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The Genevac HT- 4 & HT- 4X Series II Evaporation Systems User

1. Run Ho Run Data Locked Hext Run Number CH for nonel Run Hane Solvent Sanple Holder Type Sample Volume Deep Hel 7 Last Used Hot yet used Last Changed LHeu entry SAHPLE HOLDER Select Sample Holder Hicrotitre Plate Plate Tube Yial Holder SanpleGuard Control Temperature C C SanpleGuard Control Channel CoolHeat Enable Pressure mbar Hininum Chamber Temperature C Rotor Speed Heat Off Option Heat Off Elapsed Time CHH HH End af Run Option End of Run Elapsed Time CHH HH Pressure Control Regine Dri Pure Final Controlled Pressure nbarl GENEVAC LTD High Elapsed Tine HH HH Elapsed Tine HH HH Dr i Pure B HELP Tl to select ENTER to accept ESC to cancel Sanple holder type to be entered Select a sample holder type from the window that opens If the required sample holder option is not available select other and enter the details no more than 31 characters Enter a value for the volume of sample in each individual well tube vial 91 Last Used Hot yet used Locked Humber CH for nonel Run Ho Run Data Hext Run Run Hane Sample Holder Type Sanple Un lune Chloroform t DCH DHF DHI DHSO SanpleGuard Control Temperature L C l SanpleGuard Control Channel CoolHeat Enable Pressure mbar Hininun Chamber Temperature C Rotor Speed Hexane Hex SOLVENT Acetonitrile
2. Integral Swing Tube Holder Tube Holder and Side Bridge Swing Sample holders requiring a separate swing or bucket may also be used Each of these swing types lifts straight out of the rotor The ideal swing type depends on the sample holder required A large range of sample holders is available Load the tubes vials beakers or flasks into the sample holders then place the sample holders in the swings Page 10 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Use of Correct Accessories Genevac supply a wide range of sample holders to cover a variety of plate tube vial or flask formats Where no holder is available custom units can be made To ensure that bespoke holders are suitable and approved for use new sample holders may be designed in collaboration with the Genevac R amp D department Criteria for approval Mass within prescribed maximum limit Matched sample holder mass within a set Correct centre of gravity Good thermal conductivity Correct hole form and size tolerance to reduce risk of tube or vial breakage under centrifugal acceleration All Genevac holders are designed with these constraints in mind 3 party accessories may not be With the exception of microtitre plates do not load any non Genevac holders into a system without gaining approval from Genevac Failure to comply may result in unrecoverable loss of samples severe damage to equipment and inval
3. Please contact your local Genevac representative for further details on run times alternatively please e mail Applications Genevac com 10 1450 Issue 3 2 January 2009 Page 51 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Programming Guides The programming guides on the following pages show examples of run profiles for some common applications Drying HPLC Fractions I Dning HPLC Fractions Run Data Locked NINN Next RunNumbr 2 RunName Fractions Fractionspart2 Fractionspat MeCN or MeOH amp MeCN or MeOH 8 MeCN or MeOH amp SampleGuard Control TempC 40 40 SampleGuardControlChannel t tO boo CoolHeat Enable Pressure 5050 V RN P RN Heat Off Elapsed Time jaskforime 0100 0800 End of Run Option Elapsed Time Elapsed Time End of Run Elapsed Time askfortime 01 00 03 00 Auto Defrost amp Drain Pressure Control T pumsr arra ohmy NR Dri Pure ERES Pressure Vacuum Dri Pure Start Pressure Dri Pure Start Pressure mbar 4750 40 for MeCN Dri Pure End Pressure cere UT UE NM NM for MeOH Dri Pure Dri Pure Ramp Time Time Final Control Pressure 40 E up MeCN 45 for MeOH Notes Remove organic Remove most of the Remove final phase aqueous phase stubborn solvents Page 52 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Fast Lyophilisation of HPLC Fractions MEE dams HPLC Fractions Run Da
4. C E E m m m 150 Issue 3 2 January 2009 Page 29 of 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Select one of the following options for End of Run and or Heat Off Elapsed Time Enter independent times for heat off and for end of run The evaporator turns off the IR lamps when the heat off time elapses and allows the system to run without heat input until the end of run time elaspes This feature enables the protection of thermally sensitive samples as they approach dryness while ensuring that all samples are dried completely Heat Flow The system monitors the rate of evaporation by looking at the demand for heat input that is required to maintain the SampleGuard control temperature When sample dryness is detected the system turns off the IR lamps and allows a final drying stage before stopping the run Sample Detection The evaporator monitors the sample temperature t detects dryness when evaporative cooling ceases turns off the IR lamps and then stops the run Note Two temperature probes are required for Sample Detection See Using the SampleGuard for details Note Evaporators with IR temperature control have no sample guard transmitter and do not offer the Sample Detection option for of end of run detection Set the IR Control Temperature in the same way as the SampleGuard Control Temperature End of Run Defrost and Drain Select yes to defrost and drain condenser at the end of the stage See th
5. DMSO or DMF amp DMSO or DMF amp DCM DCM DCM SampleGuard Control Temp C40 Mo Ci oO SampleGuard Control Channel 40 1 1 CoolHeat Enable Pressure 90 Chamber Temperature control preheat to 15 preheat to 40 preheat to 30 Rotor Speed a Heat Off Elapsed Time askfortime 0000 End of Run Option ElapsedTime ElapsedTime End of Run Elapsed Time askfortme 0100 o a Auto Defrost amp Drain 40 1 50 Pressure Control Regime Variable Dri Pure Full Vacuum Full Vacuum Dri Pure Start Pressure mbar T 50 Dri Pure End Pressure mbar TO Dri Pure Ramp Time E E Notes Remove MeCN Dry high BP solvent Final Drying Page 54 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Technical Data Mechanical data 1 Condenser Max rotor speed 1300 standard Temperature max low 45 C HT4 SII 1800 Dri Pure 50 C HT4X SII Max force 300 500G Temperature max high 60 C Drive system Direct Vacuum pot capacity 1 5 litres HT4 SII Operational imbalance 85g 2 3 litres HT4X SII Max load 4x1 5kg 500G Exhaust pot capacity 0 4 litres IR lamps number 2 Condenser level No Weight 109 kg HT4 SII detector 316 Stainless steel 118 kg HT4X SII Condenser chamber Stainless steel PTFE Condenser drain valve Vacuum System Vacuum Pump Scrol Pressure resolution 1 1000 mbar Weight 28kg Vacuum control 1 1000 mbar Maximum vac
6. Do not exceed the mass limit under any circumstances n most cases with normal solvent volumes sample holders sold by Genevac fall within the mass limit for a series Il system If in any doubt load up a full swing and weigh it 10 1450 Issue 3 2 January 2009 Page 11 of 58 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Safe Loading of Sample Holders into Swings and series Il equipment is used in the same This information is applicable where Series 1 laboratory There are two possible ways in which a sample holder may be miss loaded into an older type of swing One is to rotate the sample holder such that its corners rest on the edges of the swing The other is to place the sample holder so that one side rests on the edge of the swing ne Sample Holder rotated Both these modes of miss loading are possible with a Series 1 open or standard swing but are virtually impossible with a Series l swing Care must still be taken when loading the samples T k Dale Lame a cu ees p Sample Holder correctly seated The Series 1 design is easy to distinguish The corners are not welded MAX MASS FOR SERIES 1 900g An q le 5 ui ANGLE x Sample Holder on edge of swing vc Corner welded The Series Il swing has angled sides and rounded corners that are welded Genevac offer an option to upgrade to the new range of sample holders and swings This upgrade perman
7. Solvents 155 C BP solvents Med BP amp 40 DMF amp DCM Mixtures of medium and volatile solvents Volatile 155 C K Methylene Chloride with high risk of bumping oo Pre heat No solvents should Rapid pre heat of chamber before a high Chamber for be present BP solvent run swings and samples must be removed before this method is used solvents High BP 140 140 DMF DMAc DMSO High BP solvents 190 C Very High BP 190 C NMP DMI Very high BP solvents Solvents HPLC Fractions Water amp Acetonitrile HPLC fractions or Methanol 5 pea only 100 C EM pe only Any Drying samples which have not been fully stubborn dried using another method The solvents condenser must be empty before this method is used 52 53 54 56 57 58 59 Page 38 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Getting the Best from the System Routine Checks For high boiling point solvents such as DMSO NMP DMF and DMI the best evaporation rates are achieved at pressures better than 0 5 mbar Carry out the following checks regularly to ensure optimum vacuum performance Check security of all clamped joints Drain the condenser pots before every run Check the pump exhaust catch pot regularly and drain as necessary Keep a log of the time taken for your system to reach full vacuum and use it to indicate deterioration of performance due to seal ageing and wear Tips for Improving System Per
8. 1 05 20 N Ammonium Hydroxide NH3OH 0 90 20 Y Chloroform TCM 1 48 20 a Dichloromethane DCM 1 33 20 Y eee m 0 94 Y pmehyemn OMA J 09 23 N x Pre 09 0235 T s er ia n Ethane OH amp S 23 Y Eth Acetate Ee eg mi 009 0 o HS Mehano MG 0 23 Y MMenyzpymldon NW 10 25 vo Bride o 09 29 MN Tetrehyerofuran THE os o v Toluene Pe Q8 29 Y WemmegE o a Y Water 1e m A E HCl Thionyl Chloride or Di Ethyl Ether compatibilities are not available lt lt lt Zz lt lt lt z lt lt lt lt x Genevac and the ATEX Directive Please note that it remains the responsibility of the user to consider any solvents being evaporated within the context of the ATEX directive The presence of solvents on the list above indicates only that they will not damage the system If further information is required please contact your Sales Representative or visit http www genevac com Those solvents with a Y in the Autoprogram Available column are available from the Solvent drop down list when setting up a run The solvents with an N against them must be entered using the Other option and the rest of the data entered manually 10 1450 Issue 3 2 January 2009 Page 15 of 58 Genevac HT 4 8 HT 4X Series I
9. 1l ml 44 15 4 5 Oligo Production Aqueous Hixture dnl 58 nl T 4H H GENEVAC LTD START EDIT GRAPH CLEAR COPY TO DRAIN MDEFRUS T FLUSH OPTIONS HELP Select Run with T1 Henu Item with keys press START to execute Starts selected Run using paraneters stored E Press the Settings key to enter the Run Data screen see the section entitled Run Data Screen for details START Press the START key to execute the highlighted option Note the Run Log screen is shown when the run starts Press the cursor direction left and right keys to highlight the options on the horizontal menu bar near the bottom of the screen Press the up and down keys move the white band cursor Note The default position for the horizontal menu bar cursor is with START highlighted Press the cursor direction left and right keys to return the cursor to START after using any of the other menu options 10 1450 Issue 3 2 January 2009 Page 23 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Functions of the Menu Bar e START Starts the highlighted run e EDIT Alternative route to the Run Data screen e GRAPH Alternative route to the graph displayed by the display key e CLEAR Clears the highlighted run profile e COPY TO The highlighted run profile may be copied to a different location This feature is useful if several similar run profiles need to be created Copy and edit a profile instead of creating each one from scratch
10. Heat Off Option HHP Heat Off Elapsed Time CHH H TFA End nf Run Option THF End of Run Elapsed Time CHH HH Toluene PhHe Hater H20 Pressure Control Regine Other Dri Pure Final Controlled Pressure nbarl C lear Done GENEVAC LTD HELP TL ENTER to select deselect select Done when finished ESC to cancel EtfAc Hex Select Yes to allow the evaporator to set the remaining run parameters or No to continue entering the remaining parameter field manually Run Ho 91 Last Used 14 47 14 07 03 Last Changed 14 47 14707703 Run Data Protection No Next Hun Number G for none a Hun Mame Example sample Holder Type Deep Well Plate sample Volume ml 0 7 350 lvent Et c Hex SampleGuard Control Temperature C 4G sampleGuard Control Channel 1 CoolHeat Enable Pressure mbar 200 Chamber Temperature Control C AUTO Cool to 32 Control at 260 Rotor Speed Low Heat Off Option Heat Flow Heat Off Threshold Not Applicable End of Run Option Not Applicable End of Run Threshold Not Applicable End of Run Defrost and Drain Yes Pressure Control Regime Controlled Pressure Controlled Pressure mbar 9 5 GENEVAC LTD HELP Tl to select ENTER to edit MENUYESC to exit Temperature to maintain using SampleGuard The screen shows the automatically programmed run parameters in blue These parameters may be overwritten manually Manually overwritten parameters are shown in white Note There are a couple of restrictions to be
11. It may be possible to concentrate more water at this stage for very large or water heavy fractions please contact Genevac for advice Freeze all the samples using high vacuum Run the system at Full vacuum with no heat for 1 hour Lyophilise the samples to dryness using heat if possible to speed up the process Run the system at full vacuum trial and error will determine the length of time that Lyophilisation takes Please contact your local Genevac representative for further details on run times alternatively please e mail Applications Genevac com Notes on Lyophilisation Some experimentation is required to set up a new fast lyophilisation method Several trials are required optimise the method and produce a fully functioning process Genevac are able to provide remote assistance by analysing evaporation data collected using the Genevac Data Logging Software An adjacent laptop or PC is required to collect this data Use both sample guard probes place probe 1 in the sample holder to control the temperature place probe 2 in a central sample to monitor the process This is essential during method development It indicates when the sample freezes and when the lyophilisation process ends Fill all positions of the sample holders when performing lyophilisation samples in partially filled holders may not freeze Do not use this method to attempt lyophilisation of samples that are grossly insoluble in water These samples crash out once the orga
12. Pump Page 6 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Identifying the Parts Condenser Vacuum Inlet Control Cable Socket Condenser Exhaust Inlet HT4X SII HT4 SII Early build HT4X SII Pump Vacuum Inlet Catch Pot Assembly r E Pump Control Cable Socket Pump Control Box Pump Exhaust Outlet Mains Power Connector System Exhaust Outlet Chamber Drain Outlet LyoSpeed System Condenser Drain Manifold with Single Drain Pipe Condenser Drain Outlet Exhaust Drain Outlet 10 1450 Issue 3 2 January 2009 Page 7 of 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Installing the Stystem These instructions refer to the installation of an HT4X SII evaporator with a scroll pump Details follow to show differences that may be encountered on different build variants Note he power to the evaporator is delivered via the pump control cable Fit the pump control box to the scroll pump using the connectors clamps and fasteners supplied Fit the pump exhaust outlet and catch pot assembly to the pump Place the evaporator and scroll pump in their intended location Ensure there is enough space above the evaporator for the lid to open Connect the 16KF convoluted vacuum tube to the pump vacuum inlet via a 16KF to 25KF reducer appropriate clamps and centre rings Connect the other end of the convoluted vacuum tube to the condenser vacuum inlet on the bac
13. bench of fume cupboard space to accommodate the system at the new location Ensure there is access to a power supply two separate mains sockets are required Ensure there is adequate ventilation Make provision for the drainage of waste solvents Make provision for the extraction of the pump exhaust Defrost and drain and if possible flush the condenser pots Remove the sample swings from the rotor Remove and retain all the clamps seals tubes cables and instructions 10 1450 Issue 3 2 January 2009 Page 45 of 58 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Additional Equipment Genevac supply a range of swings and sample holders which may be utilised to adapt existing systems for new applications All sample holders are of a solid aluminium construction and are black anodised to improve heat absorption Solid aluminium tube holders provide even heat distribution for uneven drying loads Maximum contact areas provide good physical support optimum heat transfer and even heat distribution The following accessories are an example of the many ways in which Genevac can assist in developing your system for the future For further information or to discuss any requirements please call Genevac Sales using the contact details on the back cover of this User Manual Side Bridge FastStack for shallow well plates FastStack for deep well plates Flask holder One piece holder for 50mlTubes Sample Genie Page 46
14. end the defrost cycle Alternatively Dage 32 ARN leara 2 2 P DONO Page 32 of 450 Issue 3 2 January 2009 Enter the Select Run screen and press the STOP key SELECT RUN Ho Mame anluent Vol Holder T HMxt 91 Example Eth c Hex iml Deep We 40 O0 92 93 PURIFICATION WATERSACETONITRILE 10ml 18 X 15 94 SOLID PHASE SYNTH TFASDCH eml DEEP WE 95 COMPOUND f CONFIRM REQUEST 96 OLIGO STH Shut down evaporator Are you sure CYH 97 SOLUTION 98 SOLUTION PHASE 2 DCHNME THANOL iml DEEP WE 99 MAINTENANCE TEST 1 ml MAINTENANCE TEST 2 ml GENEVAC LTD MEMU SSB EDIT GRAPH CLEAR COPY TO DRAIN DEFROST FLUSH OPTIONS HELP select Run with Tl Menu Item with gt keys press START to execute Starts selected Run using parameters stored Select Y to shut down the evaporator The evaporator continues to purge the vacuum pump for a time period indicated on the screen Press the START key at any time to restart the evaporator Do not turn off the evaporator until the Purge Time has elapsed o H cRNF N N m X 150 Issue 3 2 January 2009 Page 33 of 5 Select Options on the horizontal Menu bar LAMP LAYER SELECTION OPERATOR CONTROLS OPTIONS MAINTENANCE G
15. of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Auto Defrost Drain Auto Defrost and Drain is a condenser option for the Genevac HT4X HT8 and HT12 series 2 evaporation systems and is standard on the HT 24 Workstation Auto Defrost and Drain enables the system to e Automatically drain the condenser of volatile solvent s between method stages e Automatically drain the condenser at the end of the method The Auto Defrost and Drain system requires no user intervention When performing an intermediate drain i e mid method the system also performs a short defrost in case residual solvent from a previous use is frozen in the outlet pipe of the condenser The intermediate drain removes volatile solvents which do not freeze at temperatures above 50 C Benefits of Auto Defrost amp Drain The principal benefit of the Auto Defrost and Drain function is to eliminate volatile solvent s from the condenser The volatile component of a mixture boils off first and is collected in the condenser To remove the higher boiling point solvents low pressures must be applied later in the process However reducing the pressure causes the previously condensed volatile solvent to re boil in the condenser generating a very large volume of vapour which must exit through the pump Until all this vapour is pumped away which can take several hours the system cannot achieve a lower pressure The volatile solvents a
16. swing is used with two 96 well microtitre plates 2ml per well In one swing the lower microtitre plate is empty the upper microtitre plate is full 1 8mls per well On the other swing the reverse is true The two swings now weigh the same However if placed opposite each other in on a rotor would be imbalanced This is because when the swings rotate to their operating attitude the centre of mass of one is at a different radius to that of the other MULL lable ibl BULL Swings are the same weight but not balanced It is also preferable to run the evaporator with all four swings fitted to each level of the rotor If there are only enough samples to fill two swings it is better to distribute the samples into four holders or at least place two empty holders in the rotor This reduces the mechanical stress on the rotor and helps to distribute the heat flow evenly between the samples 10 1450 Issue 3 2 January 2009 Page 13 of 58 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Good Procedural Practice Finally there are a few general rules for safe operation of a system Only permit users familiar with all the issues outlined in this document to operate the equipment Only load swings and sample holders that are approved by Genevac The same user should be responsible for loading and starting the system Never leave the system unevenly loaded with the door closed Someone may start it Never start or restart a
17. system without checking it is evenly loaded all sample holders are correctly seated and all holders swing freely Miss loading may result in unrecoverable sample loss damage to equipment and could M void the warranty Loading the Rotor Samples in the chamber are subjected to accelerations of up to 500G The maximum load capacity is 1 5kg per swing The load capacity includes tubes solvent sample sample holder and swing M Always observe the following Precautions e Never exceed the maximum load capacity of 1 5 kg per swing e Ensure tubes locate correctly in tube holders e Locate sample blocks correctly in sample swings e Load two or four tube holders in opposite and balanced configurations e Distribute tubes in sample holders symmetrically e Balance oppositely loaded pairs of sample holders to within 10g ILTODAGE ERR arl Rotate the rotor by hand Check that all tube holders and plates are correctly located and swing freely Use only the sample holders supplied with the system or that are specified for use with the system Never use non Genevac approved sample holders Genevac Ltd will not accept responsibility for any loss or damage incurred by improperly or excessively loaded rotors Page 14 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Solvents Common Acceptable Solvents Autoprogram Density g cm Density Temp C Available Acetic Acid
18. the contents of the delivery against the delivery note as soon as possible Notify Genevac Ltd immediately if any parts are missing or damaged Refer to the back cover for contact details Arranging Commissioning If your system is to be delivered separately Genevac Ltd will contact you prior to delivery to agree a convenient date to commission your system Training Commissioning normally includes training in the basic operation of the system Further in house training is recommended to fully exploit the flexibility of the system The HT4 evaporator must not be operated by personnel who lack the training or experience to comprehend the hazards that can arise when using the system Personnel without such training require thorough instruction These operating instructions should form the basis of this instruction Positioning the Evaporator The evaporator must be sited on a level and sturdy work surface Position the evaporator at least 300mm away from the edge of a bench and the same distance clear of any breakable objects or areas where entrapment could occur If this positioning requirement is impractical then the evaporator should be bolted to the bench or trolley by its five mounting feet using M10 high tensile bolts Consult Genevac for advice on any other positioning requirements Pipe Connection Overview To Fume Extraction System System Exhaust Outlet Condenser Vacuum Inlet B Condenser Exhaust Inlet F
19. ACH finnonium Hydroxide CHH3UH ICE Diethyl Ether DEE Ethanol EtOH Ethyl Acetate CEtAc Hethanol MeOH HHP TFA THF Heat Off Option Heat Off Elapsed Time CHH HH End nf Run Option End of Run Elapsed Time CHH HH Hater Other H20 Pressure Control Regime Dri Pure Final Controlled Pressure Cnbar C lear Done GENEVAC LTD HELP Toluene PhHe TL ENTER to select deselect Done ENTER to accept ESC to cancel Select a solvent from the window that opens mixture of solvents More than one solvent may be selected if using a Selected solvents are highlighted in blue Select Done when the solvent or solvents have been selected Alternatively select Other and enter the solvent name no more than 31 characters E M M e Va c nf 2 J Y le esr n1 a 7 m 3 rr YC i Page 26 of 6C 150 Issue 3 2 January 2009 Run Ha 981 Last Used Hot yet used SOLVENT Run Data Locked Hext Run Number CH for none Acetonitrile ACN Run Hane finnonium Hydroxide CHH3UH Sample Holder Type Chloroform TCE 5 RUTU PR BRRH DCH Diethyl Ether DEE Auto Programme DHF remaining parameter DHI 48 73 P4 ERE DHSO Ethanol EtOH Ethyl Acetate CEtAc Rotor Speed Hexane Hex Hethanol HeOH
20. ENEVAC LTD HELP TL to move to required option ENTER to select ESC to leave this menu Option not available in this mode or configuration Lamp Layer Selection Disable associated lamp layers if 2 or 3 rotor levels are not used Operator Controls Opens the Controls Menu Options Enable Auto Shutdown and Pre Run Checklist Maintenance For engineer use only Status Displays information relevant to fault diagnostics Adjust Screen Brightness Keypress Beep On Off Off User Intervention Beeps On Off Off End of Run Beeps On Off Off GENEVAC LTD HELP TL to move to required option ENTER to select ESC to leave this menu Adjusts brightness and optinum screen viewing angle Adjust Screen Brightness Adjusts the screen viewing angle The function is not available on newer instruments fitted with high contrast screens Keypress Beep On Off Turns off the key press beep response User Intervention Beeps On Off Turns off the user intervention beep response End of Run Beeps On Off Turns off repeating end of run alarm Press the ESC key to leave these menu screens Page 34 of 6 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evaporating Systems Starting a Run This section describes the steps required to carry out a typical evaporation run for DMSO In this example two sets of eight 28 x 60 mm scintillation vials each containing 5 ml of DMSO are placed in solid aluminiu
21. Fractions 52 Fast Lyophilisation of HPLC Fractions o3 Mixtures of High and Low Boiling Point Solvents AE E 54 Technical DATA z s u nmik se n PRAE MEER K ES RKE MEAE 55 EC Declaration of Conformity 56 Warranty Statement 56 Amendment Control Form 57 Useful Information 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Introduction The Genevac Series Il range of evaporation systems provide very high performance coupled with ease of use The systems are simple to set up easy to operate and very flexible The HT4 SII and HT4X SII evaporation systems are comprised of an evaporation chamber and rotor combined with a in built cryopump condenser unit Vacuum is provided by a Scroll Pump although other types of vacuum pumps can be used Solid state case heaters and CoolHeat radiant lamps heat the chamber and samples The control of chamber sample holder and sample temperature vacuum ramping rate chamber pressure rotor speed and run time are all handled by an embedded PC Lid CoolHeat lamps Embedded PC Exhaust High definition LCD SampleGuard Transmitter Lid release switch Condenser Chamber Condenser Direct Drive and chamber Motor drains Remote Lid p Switch ON OFF switch The system offers the facility to auto program run parameters for any r
22. I 00 86 End of Run Defrost and Drain No Pressure Control Reg ime Dr i Pure Final Controlled Pressure mbar 0 0 GENEUAC LTD HELP fi to select ENTER to edit MENU ESC to exit Select leuel of Run Data protection 3 Run Log Screen Gumel 1 tewerstere C Z The Run Log screen is displayed whilst a run is Channel 2 Tenperature C Mu Id in progress It shows the current status of the opin Mate Creed i evaporator in numerical and graphical form Eu ao 7569 When the SampleGuard probes are appropriately configured it is possible to extrapolate information from the graph that relates to sample drying progress An evaporative cooling effect can be seen in the divergence of the channel 1 and channel 2 traces Conversely converging traces reveal when a sample is dry See Using SampleGuard for details Eva pora ti na Page 22 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evaporating Systems Select Run Screen The Select Run screen lists a library of up to 100 evaporation run profiles Unused run locations remain blank and are available for creating new runs Press the Cursor Direction up and down keys to scroll through the run profiles Run profiles are displayed on the screen 10 at a time SELEC Ho Mame Solvent Unl Holder T 1 Oligosynthesis Annonia eml DEEP WE 35 2 Oligo Purification Water ACH Oml DEEP WE 3H 3 PCR Purification Hater ACH im DEEP WE 38 4 RNA Purification Hater
23. OP to end the run at any time 10 1450 Issue 3 2 January 2009 Page 31 of 58 The following screen appears after the run finishes RUH 91 Channel 1 Tenperature Channel 2 Temperature Chamber Temperature Condenser Gas Temp Pressure Lmhar Spin Rate Crpn Exanple ALARHS MI TxD C TxD ME 2b ME m 1137 H Total 64 46 15 End of Run HH HH HH OO 40 Pressure Spin Rate mbar FIHISHED 00 45 00 50 Select Option or press STOP to skip to select next run Select Skip Drain or Defrost using the numeric keys indicated Skip The evaporator returns to the Run Select screen Drain The system opens the drain valve and pumps any waste solvent into the Waste Solvent Container Defrost Enter the defrost menu Select START to begin the defrost cycle VARIABLES Defrost Valve Drain Valve Flush Valve Isolation Valve Vent Valve Rotor Chanber Heat Spin Rate rpnl Pressure nhar Chamber Temperature Condenser Gas Temp Defrost Start Defrost Drain Done ALARHS Closed Hanua L Hot Fitted Closed Open Stopped Off C C Completed when Elapsed Tine Press START to commence DEFROST sequence STOP to cancel Press START to commence operation The evaporator defrosts the condenser until solvent defrost is automatically detected press the STOP key to
24. Vol Holder T The Select Run screen has the capacity to store Liigade dentis a 8 up to 100 different run profiles Runs 51 to 98 are D MUN LE preloaded to provide a range of standard run M M Bl configurations Runs 99 and 100 are for diagnostic use by engineers Run locations 1 to 50 are available for users to insert their own run profiles 4 RNA Purification Hater 10nl 24 X 15 4 5 Oligo Production fiquecous Mixture dni 58 nl T 46 The Select Run screen is displayed shortly after GENEUAC LTD the system is switched on The most commonly START EDIT GRAPH CLEAR COPY TO DRAIN DEF ROS TD OPTIONS used run IS highlighted by a white band across the HELP Select Run with Tl Menu Item with keys press START to execute screen Starts selected Run using parameters stored 2 Run Data Screen x EN 91 Used Not yet usedl Last Changed New abe Press the Settings key to display the Run Data Next Run Number O for none 8 Rum Name screen It shows the parameters that combine to Sample Holder Type 17 Ta zx form a run profile The screen is used to create IR Sensor Control Temperature C 20 and edit runs It may be accessed whilst a run is Palin eaae ee p in progress allowing control parameters to be Chamber Temperature Control C Wait to cool to 20 Rotor Speed HI adjusted mid run Heat Dff Option Elapsed Time Heat D ff Elapsed Time HH MM 66 68 End of Run Option Elapsed Time End of Run Elapsed Time HH MM
25. ant gas entering condenser Pressure Vacuum chamber and condenser pressure Spin Rate Rotor speed Total Time elapsed since run started including completed linked stages This Stage Time elapsed since start of current stage changes to End of Run or End of Stage and begins to count down when final run time is known Graphical display for Channel 1 Temperature Channel 2 Temperature Chamber Pressure Logarithmic scale Spin rate Other relevant system status appears above and below the graph area Alarms If an error is encountered a description of the problem is shown in the ALARMS field Safety critical errors cause the evaporator to stop and report the reason for stoppage non critical errors allow the evaporator to continue with compromised performance and alert the user to the fault Note Rectify the problem and switch the evaporator off to clear the error from the screen RUN 91 Example RUN 91 Channel 1 Temperature C Channel 1 Temperature C Channel 2 Temperature C Channel 2 Temperature C Chamber Temperature C Chamber Temperature C Condenser Gas Temp C Condenser Gas Temp C Pressure mbar Pressure mbar Spin Rate rpn Spin Rate rpm 1666 Total 88 83 84 This Stage BB 83 84 Total 66 45 43 End of Run 46 82 32 pinning 00 LHea1 pinning Pil j Post Run Final Drying Period Press the DISPLAY key during a run to return to the RUN LOG screen Press the ST
26. ar in mind when using the Auto Program function Auto Program only works with the commonly used solvents shown in the Solvent window If more than one solvent is selected the evaporator selects a run profile which is suitable for the highest boiling point solvent However this may not be the most efficient method for the mixture It is usually more efficient to set a run profile for the more volatile solvent and link this to another run profile for the other component or components of the mixture z E X A 150 Issue 3 2 Jai uary y 2009 Page 2 27 of 5 Genevac HT 4 amp HT 4X Series II Evaporating Systems The following details relate to the remaining run profile fields when the Auto Programme function is not used SampleGuard Control Temperature Enter a temperature value between 20 and 70 C The system heats the sample holders to this temperature Note For evaporators equipped with infra red temperature control set R Control Temperature instead of SampleGuard Control Temperature Only select control temperatures that are safe for the dried sample SampleGuard Control Channel The default setting is channel 1 The option to change to channel 2 is provided to allow continued operation of the system should a fault arise with channel 1 or its associated probe CoolHeat Enable Pressure Enter a pressure value between 5 and 400mbar The infra red lamps do not come on un
27. ards Principles of design and selection BS EN ISO 12100 pts 1 amp 2 2003 Safety of Machinery Basic concepts general principles for design BS EN 50082 1 1998 Electromagnetic compatibility Generic immunity standard BS EN 61010 1 2001 Safety requirements for electrical equipment for measurement control and laboratory use general requirements Warranty Statement This product is guaranteed for period of 12 months from the date of delivery to site In the unlikely event of any defect arising due to faulty materials or construction resulting in system failure the unit will be repaired free of charge This includes all labour and component costs incurred This warranty is subject to the following provisions 1 System must be sited installed and operated in accordance with operator instruction manual 2 he system is only used for purpose it was sold and in accordance with Genevac published compatible solvent list 3 The regular cleaning and preventative maintenance schedule must be adhered to as detailed in operator s manual 4 The warranty does not cover accidental damage misuse modifications or inappropriate repair by untrained personnel 5 The warranty does not cover the following consumable items Sample Guard thermocouple probes control fuses Failure to adhere to the above may result in the costs of repairs being charged Page 56 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evapor
28. ating Systems Amendment Control Form Issue Reason for Change Datelssued 2 7 T ES Integration of The Importance of Safe Loading Document 2 8 Introduction of new Pre Set runs 51 100 within the software 01 March 2004 Introduction of Scroll Pump 2 9 2 9 Introduction of Warranty Statement 26Aprl2004 of Annex A Getting the best from Auto Defrost and 15 September 2006 Converted to print A5 Booklet 08 December 2006 Add Maintenance of Rotor Swings and Sample Holders 09 April 2008 Update page footers 04 June 2008 Reformat layout remove mega amp HT12 references default to 3 current build version amp include old builds as variances o December 2008 Update Statement of Conformity 1 Update sample holder images 26 January 2009 These instructions are correct at time of going to press and may be subject to change without notice No part of these instructions may be reproduced in any form or be processed duplicated or distributed by electronic or optical means without the written permission of Genevac Limited All rights reserved Genevac Limited 2009 These operating instructions should be read before you use the Genevac HT4 SII or HT4X SII evaporation system Your attention is drawn in particular to the section entitled Safety The evaporator should not be discarded in your regular disposal stream Contact your Distributor or Genevac for proper disposa
29. cd EU dS 15 Common Acceptable Solvents 15 Genevac and the ATEX Directive 15 Getting Started 16 Switching on the Pump 16 Switching on the Evaporator 16 Opening the Lid see 16 Using SampleGuard 17 Verifying the Sample Guard Calibration 18 The CONC GIS OE isse eiussak bann te pUR eR Uus E UpEAES 19 Manual Defrost and Drain 19 Auto Defrost and Drain LyoSpeed enabled Systems Only een 20 Flushing the Condenser 20 Evaporator Controls 21 Control Screens an Overview 22 Select Run Screen 23 Functions of the Menu Bar 24 Entering Control Data 24 Run Data Screen su e siki aa akaduoad ak e 25 Run Parameter Details 25 Run Log SerGolicecmee uncle sus used ass arer EUM 31 VST ap RP K Se 31 Shutting DOWN uioocni io roo ved ci uasd sueese 33 Options Menu 34 Starting A UL o eoe otet er pE n pep EbE En Ep cEeidEr 35 The Evaporation Process 36 Optimising a PUT aspi oa a de onus une d 37 Limiting the Chamber Pressure 3 Linking RUNS
30. celeration force approximately equal to 500G Low for most other applications There are few applications where very low speed is required The option is designed to prevent the compression of dried compound during lyophilisation However experimentation reveals the effect to be negligible in most circumstances Note The SampleGuard system does not function when the Very Low rotor speed is selected Therefore heat input is not possible via the infra red lamps Hun Ho 91 Last Used 14 40 03 03 03 Last Changed 12 35 03703703 Run Data Locked No Next Hun Humber 0 for none 0 Run Name Example sample Holder Type Deep Well Plate Sample Volume ml 0 70 solvent Etfic Hex sanpleGuard Control Temperatur HEAT OFF OPTION sanpleGuard Control Channel CoolHeat Enable Pressure I mbar Select option for turning off CoolHeat Chamber Temperature Control Rotor Speed Elapsed Time eat Off Option sample Detection Heat Off Threshold End of Run Option End of Run Threshold End of Hun Defrost and Drain Yes Pressure Control Regime Controlled Pressure Controlled Pressure mbar 10 GENEVAC LTD HELP Tl to select ENTER to accept ESC to cancel switch CoolHeat off when Heat Flow drops below predetermined level The Heat Off Option may be set independently from the End of Run option This allows a final drying stage to run without heat input from the IR lamps
31. ch the system determines automatically 2 Second Stage removal of the aqueous phase Control the pressure at 8mbar the BP stays above 0 C and the water cannot freeze Select high rotor speed promoting good convection amp hence heat flow in the solution c Endthe method using Heat Flow rather than specifying the duration for the stage DM 3 Third Stage drying the stubborn samples Run the system at Full Vacuum for 1 to 3 hours Experimentation is required to optimise this stage Different compounds require different times to reach final dryness highly polar molecules often take the longest c Auto Defrost and Drain at the end of the stage this is a full defrost and drain as there are no more stages to follow om See appendix A for programming details Please contact your local Genevac representative for further details on run times alternatively please e mail Applications Genevac com 10 1450 Issue 3 2 January 2009 Page 49 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Lyophilising HPLC Fractions The best optimised evaporation method has the following stages 1 2 Follow stage 1 of the Drying HPLC Fractions method to remove the organic solvent Cool the samples concentrating some of the water without any heat input Set the controlled pressure to 8mbar to boil away some of the water without any heat input this cools the holders and helps achieve good freezing in the next stage
32. ct Genevac Service for evaluation Cleaning the Chamber Rotor and Swings TFA creep can cause debris deposits on the inside of the chamber and on the Quartz glass see Problem Prevention for details Routinely inspect the inside of the chamber and quartz glass for build up of debris and potential contaminants Check the sample swings are able to move freely Clean the Quartz Glass using a suitable solvent such as methanol or acetone and a lint free cloth or paper towel Clean the swings and rotor in the same manner Take care to avoid solvent contact with the outside paintwork and accessories of the chamber Scroll Pump Check the pump exhaust catch pot regularly and empty it as necessary No further routine maintenance is required Page 44 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Further Notes for CVP Pumps Check the pump oil level weekly Ensure the oil level is within the notch on the dipstick Top it up if necessary using the correct grade of silicon oil Do not apply vacuum to a recently defrosted condenser containing traces of liquid DMF DMSO or NMP This is likely to cause pump oil contamination Correct Oil level centre of dipstick notch Pump Type Part Number CVP100 CP SCF025 AS1616 1 litre CVP100 CPC Crylin 614 AC2310 1kg The pump must have an adeguate supply of cooling air and a minimum 300mm of free space adjacent to the heat exhaust Do not place
33. d simplicity of use The frequently used function keys are on the left hand side of the keyboard The right side illuminates to accept input when the Run data screen is accessed STOP START Press the START and STOP keys to start and stop the selected run Press the Cursor Direction Keys to move around the screen in the direction of the arrows Press the Enter key to open or close fields in the Run Data screen for inputting or amending data Note the START key acts Enter as an enter key when the keyboard is not illuminated Press the Menu key to display the User Menu screen This only operates when the rotor is not spinning and the chamber is at Menu atmospheric pressure Press the Display key to show the graph from the last completed run This function only operates when a run has been completed Display Press the Cursor Direction Keys to show different segments of the graph Press the Settings key to display the Run Data screen for the selected run Note the Run Data screen can also be accessed Settings from the View Edit Details option on the SELECT RUN screen W BU Bop 10 1450 Issue 3 2 January 2009 Page 21 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Control Screens an Overview There are three main control screens The information on this page is a brief overview of what the screens do Detailed descriptions are provided in following sections 1 Select Run Screen No Nane Solvent
34. desicoasindnsscisueiustornaiasdolieivadasheninn d sn 3 Pre programmed Runs ee 37 Getting the Best from the System 39 Routine Checks 39 Tips for Improving System Performance 39 Further Checks for CVP Pumps 39 Run Parameters Quick Reference 40 Problem Prevention 43 Condensation eee 43 TFA CTE6P se5eshasn ke 43 BODIN mt S 43 Maintenance eere eee 44 Cleaning the Sample Holders and Swings 44 Cleaning the Chamber Rotor and Swings 44 Scroll PUMP saci Sercs deenedai bnsendaskiocexded cxcweeeoosente 44 Further Notes for CVP Pumps 45 Maintenance and Service 45 Moving the System ee 45 Additional Equipment 46 Auto Defrost Drain 47 Benefits of Auto Defrost Drain 47 md Me Mm 47 How WW To y E 48 When to use Auto Defrost and Drain 48 When not to use Auto Defrost and Drain 49 Drying HPLC Fractions 49 Lyophilising HPLC Fractions 50 Notes on Lyophilisation 50 Drying Mixed High and Low Boiling Point SDIO S aoi O 51 Programming Guides 52 Drying HPLC
35. e DRAIN Drains the condenser Applicable only to LyoSpeed or automated systems e DEFROST Enters the Condenser Defrost menu e FLUSH Enters the Condenser Flush menu Applicable only if the flush option is installed e OPTIONS Enters the Options Menu Entering Control Data Enter data in the Run Data screen From start up of the system and the software control screen press START to display the Select Run o O START Select the View Edit Details option and press START to display the Run Data screen START Use the UP and DOWN cursor keys to move between fields Unless otherwise stated press ENTER to open a field Input your requirement and press ENTER again to close the field E Oven Page 24 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evaporating Systems Run Data Screen Each of the method profiles shown on the Select Run screen is generated from the Run Data screen Select the required run profile and press the Settings key to enter the Run Data screen The parameters of the selected run are shown on the screen A default set of parameters is shown if an unused run location is selected The Run Data screen can also be accessed when a run is in progress Run Ha G Last Used Hot yet used Last Changed CHew entry Hext Run Number CH for none Run Hane Solvent Sample Holder Type Sanple Vo lune SanpleGuard Control Temperature 70 SanpleGuard Cont
36. e section entitled Getting the Best From Auto Defrost and Drain Pressure Control Regime Select one of the following Full Vacuum The evaporator reduces the chamber to the lowest attainable pressure Controlled Pressure Enter a value for the required chamber pressure DriPure The evaporator selects high rotor speed and reduces the chamber pressure slowly Use this setting if bumping is anticipated VariableDriPure Enter values for Dri Pure Start Pressure Dri Pure End Pressure Dri Pure Ramp Time and Final Controlled Pressure This offers a more flexibility than the standard Dri Pure option The evaporator selects high rotor speed and reduces the pressure according to the set parameters To Save the settings and Create a new Run Profile Press the ESC key on the keyboard Press the Y key to confirm the changes Page 30 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Run Log Screen The Run Log screen shows information relating to sample drying progress Relevant system status information is shown with key parameter values represented graphically to reveal change trends in real time Numerical values are shown for Channel 1 Temperature SampleGuard channel 1 probe connected to sample holder Channel 2 Temperature SampleGuard channel 2 optional probes submerged in sample Chamber Temperature Temperature of vacuum chamber wall Condenser Gas Temperature Temperature of cool
37. ecognised solvent or mixture Simply select the solvent s from a drop down menu enter details for volume and sample holder type select Auto Program and optimised run parameters appear highlighted in cyan on the display screen The status of the system is shown on an LCD screen Programming input is via a keypad and simple to use up down controls enable the run time rotor and chamber temperatures to be set in an instant Page 2 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series II Evaporating Systems Lyophilisation Freeze Drying may be achieved in LyoSpeed enabled systems fitted with an Auto Defrost amp Drain condenser Samples must be frozen before loading into the evaporator Automatic end of run shut down may be programmed manually with a simple time setting or may be achieved by automatic end of run prediction using Heat Flow or Sample Detection methods The Run Progress screen has a fully featured graphical display providing annotated plots for temperature and pressure The control software enables the user to specify and store a library of up to 100 different evaporation profiles Evaporator Screen and Keypad Run profiles can also be linked to provide multi stage runs Up to 100 different profile steps can be linked and iterative loops can also be programmed With a maximum single run time of just below 100 hours this makes the system extremely flexible This manual will guide you through the re
38. ently avoids the possibility of mis loading Sample Holder correctly seated Page 12 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series II Evaporating Systems Balancing Sample Holders and Swings Opposite pairs of swings must be balanced within 10g and the swings must be of the same A type and version Please note that there are several versions of Side Bridge Swings in circulation with a static weight ranging from 375g to 445g Place swings of the same static weight in diametric opposition on the rotor ideally use the same version of swings in all four positions of each rotor level Genevac systems have some inbuilt tolerance for imbalance and a safety system which stops the rotor if the out of balance is unacceptably high However to minimise noise nuisance and wear and tear the balance limit should always be observed If the evaporator is to be partially loaded always fill the top rotor level first Then fill the second level then the third third level applies to HT12 SII evaporators only Real loads may be balanced using Dummy samples They must be of a similar solvent composition For example do not balance 200g of 50 50 Water Acetonitrile with 200g of water Partway through the run the acetonitrile evaporates but the water remains resulting in an imbalance of 100g Note that with a system such as the Fast Stack swing balancing is slightly more complex Suppose a Fast Stack Deepwell
39. entrifugal acceleration 10 1450 Issue 3 2 January 2009 Page 43 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Maintenance Refer to the section entitled Getting the Best from Your System for details of routine maintenance checks This section describes some further proactive maintenance procedures Excessive build up of debris on the pivoting faces of the sample swings and rotor can M cause the sample swings to stick in the out position when the rotor stops This can cause unrecoverable sample loss Cleaning the Sample Holders and Swings Regular inspection and maintenance of swings and sample holders should be performed at least monthly The following inspection routine is mandatory following any tube breakage or solvent spillage Never use wet swings or holders in an evaporator Visually inspect the sample holders monthly Clean off any debris especially in the sample holder wells as this may cause high points that lead to stress in the glassware resulting in breakage The main cause of repeat glassware breakage is fragments from a previously broken tube Solvent can stick the glass fragments to the holder making it difficult to remove Residual solvent or sample material must be cleaned off Superficial surface damage e g scratches do not affect the performance of a holder or swing However if there is any structural damage if any part of the holder swing or rotor is bent or deformed do not use it Conta
40. er pressure to a set value Enter a value for the required Controlled Pressure between 0 and 500 mbar e Dri Pure Reduces the pressure to 50 mbar by equal increments over a 40 minute time period Then goes to the control pressure This ramp feature is particularly useful for preventing bumping e Variable Dri Pure As Dri Pure but with additional user settable parameters for the ramp start pressure the ramp end pressure the ramp duration Bumping the violent and uncontrolled boiling of solvents resulting in cross contamination of samples Note The Coolheat function is disabled during the Dri Pure cycle Page 42 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Problem Prevention Condensation Solvent condensation within the evaporator occurs when the chamber walls are cooler than the solvent vapour This is most likely to occur with high boiling point solvents such as NMP DMI DMSO and possibly DMF Pre heat the evaporator chamber to prevent this happening To do this enter the Run Data screen set the Minimum Chamber Temperature field to 40 C and start the run The chamber takes approximately 20 minutes to reach this temperature Note the CoolHeat lamps do not operate during this pre heating cycle If condensation occurs unexpectedly switch off the lamps by entering O into the Heat off Elapsed Time field on the Run Data screen Do not pre heat the chamber when evaporatin
41. evac personnel or approved representatives of Genevac using only approved spare parts Limitations of Use following circumstances The HT4 SII and HT4X SII evaporation systems are unsuitable for use under the o With strong mineral acids such as HCI and HBr at all concentrations unless specifically built to order o Evaporating diethyl ether and other similar low auto ignition solvents e For use as a pressure vessel Page 4 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Options Available options include e Bump protection Dri Pure and Variable Dri Pure e High power Coolheat lamps e Low UV lamp lenses Data Logging is available The easy to use package provides the data needed for process and quality control Hardware Required e PCrunning Windows 95 98 NT 2000 or XP e Around 5Mbytes of free space on your hard drive e Serial Port on the PC or USB to Serial Adapter e Serial Cable to connect the PC to the Evaporator Contact your sales representative for purchase and installation details 10 1450 Issue 3 2 January 2009 Page 5 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Delivery and Installation Installation and commissioning by Genevac personnel is an option available with every new Genevac HT system Installation instructions are provided should the commissioning option not be selected Checking the Delivery Check
42. formance e Increase evaporation speed for high boiling point solvents by pre heating the aluminium sample holders e Use the link run facility when evaporating solvent mixtures with large differences in boiling point See the section entitled Optimising a Run for details Further Checks for CVP Pumps e Check the pump oil level weekly e Ensure that the oil level is within the notch on the dipstick e Never apply vacuum to a heated condenser after defrosting containing traces of liquid DMF DMSO or NMP This causes pump contamination 10 1450 Issue 3 2 January 2009 Page 39 of 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Run Parameters Quick Reference Run Data Locked Set to Yes to protect the run data from inadvertent changing Press the ENTER key to toggle between Yes and No lock the data after completing the run entry Next Run Number Enables the creation of multistage runs by linking runs in any order Enter the number of the run that is required to follow the current run Runs may also be ooped by linking to themselves this makes the run cycle repeatedly until interrupted by a press of the STOP key Run Name Identifies the run profile Sample Holder Type Select the sample holder type from the drop down menu or select OTHER and enter the holder name Sample Volume Enter the volume of the individual samples in mls Solvent Select the solvent from the drop down menu or select OTHER and ente
43. g volatile solvents or mixtures prone to bumping The system waits for the chamber to cool before allowing the run to start This helps to prevent sudden uncontrolled boiling as the chamber pressure reduces Note The chamber will not cool below the ambient temperature Use Automatic Control to slightly speed up the evaporation of high boiling point solvents The system continues to heat the chamber temperature to the set value while the run commences Page 28 of 60 10 1450 Issue 3 2 January 2009 91 Last Used 12 25 03 03 03 L ROTOR SPEED Run No Run Data Locked Next Run Number O for none Select Rotor Speed Run Name Sample Holder Type High 500g Sample Volume ml Lou 30091 solvent Very Lou 50g SampleGuard Control Temperature C SampleGuard Control Channel CoolHeat Enable Pressure mbar Chamber Temperature Control C AUTO Cool to 32 Control at 20 Heat 0ff Option Heat Flow Heat Off Threshold Not Applicable End of Run Option Not Applicable End of Run Threshold Not fipplicable End of Run Defrost and Drain Yes Pressure Control Regime Controlled Pressure Controlled Pressure mbar 10 GENEVAC LTD HELP TL to select ENTER to accept ESC to cancel Rotor Speed Low Select one of the following rotor speed options High f microtitre plates or very full tubes are to be used or if the solvent or solvent mixtures are prone to bumping Samples are subjected to an ac
44. g volatile solvents such as TFA acetonitrile or methanol TFA Creep TFA exhibits the property of creeping This is the movement of the TFA in liquid phase up the inside of the tubes vials or microtitre plates Problems can arise if solvent containing product is deposited in this way on the top face of plates Solvent and product may also be thrown onto the side of the chamber and the Quartz glass lamp windows as the rotor spins Kura S A a aM Whilst the solvent evaporates the product becomes carbonised by the heat from the lamps and forms sites where crack propagation can occur Inspect the lamp glass at regular intervals and clean with a lint free cloth and acetone Contact Genevac Service if the contamination becomes excessive and carbonised as shown A range of specialised sample holders is available to protect the Quartz lenses Contact Genevac Sales for details Bumping Bumping can also cause product to deposit on the glass lenses as previously described It is unpredictable and may occur with any solvent or mixture it is also a potential source of cross contamination between samples Avoid bumping by selecting the Dri Pure option from the Pressure Control Regime drop down menu on the Run Edit screen This option sets a high rotor speed and avoids super heating the samples by reducing the pressure in the vacuum chamber by gradual increments Evaporation begins progressively and samples are contained due to the higher c
45. however respond entirely differently At full vacuum a reasonable evaporation rate is achieved At 8 mbar the time required for evaporation increases significantly When evaporating 40 ml fractions in 24 x 150 mm glass tubes typical evaporation times for water acetonitrile mixtures can be in excess of 8 hours The same applies to larger volumes in beakers A reduced evaporation time can be achieved by setting the SampleGuard control temperature to 60 C for a defined period Provided this period is not excessive the sample temperature is likely to remain below 40 C as result of evaporative cooling This is the case even though the CoolHeat lamps remain on After this period a second or a number of successive runs can be linked at reduced SampleGuard temperatures and different pressures Some experimentation is necessary to ensure that safe sample temperatures are not exceeded Pre programmed Runs HT8 and HT12 SII evaporators are pre programmed with a number of evaporation methods These runs are located at 51 to 60 of the RUN selection screen Desired runs can be copied to other locations using the copy to function Runs 61 through to 98 are all associated with these pre programmed methods and runs 99 and 100 are for use by Genevac service engineers please do not alter them The pre programmed runs are designed to cover a group of solvents such as high boiling point The following table provides a guide to the correct run selectio
46. i P C A Nu B i g pts a eS P p 2 R 3 j r y User Manual Issue 3 2 January 2009 Part Number 10 1450 Contents I OG HO o AP 2 os Le AY enn oe ee M pe p al Safety Symbols 4 Genevac Evaporators and Combustible SOMNIS seanair AE TEE 4 Electrical Safety satum sckex its Ta ricotta RE ai iiaei 4 Limitations of USE 4 Options ae HARE PFURPPMIEONSURPEFONDU se Ona S 5 Delivery and Installation 6 Checking the Delivery 6 Arranging Commissioning 6 Ic T 6 Positioning the Evaporator 6 Pipe Connection Overview 6 Identifying the Parts 7 Installing the Stystem sss 8 Installation Variations Valve Block 9 Intsallation Variations Lyospeed Systems 9 Installation Variations CVP Vacuum Pump 9 Safe Loading of Rotor General Document 10 Nomenclature eee 10 Use of Correct Accessories 11 Adherence to Mass Limit 11 oafe Loading of Sample Holders into Swings 12 Balancing Sample Holders and Swings 13 Good Procedural Practice 14 Loading the Rotor 14 OST ocenwronn dnas nanic o d edi
47. idation of the warranty applicable particularly where Series and Series evaporators are used within the same laboratory For example some sample holders designed for use in Series systems might appear to fit in a Series system but would exceed the weight limitations If in doubt consult Genevac before using such holders i All swings and holders must be approved for the Genevac system in which they are used There are also instances where a sample holder intended for one tube or vial becomes unsuitable if used with something else even though it might appear that the alternative tube fits The Genevac Accessories Brochure indicates the maximum tube length that each holder is designed to take Always adhere to these limits Similarly sample holders intended for use in a Side Bridge swing must not be used in an Open swing even though they might appear to fit The Genevac Accessories Brochure has a note For use in Side Bridge Swing by these items but if in doubt ask Genevac Please note that some not all of the Bohdan Miniblock system sample holders significantly exceed the mass limitations of a Genevac system f you plan to use Bohdan Miniblocks in a Genevac system please contact Genevac for a list of the relevant weights Adherence to Mass Limit The total mass that can be loaded onto each position of a Genevac swung rotor This mass includes The swing The sample holder The tubes or vials The sample solutions
48. includes the following features Enhanced condenser draining with minimum hold up Automation of the drain valves Specific defrost of condenser outlet pipe Mid method short defrost and drain to remove volatiles Automated full defrost and drain at end of method Auto Defrost and Drain appears as an option in the Run Data screen when entering the method parameters The evaporator performs in one of two ways depending on whether the method is part of a linked series of methods If the method stands alone and is not linked to any other method the system performs a full defrost at the end of the method and then drains the condenser automatically If the method is linked other methods follow it the system performs a short defrost sufficient only to defrost any frozen solvent trapped in the outlet pipe then drains the condenser When this is complete the following linked method continues automatically If the method has other methods linked to it but is the last in the chain then at the end of the method the system a full defrost and drains the condenser automatically When to use Auto Defrost and Drain Auto Defrost and Drain has two main functions 1 To automatically drain the condenser mid process to eliminate volatile solvents enabling the system to reach full vacuum in the later stages of evaporation This allows the system to achieve better final drying of the sample and to get better evaporation of mixtures of solvents with wide
49. ing TFA intermediate short defrost and drain is permitted Full defrost and drain at the end of the method should not be performed if there is residual TFA in the condenser Perform a manual defrost for 10 minutes manually stop the defrost cycle and drain the system e At the end of a lyophilisation method water vapour may travel back from the cold trap to the chamber and cause the powders to collapse Remove the samples first then defrost and drain Drying HPLC Fractions The best optimised evaporation method has the following stages 1 First Stage removal of the organic phase a Use Variable Dri Pure to prevent bumping Ramp the pressure down from 175mbar to 40 mbar acetonitrile or 45mbar methanol in 20 minutes at high rotor speed 500g Control the pressure at 40mbar for Acetonitrile and 45mbar for Methanol these control pressures are chosen to keep the boiling point above O C i e prevent the water freezing b Auto Defrost and Drain at the end of the stage this is a short defrost in case a small amount of water is frozen in the drain port The system then drains the organic solvent from the condenser allowing high vacuum levels to be achieved later in the run c Consult your local Genevac representative for advice on the evaporation time for this stage However a good rule of thumb is that for 50 50 Acetonitrile water the overall length of this stage should be approximately 1 3 as long as the length of stage 2 whi
50. ions Wait for Chamber to Heat Range 0 C to 45 C Wait for Chamber to Cool Range 0 C to 45 C Automatic Control The control temperature is automatically set to an optimised figure for the recognised solvent mixture selected Enter the chamber temperature required before spin up commences Note do not set the Wait for Chamber to Cool value below the ambient temperature Rotor Speed Select from 3 available options High Maximum acceleration applied to samples 500G Low Maximum acceleration applied to samples 300G Very Low Maximum acceleration applied to samples 50G The default setting is Low if no other selection is made If the Dri Pure option described later is selected it over rides the rotor speed setting and sets High speed Heat Off Option Select from 3 available options e Elapsed Time This can be in a range of 0 lamps off for the entire run to 99 hours 59 minutes e Heat Flow Automatically detects end of run by monitoring evaporative heat demand Heat Flow can operate with 1 SampleGuard probe fitted only The control channel probe must be placed in the sample holder The system detects dryness by monitoring the demand for heat input proportional to the rate at which the solvent is evaporating Heat flow may not work at very low control temperatures or with very low sample loading In these instances the proportion of evaporation energy drawn from ambient temperature becomes significant enough to affect the
51. k of the evaporator Connect a length of exhaust tube to the spigot on top of the pump catch pot Connect the other end of the exhaust tube to the condenser exhaust inlet on the back of the evaporator Connect the pump control cable to the pump control cable socket Connect the other end of the control cable to the control cable socket on the back of the evaporator Note The pump control cable has a male connector at one end a female at the other end and only connects to the corresponding sockets in the correct orientation To connect the control cable push the connector into the socket and twist the knurled grip clockwise until it clicks into place Connect the remaining length of exhaust tube to the system exhaust outlet and secure using a pipe clamp connect the other end of the exhaust tube to the laboratory fume extraction system Connect drain pipes not supplied to all three drain connectors Place the other end of the drain pipes in a suitable waste solvent container not supplied Ensure the end of the drain pipes cannot be submerged in the waste solvent x v Connect the mains power cable to the pump mains power connector Connect the mains power cable to a suitable mains power outlet The system is now ready to switch on Carry out a safety inspection before operating the system Page 8 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evaporating Systems Installation Variations Valve Block A va
52. l G instructions Within the EU it is Genevac s responsibility under the WEEE directive to provide for the recycling of their products 10 1450 Issue 3 2 January 2009 Page 57 of 58 Genevac Limited The Sovereign Centre Farthing Road Ipswich IP1 5AP United Kingdom Sales and Service Hotlines Service Hotline 44 0 1473 243000 Sales Hotline 44 0 1473 240000 Fax 44 0 1473 461176 Email mailto salesinfo genevac co uk Web site http www genevac com Genevac Inc SP Industries 815 State Route 208 Gardiner NY 12525 United States of America Sales and Service Hotline 1 845 267 2211 Fax 1 845 267 2212 Email salesinfo genevacusa com Useful Information lf you need to contact Genevac for assistance use either the telephone or fax Hotlines shown It always helps Genevac Service if you have the serial numbers at hand for the components of your system lf you need to contact Genevac Sales for information on Service Contracts or products use the telephone or fax Hotlines shown Alternatively Email or visit our web site These instructions are subject to change without notice No part of these instructions may be reproduced in any form or be processed duplicated or distributed by electronic or optical means without the written permission of Genevac Limited All rights reserved Genevac Limited Read these operating instructions before using the Genevac HT4 SII or HTAX SII Evap
53. l Evaporating Systems Getting Started The following notes provide basic instructions for starting up the evaporation system Refer to the relevant sections of this manual for detailed information on specific steps Switching on the Pump Connect the pump to the mains and switch on the mains Switch on the pump power switch Note The pump does not start until the evaporator is switched on Switching on the Evaporator owitch on the evaporator power switch There is a short delay while the imbedded PC completes its boot up sequence The display shows the Software Control screen The system is now in stand by mode Evaporator power switch Press the START key to start the system e The pump starts e The display shows the Run Select screen e The condenser starts after a delay of approximately three minutes Note The system is not available for use until e The pump reaches its operating temperature CVP pumps Software Control Screen only e he system Pump Warming delay times out HCL systems with a scroll pump only e The condenser temperature cools below 0 C Opening the Lid Press the button on the front panel to open stop and close the lid The lid is operated by an electric actuator and is controlled by safety sensors f an object prevents the lid closing it re opens automatically to prevent entrapment HIC CPAN EUKON Note The lid only opens if the rotor is stationary and the chambe
54. lve block and T piece are required to connect a scroll pump to an HT4 SII or an early build variant HT4X SII evaporator These models can be recognised by metal condenser vacuum inlet and condenser exhaust inlet The valve block is necessary to prevent the possibility of damaging back pressure being applied to the scroll pump exhaust if ice forms in the condenser exhaust pot the later HT4X SII features an internal pressure relief valve Valve block T Piece To Fume Extraction System System Exhaust Outlet Intsallation Variations Lyospeed Systems Connect the single solvent drain pipe to the drain outlet Balance pipe manifold of an HT4X SII LyoSpeed system mE Single drain Ensure the end of the drain pipe cannot be submerged in the waste solvent Installation Variations CVP Vacuum Pump Install the CVP pump in the same way as the scroll pump the following additional instructions apply CVP Pump exhaust outlet Connect a short length of exhaust tubing to the pump exhaust outlet and seal with a pipe clamp Connect the other end of the short tube to a pump catch pot spigot and seal with a pipe clamp Connect another length of exhaust tubing to the second catch pot spigot seal with a pipe clamp Connect the other end of this exhaust tubing to the condenser exhaust inlet on the back of the evaporator Note Early build versions of the CVP pump require a different pump control cable which connects to the pump via a plas
55. ly differing boiling points To automatically defrost and drain the condenser at the end of the method saving the user time This means that for an overnight method which finishes before the user comes to the Lab in the morning the system is defrosted drained and is ready to use straight away This has a benefit for any solvent The second of these requires no further explanation however there are a number of applications for the first the intermediate defrost and drain These include Drying of HPLC fractions where high vacuum in the final stages of evaporation is beneficial Use of the Genevac fast lyophilisation method for HPLC fractions where high vacuum in the latter stages of the process is essential Evaporation of DMF or DMSO mixed with a volatile solvent e g dichloromethane also known as DCM or methylene chloride where the mixture of solvents necessitates high vacuum for the high boiling point solvent which is removed last but where the volatile solvents removed first sit in the condenser and spoil the level of vacuum achieved in the latter stages of the run Page 48 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems When not to use Auto Defrost and Drain There are certain circumstances when Auto Defrost and Drain should not be used This is to protect the system and or samples from solvent damage Do not use Auto Defrost and Drain in the following circumstances e Evaporat
56. m sample holders Switch on the HT8 or HT12 SII evaporation system select the Run Data screen go to an unused run location and input the following data Run Data Locked ennen No Next Run Number ee 0 Run Name DMSO 28 x 60 mm tubes Sample Holder Type Solid Aluminium 28 x 60 Sample Volume 5 olo V 1 SERERE O DMSO SampleGuard Control Temperature 40 SampleGuard Control Channel 1 CoolHeat Enable Pressure 100 Chamber Temperature Control 40 Rotor SDOOGQS cuente nrc qaa ir aia iR RUE Low Heat Off Elapsed Time 01 40 End of Run Elapsed Time 01 40 Controlled Pressure Full Vacuum Once the data is entered the run profile is stored for future use The SampleGuard control temperature is set to 40 C and the chamber pressure to full vacuum The chamber is preheated to 40 C to prevent solvent condensing in the chamber 10 1450 Issue 3 2 January 2009 Page 35 of 58 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Dispense the DMSO samples into the vials and place the sample holders into the sample swings Load the sample holders and swings into the evaporator ensuring that the vials sample holders and sample swings are correctly and securely located Refer to the sec
57. n Each run is programmed to be used with a particular group of solvents Therefore it may be possible to program a more efficient method for just one of those solvents For advice on programming a suitable method for a specific solvent or solvent mixture please contact your Genevac representative or go to applications genevac com 10 1450 Issue 3 2 January 2009 Page 37 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems The pre programmed runs are designed to make use of all the appropriate features of the system and to provide optimal evaporation conditions All methods make use of the automatic end of run detection feature so that run times do not need be set the system stops when all the samples are dry Each run has a venting procedure linked to the end of the evaporation process This helps to remove residual vapours from the chamber k The preset programs will only function correctly if SampleGuard probe 1 is placed in the j aluminium sample holder block or fast stack swing See the section entitled Using SampleGuard for details Run Name BP Solvent Examples Application Number Range 51 Volatiles not 60 90 C Ethyl Acetate or Single volatile solvents with no risk of DCM Methanol bumping Very Volatile amp 40 90 C DCM Methylene Volatile solvent mixtures and DCM DCM Chloride or Methylene chloride where risk of bumping Chloroform is high Medium BP 90 DMF or Toluene Medium BP solvent or mixture of medium
58. nce positioned the probe stays firmly in position under centrifugal force Verifying the Sample Guard Calibration The following operation requires the use of a Sample Guard Power supply This is may be ordered as an option or may be purchased from Genevac With the evaporator switched on open the evaporator door and remove the Sample Guard Stuffer Plug Connect SampleGuard probes to channels 1 and 2 and immerse their ends in a beaker of water at approximately 40 C Sample Guard Stuffer Plug Connect the power lead from the Sample Guard Power Supply to connector 3 of the Sample Guard transmitter Plug the Sample Guard Power Supply into a suitable mains power outlet and switch it on Close the door so that the screen may be viewed but do not lock it This prevents any chance of inadvertently starting the rotor with the power supply cable connected Access temperature display Press a hidden key on the keypad as shown and verify the with Hidden Key indicated temperatures against a calibrated digital thermometer Compare the readings on the display with that of a calibrated reference thermometer measuring the temperature of the same water The frequency of verification and record retention should meet the requirements of your ISO EN BS 9000 series or NAMAS procedures Disconnect the SampleGuard Power Supply lead from the SampleGuard Transmitter refit the SampleGuard Stuffer Plug Comparison Thermometer The SampleG
59. nic solvent is removed from the mixture Never use Auto Defrost and Drain on the final stages of a lyophilisation method solvent vapour from the condenser may re enter the samples and cause the powder to collapse Feedback from some Genevac users suggests that this is worse when samples are TFA salts where as HCl salts are reportedly more robust These observations have not been proven Remove the samples from the system before defrosting the condenser Page 50 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Drying Mixed High and Low Boiling Point Samples The actual method required depends on the solvents in the mixture A mixture of DMF or DMSO and DCM is outlines in this illustration For other details of mixtures please contact Genevac 1 2 Select Variable Dri Pure to prevent bumping Ramp from 750mbar to 70 mbar in 55 minutes Evaporate the DCM at 65mbar and collect it all in the cold trap Select Auto Defrost and Drain this is a short defrost and drain to remove the organic solvent from the condenser allowing high vacuum levels to be achieved later when drying the high boiling point solvent Evaporate the high boiling point solvent Select full vacuum end the method using heat flow Dry any stubborn leftover solvent Select full vacuum and let it run for 1 hour Select Auto Defrost and Drain this is a full defrost and drain See appendix C for programming details
60. o the probe hole of a sample holder The sample temperature cannot now be monitored Use the cursor keys to select the SampleGuard Control Temperature field and press ENTER Input the new value and press ENTER again The system requests a confirmation command to make the change and close the Run Data screen Press Y for yes and N for no The SampleGuard transmitter requires the rotor to spin at sufficient speed before it operates The message TxD displayed on the screen indicates that the SampleGuard is not transmitting This could be because the rotor is spinning up or is running at Very Low speed Page 17 of 58 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Note Significant cooling and possibly freezing occurs during evaporation the extent is dependant upon the solvent It is advisable to position the sample probe in a sample near the centre of the holder Since the central wells are surrounded by other frozen or cold wells there is a significant thermal drain during evaporation This effect is particularly prevalent when using microtitre plates Under these conditions dryness may occur in the outer wells whist the central samples remain in solution or frozen The use of Genevac Heat Transfer Plates is beneficial in reducing this effect by providing an even heat transfer across the plate When positioning the sample probe always ensure that the probe tip is located firmly at the bottom of the well vial or tube O
61. orating Systems Keep them near the system for easy reference Your attention is drawn in particular to the section entitled Safety
62. quirements for setting up operating and maintaining the system It will facilitate the most efficient procedures to protect your product s integrity and ensure optimum performance at all times 10 1450 Issue 3 2 January 2009 Page 3 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Safety Safety Symbols The following safety symbols are used throughout this manual and are defined as follows Hazards that can be harmful to health or lead to serious damage or injury Possible risk to sample integrity Genevac Evaporators and Combustible Solvents Please note it remains the responsibility of the user to consider safety when evaporating any combustible solvents and to place the system in a well ventilated environment Genevac s position regarding evaporation of such solvents particularly with respect to the European ATEX directive is available on our website or from your local sales representative Electrical Safety Important the system must be earthed This evaporation system is a safety class 1 product according to IEC classification It must never be used with any interruption to the safety earth conductor It is an installation category l product and is intended to operate from a normal single phase power supply This evaporator is designed for use in a degree 1 environment no pollution or only dry non conductive pollution Any maintenance or repair of this product must be carried out by Gen
63. r is at atmospheric pressure Page 16 of 60 10 1450 Issue 3 2 January 2009 Using SampleGuard SampleGuard Transmitter and Probe Sample holder probe hole 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series II Evaporating Systems SampleGuard is a dual channel temperature monitoring system that operates when the rotor spins One channel allows the evaporator to control the temperature of a sample holder the other monitors the temperature of a sample within the holder The temperature differential caused by evaporative cooling is used to monitor sample drying progress Connect the SampleGuard Probes to the SampleGuard Transmitter as shown The numbers 1 and 2 stamped into the SampleGuard transmitter identify the input connectors for each channel Connect a SampleGuard Stuffer Plug to the third connector for normal system operation Insert the Channel 1 control channel temperature probe into the small probe hole in one of the sample holders Insert the Channel 2 temperature probe into a sample tube vial well etc Press the SETTINGS key to display the Run Data screen Use the cursor keys to select the SampleGuard Control Channel field and select channel 1 as the control channel Note Only use the option to select channel 2 as the SampleGuard Control Channel if there is a fault with channel 1 or its associated temperature probe In this instance insert the channel 2 probe int
64. r the solvent name no mope that 31 characters Assuming that recognised data was entered in the preceding fields the Auto Program option appears Select this to automatically programme the remaining run parameters Auto programmed parameters appear highlighted in cyan and may be overwritten manually SampleGuard Control Temperature Enter the maximum temperature to which the samples holders are heated during evaporation The system s ability to control the sample holders at lower range temperatures is dependant upon the solvent boiling point i e Evaporative cooling and the ambient temperature within the vacuum chamber This can be set within the range 20 to 70 C The default setting is 30 C if no other value is entered Note this is not available for very low rotor speed Sample Guard Control Channel Channel 1 is assigned as the control channel by default channel 1 probe is placed in the sample holder channel 2 probe is optionally placed in the sample Assign control to channel 2 and place the channel 2 probe in the sample holder only if a fault affects channel 1 or its associated probe CoolHeat Enable Pressure Enter the pressure below which the lamps turn on This can be in the range of 5 400 mbar The default setting is 400mbar if no other value is entered Page 40 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series II Evaporating Systems Chamber Temperature Control Select from 3 available opt
65. re said to spoil the vacuum and so the higher boiling point solvents do not boil Vacuum spoiling affects final dryness of samples or in the very worst cases the ability to evaporate higher boiling point solvents at all To overcome this problem manual intervention was previously required to drain the condenser after the volatile solvent was captured in the condenser This draining operation can now be automated An additional benefit of Auto Defrost and Drain is that volatile solvents are collected and can be disposed of safely reducing VOC emissions Evaporators equipped with the Auto Defrost and Drain facility are identified by a Lyo Speed Enabled label The Auto Defrost and Drain option also appears in the run menu when programming methods Flexibility A Genevac evaporator enhanced with Auto defrost and Drain functionality can be used as part of the LyoSpeed process In addition it can also deliver improved results when working with any mixture of solvents with differing boiling points Auto defrost and drain helps achieve excellent final dryness when evaporating HPLC fractions It also facilitates automated drying of DCM and DMSO or DMF mixtures These are otherwise almost impossible to evaporate without draining the DCM before tackling the higher boiling point solvent 10 1450 Issue 3 2 January 2009 Page 47 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems How it Works The Auto Defrost and Drain condenser
66. rol Channel CoolHeat Enable Pressure Cobar Hininun Chamber Temperature C Rotor Speed High Lou Heat Off Option Elapsed Tine Heat Off Elapsed Time CHH HH HH HB End nf Run Option Elapsed Tine End af Run Elapsed Time HH HH1 AA BA Pressure Control Regine Controlled Pressure Controlled Pressure Lnbar GENEVAC LTD HELP T4 to select ENTER to edit MENU ESC to exit Press the cursor direction up or down keys to move between fields Press the Enter key to open a field Enter a new value for the relevant parameter and press the Enter key again to close the field Run Parameter Details Run Data Protection The run profile may be protected against accidental alteration Set the Run Data Protection field to No before attempting to edit an existing run profile Set the Run Data Protection field to Yes to lock the profile Next Run Number Runs may be linked together Enter the number of the run that requires to be linked The linked run commences when the current run finishes Enter O in the Next Run Number field if no run is to be linked Note A run may be linked to itself This causes the run to continue repeatedly Run Name Enter a name no more than 20 characters to identify the run profile Text entered on the keyboard appears in the bottom part of the screen Press the Enter key to enter the text into the Run Name field 10 1450 Issue 3 2 January 2009 Page 25 of 58
67. stems to a suitable waste solvent container 10 1450 Issue 3 2 January 2009 Page 19 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems Auto Defrost and Drain LyoSpeed enabled Systems Only Ensure that a suitable waste solvent container is connected to the condenser drain pipe at AN all times Draining occurs automatically on LyoSpeed systems even after the run has completed Ensure that the end of the drain hose remains above the level of waste solvent in the container Flushing the Condenser Use the condenser flushing system if fitted to clean traces of volatile solvent from the condenser before evaporating a less volatile solvents the condenser operates most efficiently when it is drained and clean Always drain the condenser before using the condenser flusher Select FLUSH on the HT4 SIl Menu Bar and press the START key Wait until the system vacuums down to approximately 5mabr Pour approximately 100 ml of acetone into the flushing solvent container and open the flushing valve Close the flushing valve after use Stop the system and allow it to vent to atmospheric pressure from the condenser vacuum pot Repeat the flushing procedure as necessary Never use the flushing valve to vent the system Page 20 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems Evaporator Controls The evaporator keyboard controls and display screens are designed for ease an
68. system s ability to detect heat input For applications where Sample Guard control temperature or low sample loading is low use either Elapsed Time or Sample Detection methods for the Heat Off Option e Sample Detection Automatically detects end of run by monitoring sample cooling in liquid phase Requires both SampleGuard probes to be fitted Channel 1 monitors the swing holder temperature Channel 2 is placed in a central well of the sample holder and monitor the sample temperature The system monitors the difference between the control temperature and the sample temperature As vacuum is applied the sample boiling point drops and the samples cool whilst in liquid phase their heat energy being absorbed by evaporation evaporative cooling The system detects dryness as the temperature of the dried product rises End of Run Option Set the run time duration 10 1450 Issue 3 2 January 2009 Page 41 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems End of Run Elapsed Time Select the elapsed time after which the run is stopped This can be in the range of 1 minute to 99 hours 59 minutes End of Run Defrost and Drain Select Yes or No Only available on LyoSpeed or automated systems Typically used to remove mixed solvents Pressure Control Regime Select from the following options e Full Vacuum Reduces the chamber pressure to the maximum vacuum capability of the pump e Controlled Pressure Reduces the chamb
69. ta Locked N N OO O ON OK Next Run Number 2 B 4 0 5 oe Lyo part Lyo part E Lyo part Fractions Lyo Sample Holder Type e Holder TE Holder UT Holder v v Holder Sample Volume ml Your Volume Volume Your Volume Volume Your Volume Volume Your Volume Volume Solvent MeCN or MeOH MeCN or MeOH MeCN or MeOH MeCN or MeOH P H20 E H20 M H20 EM H20 Em Temp C 40 40 m RN NN Channel 1 1 1 1 procure boo Pressure Seer jean pated penes pat control preheat to 25 preheat to O preheat to O preheat to 30 Rotor Rotor Speed sits High is High Heat Off Option Elapsed Time Elapsed Time Elapsed Time Elapsed Time Heat Off Elapsed Time lask for time 0 00 00 00 05 00 End of Run Option Elapsed Time Elapsed Time Elapsed Time Elapsed Time End of Run Elapsed Time ask for time 0 30 01 00 10 00 Auto Defrost amp Drain S S O M Z hada NOVY RE PVO VON Regime Variable Dri Pure Pressure Full Vacuum Full Vacuum T V RN NN QR NE mbar 175 OMM BBE LL mn 45 for MeOH Dri Pure Dri Pure Ramp Time Time Final Control Pressure 2 NN MeCN 45 for MeOH Notes Remove MeCN Cool the water Freeze the water Lyophilise the water 10 1450 Issue 3 2 January 2009 Page 53 of 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Mixtures of High and Low Boiling Point Solvents Drying High Low Mixtures Run number O 0 o S e B Run Data Locked 2 ff Next Run Number Run Name High Low Mix Solvent DMSO or DMF amp
70. the pump in a space with restricted airflow such as a cupboard Planned Maintenance and Service Whilst every effort is made to design and manufacture the HT4 SII and HTA4X SII evaporation systems to the highest build quality and to provide assured reliability there will be some degree of wear and ageing of the seals and bearings of the chamber condenser and pump The extent of wear and ageing depends on the utilisation of the system the severity of temperature cycling and the nature of the solvents used Some solvents may eventually cause pin hole corrosion in the connecting tubes resulting in a decline in performance A gradual decline in system performance may not be noticed if it occurs over a period of time Monitor the system performance by keeping a weekly log of the time taken for the system to reach full vacuum and the full vacuum achieved In order to maintain peak performance and avoid costly and unscheduled down time Genevac strongly recommend implementing a schedule of planned maintenance Changing parts in the field is complex and demands a high level of skill To this end Genevac offers a range of preventative maintenance service and breakdown contracts Moving the System Refer to the section entitled Positioning the Evaporator Refer also to the following notes if it is necessary to move a system to a new location Address the following key points before moving an HT4 SII or HTAX SII evaporation system Clear sufficient
71. tic connector Do not attempt to exchange a CVP pump for a scroll pump This operation requires a set up in the system software that may only be carried out by Genevac Service or a trained representative of Genevac CVP Pump vacuum inlet 10 1450 Issue 3 2 January 2009 Page 9 of 58 Genevac HT 4 8 HT 4X Series II Evaporating Systems Safe Loading of Rotor General Document Genevac are obliged to include the following information in its entirety irrespective of the system type As with all centrifuges Genevac centrifugal evaporators must be loaded correctly to remove the risk of damage Failure to correctly load a system can lead to unrecoverable loss of samples and damage to the system This guide is intended for new users and also as a reminder for more experienced users The principles outlined apply to all Genevac evaporators The following instructions deal with various aspects of loading Use of correct swings and sample holders Observation of weight limits oafe loading of sample holders into swings Balancing of swings and sample holders Good procedural practice Nomenclature Some Genevac systems feature fixed rotors which have angled holes for individual tubes or holders The following instructions are primarily concerned with the more common swung rotors The new range of Genevac sample holders blue in colour include integral swing holders such as the example shown
72. til the CoolHeat Enable Pressure is reached This prevents sudden uncontrolled boiling of volatile solvents as the chamber pressure reduces Chamber Temperature Control Run Ho 91 Last Used 12 25 03 03 03 Last Changed 12 31 03703703 Kun Data Locked No Next Run Number 0 for none 0 Run Name Example sample Holder Type Deep Well Plate Sample Volume ml 0 70 50 l vent Et c Hex sanpleGuard Control Temperature I CHAMBER TEMPERATURE sanpleGuard Control Channel CoolHeat Enable Pressure mbar select Chamber Temp control regime Rotor Speed Wait for Chamber to Heat Wait for Chamber to Cool Heat ff Option Automatic Control Heat Off Threshold End of Run Option End of Run Threshold Not Applicable End of Run Defrost and Drain Yes Pressure Control Regime Controlled Pressure Controlled Pressure mbar 10 GENEVAC LTD HELP Tl to select ENTER to accept ESC to cancel Chamber temperature controlled to suit selected solvent or mixture Select from the options that appear in the window and enter a temperature value between O and 45 C Use Wait for Chamber to Heat to pre heat the vacuum chamber before removing high boiling point solvents The system heats the chamber to the set value before allowing the run to start This prevents high boiling point solvents condensing on the chamber walls Note The chamber heaters take approximately a minute to raise the chamber temperature by 1 C Use Wait for Chamber to Cool when removin
73. tion entitled Loading the Rotor for details Position the channel 1 SampleGuard probe in its locating hole in the sample holder Position the channel 2 sample SampleGuard probe in an outer tube or well Refer to the section entitled Using SampleGuard for details Always ensure that the tip of the sample probe is located at the bottom of the tube Close the evaporator door and press the START key SampleGuard Probe Location Hole The display indicates that the chamber is warming up this takes approximately twenty minutes The system starts automatically when the chamber temperature reaches the Chamber Temperature Control value Some time can be gained by preheating solid aluminium sample holders to 40 C in an oven Other evaporation run profiles are suggested in the section entitled Optimising a Run The Evaporation Process This section examines the process that occurs within the evaporator during the run When the previously described evaporation run starts the pressure drops steadily as air is evacuated from the chamber and condenser The CoolHeat lamps operate when the pressure reaches 100 mbar and because the chamber is pre heated to 40 C the sample holders quickly reach the pre set temperature The SampleGuard maintains the 40 C temperature ceiling As solvent starts to evaporate the rate of pressure change reduces The temperature of the sample drops due to evaporative cooling Provided there is sufficient vac
74. uard system will not operate without the Stuffer Plug fitted Page 18 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 amp HT 4X Series Il Evaporating Systems The Condenser The condenser starts automatically a short time approximately 3 minutes after the evaporator is switched on There is a further short delay before the condenser reaches operating temperature Drain the condenser defrost first if necessary before each run and at the end of each day Access the DEFROST DRAIN CYCLE for the condenser via the Select Run Screen See the section entitled Select Run Screen for details Manual Defrost and Drain To start the defrost cycle move the cursor to the DEFROST DRAIN CYCLE using the up down cursor keys and press the ENTER key The DEFROST VALVE opens and the defrost cycle begins The required frequency of defrosting and draining the condenser depends on the volume and nature of the evaporated solvents The maximum defrost period should be no longer than two hours Defrost and drain the condenser after each run to obtain optimum performance from the condenser Open the lid and lift the drain valve plunger to open the valves Note Close the drain valves manually do not rely on the lid to push down the drain valve plunger when it closes Before opening the condenser drain valves ensure that pipes connect the chamber AN drain condenser drain and exhaust drain outlets or single drain pipe for LyoSpeed sy
75. uum the drop in sample temperature occurs even though the CoolHeat lamps are on i e all the energy goes into evaporation and not into sample warming The evaporation rate and vapour flow drops until the pressure stabilises and a steady state is reached There is then normally a long period of constant pressure and vapour flow whilst the bulk of solvent is evaporated As the solvent approaches dryness the evaporation rate often reduces causing the vapour pressure to drop This is particularly noticeable with oily samples whose vapour pressure is very low At this point the sample temperature starts to rise reaching the SampleGuard control temperature in a reasonably short time Page 36 of 60 10 1450 Issue 3 2 January 2009 Genevac HT 4 8 HT 4X Series Il Evaporating Systems Optimising a Run This section describes the general principles by which the Series Il control software can optimise evaporation rates Limiting the Chamber Pressure Pressure control can be used to significantly increase the evaporation rate for aqueous mixtures of greater than 30 water when contained in glass tubes and beakers When evaporating these mixtures at pressures of less than 4 mbar ice forms extending the evaporation time By controlling the evaporator at a pressure of 6 mbar ice formation is prevented and the time required for evaporation can be reduced by up to 309 Linking Runs Mixtures of water and methanol in deep well microtitre plates
76. uum 0 15 mbar 50Hz Dri Pure Yes 0 12 mabr 60Hz Auto vacuum vent valve Yes Flow rate 3 6 mh Rapid defrost Yes Ultimate system vacuum 0 4 mbar Vacuumpump CVP Weight Evaporator W xD x H 540 x 640 x 577mm HT4 Maximum vacuum 590 x 640 x 590mm HT4X Flow rate Scroll pump 530 x 305 x 398 CVP pump 540 x 290 x 405 Electrical jq 0 0000 Power Supply single phase 9A 230V 50Hz 208V 60Hz Operating Environment Storage Environment Ambient temperature 15 C to 30 C Ambient temperature 10 C to 60 C Relative humidity 10 60 Relative humidity 10 80 Altitude Sea level to 12 000m Altitude Sea level to 12 000m 10 1450 Issue 3 2 January 2009 Page 55 of 58 Genevac HT 4 amp HT 4X Series II Evaporating Systems EC Declaration of Conformity We Genevac Limited declare that this product Series Il Evaporating System Complies with the relevant Essential Health and Safety Requirements of the European Machinery Directive 98 37 EEC the EMC Directive 89 336 EEC and the Low voltage Directive 73 23 EEC Conformity is demonstrated by compliance with the following specifications EN 60204 1 2006 Safety of machinery Electrical equipment of machines Pt 1 General Requirements EN 249 1992 Safety of machinery Safety distances to prevent danger zones being reached by upper limbs EN 1088 1995 A1 2007 Safety of machinery Interlocking devices associated with gu

The Genevac HT- 4 & HT- 4X Series II Evaporation Systems User

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The Genevac HT- 4 &amp; HT- 4X Series II Evaporation Systems User

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The Genevac HT- 4 & HT- 4X Series II Evaporation Systems User