drying change of densities that occurs when the fluid embedding the sample and permeating its ultrastructure is converted to gas Most liquids used to replace water in samples have a well defined critical point a specific pressure and temperature at constant volume for each of them At the critical point the densities of the gas and liquid phases of the transitional fluid are equal therefore a phase boundary does not exist After the critical point transition from the liquid to vapor phase has taken place the vapor phase can be removed while above atmospheric pressure and the dried sample preserved without structural damages due to surface tension forces
31. nnect 6 High Pressure Hose Connect 5 Inlet Outlet Setting 7 Metering Valve w Vernier Handle Setting Example 21 Power Connection 4 Setup Overview 3 39 Venting Precautions 20 SAMDRI PVT 3D Operation BLEED Valve Adjust 11 COOL Valve Adjust 9 FILL Valve Adjust 9 PURGE VENT Valve Adjust 10 Turning HEAT ON OFF 10 Turning Power ON OFF 8 Typical Drying Cycle 16 SAMDRI PVT 3D with SOTER Condenser Chamber LCO2 Supply Connect 44 Condenser Drain 42 Condenser Exhaust Connect 42 Drain Valve 49 Exhaust Connect Line Exhaust amp Condenser Vent Insulate 40 High Pressure Hose Connect 44 Inlet Outlet Connect 40 45 Over View 43 45 47 Power Switch 49 Secure Chamber 48 SOTER Condenser Connect 41 Power Strip Connect 46 Typical Chamber Temperature during Pressure Reduction BLEED 15 Typical Paths that Critical Point Passage May Follow during Heat Phase 14 Typical Range of Paths that Pressure Reduction May Follow in the SAMDRI PVT 3D 15 Page 50 2008 tousimis User s Note 2008 tousimis Page 51 User s Note a Page 52 2008 tousimis
32. not needed between the LCO tank and the 3D The 3D is designed to simply operate from LCO direct tank pressure Is the chamber necessary to heat during BLEED mode YES During the BLEED mode the HEAT switch should be kept ON The HEAT mode will maintain chamber temperature automatically above 31 C and keep the process chamber dry How do I replace the 8784A filter elements To replace 8784A filter element loosen and remove lower part B by turning counter clockwise Remove old element and replace with new See illustration p 24 25 How do I secure the chamber lid Evenly finger tighten the chamber lid with the 3 Knurled Nuts Use even and steady finger pressure on all Knurl Nuts alternatively Never use a non compatible tool or excessive force i e never use a wrench etc Should I use High Pressure Head tanks such as Helium or other high pressure gases NO Never use high pressure tanks Typical proper pressure range for LCO tanks are between 750 900 psi Higher pressures may damage SAMDRI PVT 3D and or cause failures Can I use lower purity alcohol or acid in chamber NO ONLY USE ULTRA PURE ALCOHOL ETHANOL METHANOL I PA etc IN CHAMBER NEVER ANY ACID CONTACT TOUSIMIS PRIOR TO USING ANY OTHER INTERMEDIATE LIQUIDS Is a siphon or dip tube type LCO tank necessary YES It is essential that the LCO tank has a siphon or dip tube on order to deliver liquid and not gaseous CO The SAMDRI PVT 3D
33. ose directly to the CGA 320 threaded male coupling at the tank top See p 24 ALL LCO tanks should be equipped with a rupture disc All LCO fittings and gasket surfaces should be kept clean and dry NEVER OVER TIGHTEN FITTINGS TUBING ATTACHED MAY BE DAMAGED Monitor the LCO tank weight via a LCO Tank Scale 8770 54 Connecting High Pressure Hose to SAMDRI PVT 3D 4 Attach the HIGH PRESSURE HOSE onto the LCO CONNECT INLET Gently tighten the High Pressure Female Connector using the two open end wrenches supplied one on the hose and the other on the Inlet Stop at the feel of first resistance re tighten if necessary should you hear a leak High Pressure To attach LCO high pressure hose end fitting to the PVI 3D LCO Connect use the supplied 9 16 and a 1 2 open end wrenches First slide 1 2 wrench over 1 2 fitting as shown in the LCO2 CONNECT photo The 1 2 wrench will INLET be used to hold the LCO Connect Assembly steady as you gently tighten the high pressure hose end fitting snugly onto each of the flare connects with a 9 16 wrench DO NOT OVER TIGHTEN 9 16 open end wrench NO TEFLON _ TAPE NECESSARY 2008 tousimis Chapter 2 5 The tousimis LCO Filter Assembly catalog 8784 is factory installed directly onto the high pressure hose See p 24 25 This helps prevent sample contamination from oil water and particulates Change the Oil Water Filter Element
34. partment 2211 Lewis Avenue Rockville Maryland 20851 USA Telephone 301 881 2450 Fax 301 881 5374 Email techsupport tousimis com REPACKAGING FOR SHIPMENT After authorization for repairs is received see warranty this general rule may be followed in repackaging a tousimis instrument for shipment a Attach identification tag to instrument Tag should indicate owner name the model and 4 digit serial number of the instrument and the type of the service or repair desired b Secure chamber lid over a properly seated O ring and tighten 8 knurl nuts evenly Do not send the high pressure hose or electrical power cord c Place instrument in original container if available If original container and packaging material is not available new packaging may be purchased from tousimis If original container is not used d Wrap the instrument in bubble plastic e Protect panel faces and instrument sides with foam or appropriate non abrasive cushioning material Use a minimum 6 of shock absorbing packing material around all points of the instrument Two double walled boxes are suggested for shipment BOX WITHIN A BOX AT 350LBS TEST STRENGTH f Use heavy duty shipping tape or metal bands to seal container g Mark shipping container with Delicate Instrument Fragile etc and insure it Page 31 APPENDIX A Chamber Lamp Replacement Installation 1 Turn the power switch OFF and unplug 120V power cord from the SAMD
35. ppendix C p 38 to Install SAMDRI PVT 3D with optional SOTER Condenser 8777 Upon receipt of your SAMDRI PVT 3D unpack the instrument carefully and check for any damage that may have occurred during shipment Report by Email trc tousimis com or Fax 301 881 5374 any irregularities immediately to tousimis Insist on clean surfaces Minimum table top space of approximately 20 51cm Width x 30 76cm Depth should be allotted for the SAMDRI PVT 3D with an additional 12 31cm x 12 31cm of floor space for the LCO tank scale See p 3 e Use bone dry min 99 8 Purity LCO with a syphon dip tube tank only e Do not use pressurized LCO with Helium or any other high pressure substitute gas e Properly secure LCO tank according to your facility s safety protocol BOC gas suppliers refer Tank pressure typically reads 800psi 5 at room temperature The amount of LCO in to 99 8 purity grade as tank is best monitored with a LCO tank scale See accessories p 30 2 8 grade e Always order LCO Typical nominal LCO tank weights for Net 50lb LCO tanks tanks with Siphon or dip abes e Full tank 140 to 170 lbs Tare of tank 90 to 120 lbs e Most of the time you may use 50 of a 501b net weight CO tank e Air Products gas i i 5 e It is good practice to have spare LCO tanks stored in reserve in case a tank runs suppliers refer to 99 8 purity grade as CP grade out during mid p
36. r to BE SURE TO KEEP CHAMBER O RING GROVE AND FACE HF or any other Acids CLEAN AND DRY AT ALL TIMES Do not use Acetone Please consult tousimis before using any non recommended intermediate fluids or process any non traditional CPD application material s 2008 tousimis Page 7 CHAPTER 3 Operating SAMDRI PVT 3D Turning Power ON OFF POWER OFF POWER ON NOTE Pressure measurement is no indication of the amount of LCO left in the tank The same PSI reading may be noted even after the liquid CO drops below the level of the siphon tube NOTE Use Ultrapure Alcohols only i e I PA Methanol Ethanol Use minimum 99 5 purity Alcohols for best results Page 8 1 Turn power ON Power light and chamber light will illuminate Allow SAMDRI PVT 3D to warm up for 3 minutes prior to use This allows time for the internal valve heaters to equilibriate 2 Make certain all metering valves FILL COOL BLEED PURGE VENT are in the closed position hand tight Open the main LCO tank valve The Siphon dip tube LCO tank should have between 25 lbs 50 lbs 13 6 kg 23 kg net weight of LCO Subtract the tare weight of the tank from the tank weight to get the net weight of LCO 3 Sample should be dehydrated completely in high purity 99 5 minimum purity alcohol Pour enough high purity alcohol in the SAMDRI chamber to completely cover your sample s prior to transfer Now
37. rocess e Minimum LCO purity A properly grounded 120V 50 60Hz outlet or Transformer Step up Step Down should be required is 99 8 located within 4ft 1 2 m of install site POWER Connection to SAMDRI PVT 3D AC BLACK COLD 120V GROUNDED OUTLET ONLY GROUND 120AC 60HZ Ac WHITE HOT Page 4 2008 Stousimis Installing SAMDRI PVT 3D INSTALLATION OF THE SAMDRI PVT 3D This SAMDRI PVT 3D is supplied with the basic accessories for operation with LCO as a transitional fluid for optional accessories see p 30 1 Install SAMDRI within 4 feet 1 2m of a properly grounded 120V 50 60Hz electrical LCO tanks used in Stet most facilities have tare weights ranging from 90 2 Position a LCO tank with dip tube within 5 feet 1 5m of the SAMDRI PVT 3D For a 120lbs 40 55kg and are longer high pressure hose length see p 30 trc 8770 33 The LCO tank should be delivered as full with net mounted on a 400lb 182kg capacity floor scale w remote LCD display tre 8770 54 to 50lbs 23kg of easily monitor LCO supply compressed CO 3 Pressure gauges or regulators should not be installed between the LCO supply tank and the Generally 50 of the net SAMDRI PVT 3D LCO Connect Inlet The stainless steel sheathed high pressure hose LCO is useable accompanying the SAMDRI is fitted with a CGA 320 female hex coupling which accepts a 3 4 plastic gasket supplied and joins the h
38. ser 8777 See Chapter 2 p 4 for installing without SOTER Condenser BOC gas suppliers refer to 99 8 purity grade as 2 8 grade Air Products gas suppliers refer to 99 8 purity grade as CP grade Always order LCO tanks with Syphon aka dip tubes Minimum LCO purity required is 99 8 LCO tanks used in most facilities have tare weights ranging from 90 120lbs 40 55kg and are delivered as full with net 50lbs 23kg of compressed LCO GENERALLY 50 IS USEABLE You are advised to monitor the tank weight Page 38 C PREPARATION OF INSTALLATION SITE Upon receipt of your SAMDRI PVT 3D unpack the instrument carefully and check for any damage that may have occurred during shipment Report by Email trc tousimis com or Fax 301 881 5374 any irregularities immediately to tousimis Insist on clean surfaces Minimum table top space of approximately 36 92cm Width x 30 76cm Depth should be allotted for the SAMDRI PVT 3D and optional SOTER Condenser with an additional 12 31cm x 12 31cm of floor space for the LCO tank scale See p 3 Use bone dry LCO with a syphon dip tube tank only Do not use pressurized LCO with Helium or any other high pressure substitute gas Secure LCO tank according to your facility s safety protocol Tank pressure typically reads 800psi 45 at room temperature The amount of LCO in tank is best monitored with a LCO tank scale See ac
39. sures 4 5 dia x 6mm ht 8764 4 Sample Holder each compartment measures 9 dia x 16mm ht 8766 Cover Slip Holder for 9mm to 13mm diameter Glass Cover Slips 8766 01 Washer for Glass Slip Holder for use with 8766 8766 02 Stainless Steel Screens for Cover Slip Holder for use with 8766 8767 Cover Slip Holder for 16mm to 22mm diameter Glass Cover Slips 8767 01 Washer for Glass Slip Holder for use with 8767 8767 02 Stainless Steel Screens for Cover Slip Holder for use with 8767 Contact tousimis 301 881 2450 or trc tousimis com for current pricing and availability or visit our web site at www tousimis com Page 30 2008 tousimis 2008 tousimis Maintenance and Support WARRANTY The SAMDRI PVT 3D is warranted to the original purchaser for two years from date of purchase against any defect in materials or workmanship Should you have any questions please feel free to contact us If it is determined that the unit should be returned for repairs to our Service Department we will send a written authorization for shipment Parts and labor are free of charge shipping charges are to be paid by customer insure instrument at current list price DO NOT ship instrument via U S Mail Use UPS FedEx or other qualified shippers only Our mailing address tousimis research corporation 2211 Lewis Avenue Rockville Maryland 20851 USA Our shipping address tousimis research corporation Attention Instrument Service De
40. ting under vacuum and subsequent study in the SEM TEM or electron probe X ray microanalyzer Isothermal of Carbon Dioxide and an Average Drying Path of Sample in the SAMDRI PVT 3D N Q w or D T 0 Li or a a Critical Point BEGIN END DENSITY CO2 g cm Sample in After 35 minutes intermediate fluid average time ethanol or methanol Dried sample now is in for non bio samples air at room temperature at room temperature ang atmospheric ae ia ala pressure Transfer to pressure moisture free container TRANSITIONAL FLUID Liquid Carbon Dioxide LCO is the preferred transitional fluid in critical point drying since it is easily accessible more economical less noxious safe in a well ventilated laboratory and provides more consistent results than any other transitional fluid Only research grade or filtered see tousimis combination filter catalog 8784 bone dry LCO should be used Use of LCO requires a dip or Siphon tube in the CO cylinder tank which provides liquid at the tank outlet for the first 25 30 lbs Tanks should be kept at room temperature for at least 2 3 days prior to use Page 18 2008 tousimis Theory of Critical Point Drying High purity or ultra pure fixatives are recommended see tousimis CAT 1008 and 1011 Acrolein is a very hazardous chemical Avoid its use unless there is no other alternative and then use as per special instructions in your
41. ulated during Critical Point Passage YES Chamber pressure will rise above 1072psi Critical Pressure for CO and automatically vent internally at 1350psi 5 20 C Is chamber temperature automatically regulated during Critical Point Passage YES Temperature is maintained between 31 C 42 C automatically with HEAT switch ON Is there back up pressure Safety YES In addition to automatic internal pressure venting above the Critical Point There is a rupture disk which automatically vents entire system at 2000psi What grade LCO is best for the SAMDRI PVT 3D 99 8 minimum purity May I replace or add parts without authorization from tousimis NO SAMDRI PVT 3D is a high pressure instrument with specific tolerances engineered into the design Please contact tousimis for authorization prior to attempting any desired changes What should I do if the initial COOL time is suddenly much slower than normal 99 of the time the reason for this is lack of Liquid CO The SAMDRI is designed to COOL the process chamber via Liquid CO and not gaseous CO Reasons that typically explain gaseous CO delivery 1 The Liquid CO level has dropped below LCO tank siphon aka dip tube and only gaseous CO is being delivered Note The best way to monitor LCO is via weight and not pressure It is best to monitor tank weight via a LCO tank scale trc 8770 54 2 Gas supplier has delivered Gaseous rather than Liquid CO b
42. will not operate properly without liquid CO Page 27 Chapter 7 Why can I only use 50 of the net amount of LCO and not 100 of the net LCO within a new LCO tank LCO is lost during the process for 2 reasons 1 As the liquid level drops in the LCO tank the gaseous head space created as the liquid level drops is taken up via gaseous CO molecules 2 Siphon aka dip tubes does not reach the absolute bottom of the LCO tank What can I do to check that the BLEED rate is properly set should it appear unusually slow The flow rate should read 8 10 SCFH at the onset of the BLEED cycle This setting should yield at average of approximately 100 150 psi min reduction in pressure This pressure reduction flow rate is the desired decompression rate between 1300 400 psi to avoid condensation You may periodically measure the BLEED rate if desired via the Flow Meter supplied by attaching the Flow Meter to the COOL BLEED CO Exhaust Outlet via a short approximately 2 piece of Tygon tubing What is the average FILL Time The FILL time should not exceed more than 2 minutes Typically the chamber will FILL in less than 1 minute What is the average PURGE time The PURGE time will vary according to the volume of ethanol in the chamber It takes approximately 7 minutes to purge 50 of the chamber volume 10 15ml Alcohol Page 28 2008 tousimis Maintenance and Support Is chamber pressure automatically reg
43. y mistake This can happen as the 2 tank types may look identical and the delivery loading Gas Company staff accidentally delivered the wrong tank type to your site The simpler solution is to replace the existing supply tank with a new LCO tank and initiate COOL mode If the same problem persists please contact customer service at either techsupport tousimis com or via tel 301 881 2450 2008 tousimis Page 29 Chapter 7 OPTIONAL ACCESSORIES Catalog Description 8777 SOTER CONDENSER 8760 01 Knurl Nut 8760 40 5 AMP Fuse 8770 10 Lamp 120V 60Hz volt 8770 32 High Pressure Hose 5 ft 8770 33 High Pressure Hose 10 ft 8770 HPS High Pressure Hose Custom Length Up To 10m 33ft 8770 45 Flow Meter Use with any 1 25 dia Samdri Chamber 20 SCFH 8770 50 Chamber Lid 8784 LCO2 Filter Housing for 8784A Filter Element 8784A Replacement LCO2 Filter Element for 8784 Filter Housing 8784B O Ring for 8784 Filter Housing Seal 8784 05 Gasket for LCO2 Tank Connect 8770 83 Internal 0 5m Brass Particulate Line Filter 8770 51 O Ring for 1 25 Diameter Autosamdri Chamber 8770 53 Power Cable three prong 120V 60Hz 8770 54 LCO2 Tank Scale w Remote LCD Display 4001b capacity 8770 55 LCO2 Tank Heater 8770 56 Step Down Transformer 220V 110V 8770 57 Step Up Transformer 100V 120V 50 60hz 8761 Grid Holder holds 12 grids 8762 12 Sample Holder each compartment measures 7 5 dia x 6mm ht 8763 24 Sample Holder each compartment mea
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