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The Genevac HT-24 Series II Workstation Systems User Manual

1. January 2009 page 43 of 60 Genevac HT 24 series Workstation How it Works The Auto Defrost and Drain condenser 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 Th
2. 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 O 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 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 liqui
3. 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 Oo Oven Page 24060 SCS lt CS lt lt S SSTTS SOSSOSOSOCOCOCCSCSCSCSC S S SSONISOD Tse 2 1 January 2009 Genevac HT 24 Series Workstation 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 Ho 6 Last Used Hot yet used Last Changed New entry Run Data Locked Ho Hext Run Number CH for none H Run Hane Solvent Sanple Holder Type Sanple Vo lune SanpleGuard Control Temperature C C SanpleGuard Control Channel CoolHeat Enable Pressure Cobar Hininunm Chamber Temperature C Rotor Speed CHigh Low Heat Off Option Elapsed Tine Heat Off Elapsed Time CHH HH AB AA End of Run Option Elapsed Tine End of Run Elapsed Time CHH HH AHA BA Pressure Control Regine Controlled Pressure Controlled Pressure Cnmbar H GENEVAC LTD HELP T to select ENTER to edit
4. CS SSS 18S Issue 2 1 January 2000 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 707 Executive Boulevard Suite D Valley Cottage New York 10989 United States of America Sales and Service Hotline 1 845 267 2211 Fax 1 845 267 2212 Email salesinfo genevacusa com Useful Information If 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 If 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 HI 24 Workstation Keep them near the system for easy reference Your attention is drawn in particular to the section entitled Safety
5. Press a hidden key on the keypad as shown and verify the 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 SampleGuard system will not operate without the Stuffer Plug fitted Page 200160 UMMM dO Issue 21 January 2009 Genevac HT 24 Series Workstation Evaporator Controls The evaporator keyboard controls and display screens are designed for ease and 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 E Settings 10 1562 Issue 2 1 January 2009 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 as an enter key when the keyboard is not illuminated Press the Menu key to display the User Menu screen This only operates whe
6. ATEX Directive 14 Waste Solvent Container cccccseeeeeeeeeees 15 Getting started a ccisccessccuienenscecsnact cnc aunntiodentianss 16 DC NAG UDe niania ari tierce 16 Switching OM actoetevnceridessecetiusssuctevencediarnccseniane 16 Unlocking the DOoOl cccccceeeeeeeeeeeeeseeeeeeeees 17 Unlocking the Door Remotely 000008 17 Locking the DOOD cccsecccseeeeeeeeeeeeeeeseeeesees 18 Extra Precautions for Fume Hood Systems 18 Using SampleGuard 00 eecesseeeeeeeeeeeeees 19 Verifying the Sample Guard Calibration 20 Evaporator Controls ccsseeseeeeeeeeeees 21 Control Screens an Overview 20 22 Select RUN Screen cccccseeeseeseeeeeeeeeenees 23 Functions of the Menu Bat c cceceeeeeeees 24 Entering Control Data ccccccccseeeeeeeeeeeeenees 24 Run Data Screen siiscsteccaicicsdccscaceitessicesevactnes 25 Run Parameter Detalls ccccseceseeeeeeeeees 25 Run Log Screen area cesecsesccanses cataysnaeateanecese 31 POPS Ss denice sesavoncidaieanamsdewerann sds cans EA 31 Shutting DOWN cccccceseeseeeeeeeeeeeeneeeeeees 33 Options Menu ccscceseeeeeeeeeeeeeeeeeeeeeees 34 Starting a RU rs cc ceccgceeseesetcies ecw sacteesicedseceses 35 The Evaporation Process ccceseeeeeees 36 Optimising a RUN ccccsceeseeseeeeeeeeeeeeees 37 Limiting the Ch
7. 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 Arun 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 1562 Issue 2 1 January 2009 page 25 of 60 Run Ho Y Last Used Hot yet used Last Changed New entry Run Data Locked SAMPLE HOLDER Hext Run Number CH for none Run Hane Select Sample Holder Solvent Microtitre Plate Sanple Vo lune Deep Hell Plate Tube Vial Holder SanpleGuard Control Temperature C SanpleGuard Control Channel CoolHeat Enable Pressure mbar Hininum Chamber Temperature C Rotor Speed High Heat Off
8. Menu bar LAMP LAYER SELECTION OPERATOR CONTROLS OPTIONS MAINTENANCE GENEVAC 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 I Genevac HT 24 Series Workstation 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 i
9. Option Elapsed Tine Heat Off Elapsed Time CHH HH AA AA End of Run Option Elapsed Tine End of Run Elapsed Time CHH HH HA Pressure Control Regime Dr i Pure Dri Pure Final Controlled Pressure Crmbar H GEHEVAC LTD HELP T1 to select ENTER to accept ESC to cancel Sample 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 Run Ho 91 Last Used Hot yet used SOLVENT Run Data Locked Hext Run Number CH for none Acetonitrile ACH Run Hane Annoniun Hydroxide CHH30H 1 Chloroform TCE Sanple Holder Type DCH Sanple Vo lune Diethyl Ether DEE DHF SanpleGuard Control Temperature C DHI SanpleGuard Control Channel DHSO CoolHeat Enable Pressure mbar Ethanol EtOH Hininum Chamber Temperature C CI Ethyl Acetate CEtAc Rotor Speed Hexane Hex Hethanol HeOH Heat Off Option HHP Heat Off Elapsed Time CHH HH TFA End of Run Option THF End of Run Elapsed Time CHH HH Toluene PhHe Hater H20 Pressure Control Regime Other Dri Pure Final Controlled Pressure Cnbar C lear Done GENEVAC LTD HELP TL ENTER to select deselect Done ENTER to accept ESC to cancel Select a solvent from the window that opens More than one solvent may be selected if using a mixture
10. 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 rpm Spin Rate rpn 1666 Total 66 63 64 This Stage 66 03 44 Total 66 45 43 End of Run 46 82 32 Pinning UU Lite q Spinning PMN j Post Run Final Drying Period Press the DISPLAY key during a run to return to the RUN LOG screen Press the STOP to end the run at any time 10 1562 Issue 2 1 January 2009 page 31 of 60 The following screen appears after the run finishes RUN 91 Exanp le ALARMS Channel 1 Temperature C C TxD Channel 2 Temperature C C TxD Chamber Temperature Condenser Gas Temp Pressure Cmbar Spin Rate Crpn c Cc 26 ad 24 1137 4 Total 44 46 15 End of Run 44 44 4A mbar OO 40 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 WAR IABLES ALARHS Defrost Valve Closed Drain Valve Hanua L Flush Valve Hot Fitted Isolation Valve Closed Vent Valve Open Rotor Stopped Chamber Heat Off Spin Rate Crpn Pressure Cmbar Chamber Temperature C Condenser Gas Tenp eA
11. 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 the 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 Pages0ore0SCSCSCS lt SSSSSSSSSS dO Issue 21 January 2000 Genevac HT 24 Series Workstation Run Log Screen The Run Log screen shows information relating to sample drying pro
12. 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 HT 24 workstation e Clear sufficient space to accommodate the workstation at the new location e Ensure there is access to a power supply e Ensure there is adequate ventilation e Make provision for the extraction of the pump exhaust e Defrost and drain and if possible flush the condenser pots e Remove the sample swings from the rotor Page 50 oreo MM A Issue 2 1 January 2000 Genevac HT 24 Series Workstation 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 d
13. 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 Contact 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 f
14. installation Please unpack your system at the point of receipt in order to ease the movement of the component parts to the point of use The HT 24 workstation must be commissioned by Genevac personnel or suitably trained Genevac representatives Checking the delivery Check 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 Genevac Ltd will contact you prior to the delivery to agree a date to commission your system Training Commissioning will normally include training in the basic operation of the System Further in house training is recommended to fully exploit the flexibility of the system Do not allow personnel to operate the HI 24 workstation who lack the training or A experience to comprehend the hazards that car arise when using the system Personnel without such training require thorough instruction The operating instructions within this manual may form the basis of that instruction Positioning the evaporator Refer to the section entitled Technical data for dimensions and a plan view drawing Refer also to the separate document entitled Installation Requirements Use the inbuilt jacks as shown to lift all four wheels clear of the floor when the workstation is in its final position The back of the system may be positioned against a wall although provisi
15. of solvents 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 At this point the option to select Auto Program is presented Run Ho 91 Last Used Hot yet used Run Data Locked Hext Run Humber CA for none Run Hane Sanple Holder Type 5 AU TO PROGRAN Auto Programme renaining paraneters YLlesJ HLol Rotor Speed Heat Off Option Heat Off Elapsed Time CHH HH End of Run Option End of Run Elapsed Time CHH HH Pressure Control Regime Dri Pure Final Controlled Pressure Crmbar GENEVAC LID SOLVENT Acetonitrile ACH Annonium Hydroxide CHH30H Chloroform TCE DCH Diethyl Ether DEE DHF DHI DHSO Ethanol EtOH Ethyl Acetate CEtAc Hexane Hex Hethanol MeOH HHP TFA THF Toluene PhHe Hater H20 Other C lear 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 No 91 Last Used 14 47 14 0 7703 Last Changed 14 47 14707703 Run Data Protection Next Run Number 0 for none Run Name sample Holder Type sample Volume ml 50 lvent SampleGuard Control Temperature C sampleGuard Control Channel CoolHeat Enable Pressure mbar Cha
16. samples from solvent damage Do not use Auto Defrost and Drain in the following circumstances e Evaporating 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 1 75mbar 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 Acetonitr
17. 009 Genevac HT 24 Series Workstation Each evaporator displays the Software Control screen Press the START key on the keyboard to access the Select Run screen ii scien Note The Select Run screen starts up at the last or most anie frequently used run 98 SOLUTION PHASE 2 DCMNMETHANOL iml DEEP UE 40 0 GENEVAC LTD MENU Sy EDIT GRAPH CLEAR COPY TO DRAIN DEFROST FLUSH OPTIONS HELT Select Run with Th Menu Iten with keys press START to execute Starts selected Run using parameters slored Unlocking the Door Select a system to use press the door OPEN button and manually open the door An evaporator door cannot be unlocked when the associated system is under vacuum or when the rotor is spinning Note When the system stops a multiple beep sounds and repeats intermittently to indicate the door may be unlocked The beep function may be disabled See the section entitled Options Menu for details Unlocking the Door Remotely A Press the OPEN CHAMBER button on the control panel to unlock the door remotely Use this feature if harmful fumes may be present in the evaporator The evaporator door opens slightly allowing the fume extraction system to clear the fumes before the fume hood doors are opened 10 1562 Issue 2 1 January 2009 page 17 of 60 Genevac HT 24 series Workstation Page 18 of 60 Locking the Door Hold the door firmly in the closed position and press and hold the d
18. 68 Chamber Temperature Control C Wait to cool to 20 Rotor Speed High Heat Off Option Elapsed Time Heat Off Elapsed Time HH MM 66 68 End of Run Option Elapsed Time End of Run Elapsed Time HH MM 00 66 End of Run Defrost and Drain No Pressure Control Reg ime Dr i Pure Final Controlled Pressure mbar 0 0 GENEUAC LTD HELP t to select ENTER to edit MENUVESC to exit Select level of Run Data pro 3 Run Log Screen RUN 91 Example Channel 1 Tenperature C Channel 2 Tenperature C Chanber Tenperature C Condenser Gas Temp C Pressure nbar Spin Rate rpn Total 66 83 84 This Stage 68 83 84 Spinning 400 Liew Page 22 of 60 The Select Run screen has the capacity to store up to 100 different run profiles Runs 51 to 98 are preloaded to provide a range of standard run 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 The Select Run screen is displayed shortly after the system is switched on The most commonly used run is highlighted by a white band across the screen Press the Settings key to display the Run Data screen It shows the parameters that combine to form a run profile The screen is used to create and edit runs It may be accessed whilst a run is in progress allowing control parameters to be adjusted mid run The Run Log screen is displayed wh
19. Defrost __ Completed when M Elapsed Time Start Defrost Drain Done 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 Alternatively press the STOP key to end the defrost cycle Enter the Select Run screen and press the STOP key SELECT RUN No Name 50 l vent Vol Holder T xt 91 Example Etc Hex iml Deep We 40 gz PURIFICATION WUATERN CETONITRILE 10m 18 X 15 SOLID PHASE SYNTH TFASDCH eml DEEP WE COMPOUND m CONFIRM REQUEST OLIGO SYN Shut down evaporator SOLUTION SOLUTION PHASE 2 DCHNME THANOL im DEEP WE MAINTENANCE TEST 1 Om MAINTENANCE TEST 2 Om GENEVAC LTD MENU vais 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 Shut down the workstation using the red OFF button on the workstation Control Panel Note Ensure that both evaporators are idle before shutting down the workstation Select Options on the horizontal
20. RENCE a EXHAUST SPIGOT REFERENCE 817 REFERENCE a O41 REFERENCE flO REFERENCE lt lt Se I FRONT Operating Environment proximity of sensitive equipment 750 1000 mbar at altitude up to 1600m 15 C to 30 C Humidity 35 70 Emissions Noise Not exceeding 66dB at one metre from the evaporator measured during defrost and drain cycle Page 54 oi60 u 1562 Issue 2 1 January 2000 Genevac HT 24 Series Workstation 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 guards 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 gener
21. 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 Page40ore0SCSCSCSCSCSCSCSCSCSSSSSSSSSdO 1562 Issue 2 1 January 2000 Genevac HT 24 Series Workstation Chamber Temperature Control Select from 3 available options 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
22. The Genevac HT 24 Series Il Workstation Systems User Manual Issue 2 1 January 20098 Part Number 10 1562 Contents Introduction icinccd etic duets doncsicumendinnretinnetinneaniies 2 BU eiaa 6 Safety Symbols cccccccssseeeceeeeecssseeesseeeeeeees 6 Genevac Evaporators and Combustible Solvents serie Sea tages lavsiiee aioe fee os sane aes ations detuemem Game ene decease 6 Electrical Safety cccccccccsssceceeseesseeeeseeeeeeaees 6 Limitations Of USC ccceccceeceseeeeeseeseseeseneeees 6 PON ONNS seon a 7 Delivery and installation eeeeeee 8 Checking the Celivery ccccceeceecseeeeeeeeeeeeees 8 Arranging COMMISSIONING 0ecceeeeeeeeeeeeeeees 8 Training 0 0 cece eeccceececeeeeceeeeaeeeseeeeseceseueeeeesaeeesaeeess 8 Positioning the evaporator ccccceceeeeeeeeeees 8 Safe Loading of Rotor General Document sale shu suse eigenen aw E N N EE A 9 Nomenclature cee cee cc eecceeeeeeeceeeee esse eeneeeneeeees 9 Use of Correct Accessories 0ccccceeeeeeeeeees 10 Adherence to Mass Limit ccceeeeseeeeeeees 10 Safe Loading of Sample Holders into Swings 11 Balancing Sample Holders and Swings 12 Good Procedural Practice ccccccceeeeeeeeees 13 Loading the Rotor c csccsscssesseeeeeeeensees 13 SOINEN CS rinia aai 14 Common Acceptable Solvents c0cc 14 Genevac and the
23. ac HT 24 series Workstation Balancing Sample Holders and Swings Opposite pairs of swings must be balanced within 10g and the swings must be of the same AN 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 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 8m
24. al requirements Note Under the Low Voltage Directive 73 23 EEC the limit for earth leakage current for Class1 portable equipment is specified at 3 5mA Whilst every effort has been taken to minimise the leakage current of the HT 24 it may slightly exceed this value at typically 4 6mA This is normal and does not indicate a problem with the system 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 The 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 SampleGuard thermocouple probes control fuses Failure to adhere to these provisions may result in the costs of repairs being charged 10 1562 Issue 2 1 January 2009 page 55 of 60 Genevac HT 24 series Work
25. amber Pressure 0008 37 Linking RUNS snccsisssssenntheaysnniantnaidnescitetancndnsisdamsene irene 3 Pre programmed RUNG cccseeeeeeeeeeseeeeeees 37 Getting the Best from the System 39 Routine CHECKS cceccccecccceeeeceeeeeseeeeeeeeeeeeees 39 Tips for Improving System Performance 39 Run Parameters Quick Reference 0 40 Auto Defrost Drain cccceeeeseeeeeeeeeeees 43 What is Auto Defrost amp Drain cccee 43 Benefits of Auto Defrost amp Drain 00 43 Fe VUE setecrecies ceeaeties seme aemencdemecescenntetedehemnecacceseanie 43 HOW it WorkS 20 00 cece ccc ceeeeceeeeeeeeeeeeeseeeeaeeeseeeess 44 When to use Auto Defrost and Drain 44 When not to use Auto Defrost and Drain 45 Drying HPLC Fractions ccccceeeseeeeeeeeeeees 45 Lyophilising HPLC Fractions cccceeeee 46 Notes on Lyophilisation ccccccseeeeeeeeeeeees 46 Drying Mixed High and Low Boiling Point SAMPES en eh eee ene ee eee 47 Problem Prevention csscsscsseeeeeeeeeseees 48 COSTS AOU sses stint ces i a ARE a 48 TFAG CO secede seas ene vee E E 48 ES COMING saeco senacaniuteaameneuaneestumteidastatancensneneasenasans 48 Maintenance ccccccsecseeseeeeeesenseneeeeeeneees 49 Cleaning the Sample Holders and Swingg 49 Cleaning the Chamber Rotor and Swingg 49 STOEP UNN eee ener rtes te ne
26. aporator ensuring that the vials sample holders and sample swings are correctly and securely located Refer to the section 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 SampleGuard Probe Close the evaporator door and press the START key 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 pres
27. ature 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 IR 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 until the CoolHeat Enable Pressure is reached This prevents sudden uncontrolled boiling of volatile solvents as the chamber pressure reduces Chamber Temperature Control Run No 91 Last Used 12 25 03 03 03 Last Changed 12 31 03 03 03 Run Data Locked No Next Run Number 0 for none 0 Run Name Example sample Holder Type Deep Well Plate sample Volume ml 0 70 30 lvent Etfic Hex sanpleGuard Control Temperature 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 Off Option 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 s
28. be 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 10 1562 Issue 2 1 January 2009 page 9 of 60 Genevac HT 24 series Workstation 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 invalidation of the warranty applicable particula
29. ble 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 420160 U U A Issue 2 1 January 2000 Genevac HT 24 Series Workstation Auto Defrost Drain What is Auto Defrost amp 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 ap
30. ce or repair of this product must be carried out by Genevac personnel or approved representatives of Genevac using only approved spare parts Limitations of Use A The HT 24 workstation is unsuitable for use under the following circumstances With strong mineral acids such as HCI and HBr at all concentrations unless specifically built to order Evaporating diethyl ether and other similar low auto ignition solvents e For use as a pressure vessel Pages oreo T Issue 2 1 January 2000 Genevac HT 24 Series Workstation Options Available options include e Bump protection Dri Pure on one or both evaporators e High power Coolheat lamps on one or both evaporators e Low UV lamp lenses on one or both evaporators not available with high power lamps e Built in fume extraction hood and pipe system Data Logging is available independently from each evaporator Dependent on user hardware both evaporators could be logged to the same PC The easy to use package provides the data needed for process and quality control Hardware Required PC running Windows 95 98 NT 2000 or XP Around 5Mbytes of free space on your hard drive Serial Port on the PC or USB to Serial Adapter Serial Cable to connect the PC to the Evaporator Contact your sales representative for purchase and installation details 10 1562 Issue 2 1 January 2009 page 7 of 60 Genevac HT 24 series Workstation Delivery and
31. ces In 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 Page 0o60 U A Issue 21 January 2000 Genevac HT 24 Series Workstation Safe Loading of Sample Holders into Swings This information is applicable where Series 1 AN and series Il equipment is used in the same 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 Both these modes of miss loading are possible with a Series 1 open or standard swing but are virtually impossible with a Series Il swing Care must still be taken when loading the samples iiie E EF K Sample Holder correctly N seated The Series 1 design is easy to distinguish The corners are not welded oO MAX MASS FOR SERIES 1 9009 a Ang le 5 ANGLE x Sample Holder on edge of swing 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 permanently avoids the possibility of mis loading Sample Holder correctly seated 10 1562 Issue 2 1 January 2009 page 11 of 60 Genev
32. d 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 1562 Issue 2 1 January 2009 page 41 of 60 Genevac HT 24 series Workstation 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 chamber 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 Varia
33. e loss damage to equipment and could AN 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 AN 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 Ta i SETE NT URLE salut in 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 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 10 1562 Issue 2 1 January 2009 page 13 of 60 Genevac HT 24 series Workstation Solvents Common Acceptable Solvents Autoprogram Solvent Density g cm Density Temp C PWETEL ey G AceticAcid ON a a a ee a a emmen ta Pichloroethane DCE o o o O o 124 S 2 S Y Dichloromethane DCM 88 Dimethylacetamide DMAc 8H a Dimethylami
34. een which shows the status of the relevant system Each evaporator can be controlled independently via its own keypad Evaporator Screen and Keypad Simple to use up down controls enable the run time rotor and chamber temperatures to be set in an instant Single push buttons set the other functions 10 1562 Issue 2 1 January 2009 page 3 of 60 Genevac HT 24 series Workstation The two evaporators share a single scroll pump by means of a vacuum valve manifold The valve manifold intelligently switches the pump to each evaporator on demand The scroll pump is a dry vacuum pump compact in size air cooled and driven directly by a single phase electric motor Data Logging is available independently from each evaporator Both evaporators can connect and log to the same PC Data Connections x 2 amp Waste Solvent Pump Mains Power Supply l Connections x 3 HT 24 Rear View amp Electrical Circuit Breakers Fume Hood rear panel removed for clarity The optional fume hood fits on top of the HT 24 workstation and provides a totally enclosed system There are 3 transparent sliding doors in the front for easy access to the evaporators and a window in each side An exhaust spigot in the roof provides for connection to a suitable fume extraction system A flow meter is located in the top right corner to monitor performance of the extraction system Page4oieo MA oae 2 1 January 2000 Genevac HT 24 Series Wo
35. eep well plates Flask holder One piece holder for 50m lTubes Sample Genie 10 1562 Issue 2 1 January 2009 page 51 of 60 Genevac HT 24 series Workstation Help h This section describes potential errors and faults that may occur and lists the probable i causes Temperature e The sample temperature exceeds the control limit e The CoolHeat lamps do not switch on Probable cause e The wrong control channel is selected or the probes are connected incorrectly refer to How to use SampleGuard e The CoolHeat enable pressure is set incorrectly refer to Entering Control Data The Run Data Screen Coolheat Enable Pressure e The heat off elapsed time is not specified or incorrectly specified refer to Entering Control Data The Run Data Screen Heat Off Elapsed Time Pressure e The system will not reach full vacuum Probable cause e The chamber pressure may be controlled refer to Entering Control Data The Select Run Screen Pressure Control Regime e Dri Pure may be selected refer to Entering Control Data The Select Run Screen Pressure Control Regime e There may be a leak in the system Refer to Help General Suspected Leak below e Check the pump oil level if applicable refer to Getting the Best from Your System Routine Checks General e Suspected leak pressure of no better than 5 mbar Probable cause e Contact Genevac Service for assistance Condenser e Condenser not getting to tempera
36. elect 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 removing 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 Pagessore0 SCSCS S lt CS SSS A Issue 2 1 January 2000 Run No 91 Last Used 12 25 03 03 03 L ROTOR SPEED Run Data Locked Next Run Number 0 for none Select Rotor Speed Run Name Sample Holder Type High 500g Sample Volume ml Low 300g Solvent Very Low 50g SampleGuard Control Temperature C SampleGuard Control Channel CoolHeat Enable Pressure mbar Chamber Temp
37. er a group of solvents such as high boiling point The following table provides a guide to the correct run selection 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 1562 Issue 2 1 January 2009 page 37 of 60 Genevac HT 24 series Workstation 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 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 BP Solvent Examples Application Range 51 Volatiles not 60 90 C Ethyl Acetate or Single volatile solvents with no risk of Methanol bumping 52 Very Volatile amp 40 90 C IDCM Methylene Volatile solvent mixtures and DCM DCM Chloride or Methylene chloride where risk of bumping Chl
38. erature Control C AUTO Cool to 32 Control at 20 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 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 acceleration 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 Run No 91 Last Used 14 40 03 03 03 Last Changed 12 35 03703703 Run Data Locked No Next Run Number 0 for none 0 Run Name Example sample Holder Type Deep Well Plate sample Volume ml 0 70 30 lvent Etfic Hex sanpleGuard Control Temperatur HEAT OFF OPTION sanpleGuard Control Channel CoolHeat Enable Pressure mbar Select option for turning off CoolHeat Chamber Temperature Control Rot
39. gress 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 coolant 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 lf 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
40. hannel 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 into 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 19 of 60 Genevac HT 24 series Workstation 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
41. hlighted 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 1562 Issue 2 1 January 2009 page 23 of 60 Genevac HT 24 series Workstation 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 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 N O D D START
42. hout any heat input this cools the holders and helps achieve good freezing in the next stage 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 lyophi
43. ile water the overall length of this stage should be approximately 1 3 as long as the length of stage 2 which 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 End the method using Heat Flow rather than specifying the duration for the stage oS 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 of 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 1562 Issue 2 1 January 2009 page 45 of 60 Genevac HT 24 series Workstation 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 wit
44. ilst a run is in progress It shows the current status of the evaporator in numerical and graphical form 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 10 1562 Issue 2 1 January 2009 Genevac HT 24 Series Workstation 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 No Name Solvent Vol Holder T 1 Oligosynthesis Annonia 2ml DEEP WE 35 2 Oligo Purification Water ACH Onl DEEP WE 3 3 PCR Purification Hater ACH im DEEP WE 38 4 RNA Purification Hater 110ml 44 15 4 5 Oligo Production Aqueous Hixture dnl SH mi T 48 A GEHEVAC LID START EDIT GRAPH CLEAR COPY TO DRAIN Waddliks FLUSH OPTIONS HELP Select Run with TL Wenu Item with keys press START to execute Starts selected Run using parameters stored ta 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 hig
45. is allows the system to achieve better final drying of the sample and to get better evaporation of mixtures of solvents with widely 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 44o Uu 1562 Issue 2 1 January 2000 Genevac HT 24 Series Workstation 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
46. lisation of samples that are grossly insoluble in water These samples crash out once the organic 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 Page4coreoSCSCSCSCS S lt STSSSSS Se Issue 2 1 January 2000 Genevac HT 24 Series Workstation 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 A
47. lose the door Note the system does not allow a new run to start if the Waste Solvent Container is full or if the Waste Solvent Container Door is not closed 10 1562 Issue 2 1 January 2009 page 15 of 60 Genevac HT 24 series Workstation Getting started Data cable connectors Mains power leads Fume hood is shown with Rear panel removed for clarity Workstation Control Panel Page 16 of 60 The following notes provide basic instructions for set up start up and running the HT 24 evaporating system Refer to the relevant sections of this manual for more detailed information on specific steps Setting up Connect the 3 mains power leads to the rear of the system Connect each power lead to a separate mains supply outlet Do not connect the cables to a common mains distribution block Switch on the mains supplies at source Connect the date cables if required Switching on Switch on each evaporator using the ON OFF switch located on the service panel towards the back lower right hand side of the evaporator Note For convenience leave the evaporator switches permanently on the HT 24 controls power distribution Reset the EMERGENCY STOP button if it has been pressed Do not use the emergency stop button to shut down the system on a regular basis Press the Green power ON button the POWER ON LED illuminates and both systems power up 10 1562 Issue 2 1 January 2
48. ls 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 ua Maalala alll UUM 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 Page 2ofr60SCSCSSSCSCSCSCSCS SSd oae 2 1 January 2009 Genevac HT 24 Series Workstation 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 system without checking it is evenly loaded all sample holders are correctly seated and all holders swing freely Miss loading may result in unrecoverable sampl
49. mber Temperature Control C Rotor Speed Heat Off Option Heat Off Threshold End of Run Option End of Run Threshold End of Run Defrost and Drain Pressure Control Regime Controlled Pressure mbar GENEUAC LTD HELP Tl to select ENTER to edit MENU ESC to exit Temperature to maintain using SampleGuard No oO Example Deep Well Plate 0 7 Etfic Hex 46 1 200 AUTO Cool to 32 Control at 20 Low Heat Flow Not Applicable Not Applicable Not Applicable Yes Controlled Pressure ps es 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 bear 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 Genevac HT 24 series Workstation The following details relate to the remaining run profile fields when the Auto Programme function is not used SampleGuard Control Temperature Enter a temper
50. n solid aluminium sample holders Switch on the HT 24 evaporation system select the Run Data screen go to an unused run location and input the following data Run Data Locked secs sainsccoris deininwatienasnatatietanerietiannaas No Next Run Number c ccccseeeseeeeseeeseeeeeeeens 0 Run Name 0000 DMSO 28 x 60 mm tubes Sample Holder Type Solid Aluminium 28 x 60 Sample VOLUN iiss santtccedvnveccotincsiveriaeermevdsaeisaoteannenes 5 SOVEN ee nn eee eee nee eee DMSO SampleGuard Control Temperature 40 SampleGuard Control Channel 1 CoolHeat Enable Pressure cccccseeeee 100 Chamber Temperature Control 0 40 Rotor Speed ccc cece ceccecce sees eeceeeceeeeeeeseeenaes Low Heat Off Elapsed Time ccccceeeeeeees 01 40 End of Run Elapsed Time 0008 01 40 Controlled Pressure 00008 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 1562 Issue 2 1 January 2009 page 35 of 60 Genevac HT 24 series Workstation Dispense the DMSO samples into the vials and place the sample holders into the sample swings Load the sample holders and swings into the ev
51. n the rotor is not spinning and the chamber is at 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 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 from the View Edit Details option on the SELECT RUN screen page 21 of 60 Genevac HT 24 series I Workstation 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 SELEC No Name Solvent Vol Holder T 1 Oligosynthesis Ammonia 2ml DEEP WE 35 2 Oligo Purification Water ACN Onl DEEP WE 36 3 PCR Purification Hater ACN inl DEEP WE 36 4 RNA Purification Hater 10n1 24 X 15 4 5 Oligo Production Aqueous Mixture dnl 58 nl T 46 GENEVAC LTD NENU START EDIT GRAPH CLEAR COPY TO DRAIN JS9TIS FLUSH OPTIONS HELP Select Run with ti Henu Item with keys press START to execute Starts selected Run using parameters stored 2 Run Data Screen Run No 91 Last Used Not yet used Last Changed New entry Next Run Number O for none 8 Run Name Sample Holder Type Sample Volume ml 8 9 Solvent IR Sensor Control Temperature C 26 CoolHeat Enable Pressure mbar 1
52. ne DMA RN Dimethylformamide DMF 984 o 5 S Y Dimethylsulfoxide DMSO to o 2 Y Ethanol EtOH ooo S on y A Y Ethyl Acetate Ema o aa yv _ Hexane He 8K y A Y a a N ew 2 a NMP 1 02 Pyidne ga Tetrahydrofuran THF p __oe9 fr ag Toluene PhMe 0 87 Tri Ethyl Amine TEA ono o o s a lt z lt x lt x lt x lt x lt x z Zx lt lt lt Trifluoroacetic acid TFA ooo oa S A Y Water tO d A Y HCI Thionyl Chloride or Di Ethyl Ether compatibilities are not available lt lt 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 Page 4o60 U A Issue 2 1 January 2000 Genevac HT 24 Series Workstation Waste Solvent Container Empty the Waste Solvent Container periodically An alarm sounds to indicate if the Waste Solvent Container becomes full Open the Waste Solvent Container door proceed as shown then c
53. on can be reduced by up to 30 Linking Runs Mixtures of water and methanol in deep well microtitre plates 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 SIl and HT12 SIl 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 cov
54. on must be made for maintenance access Leave suitable space on either side of the workstation to allow the waste solvent container door and the pump and catch pot door to open Thumbscrews retract or lower the inbuilt jacks Pages oreo M A oae 2 1 January 2009 Genevac HT 24 Series Workstation 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 Safe 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 Integral Swing Tube Holder Tu
55. oor close button A single audible beep indicates when the door is locked and it is safe to proceed A proximity sensor prevents the lock mechanism activating when the door is not closed Extra Precautions for Fume Hood Systems Take care when opening or closing the evaporator doors There is a possibility of hand entrapment between the left hand evaporator door and the side of the fume hood Take care also when closing the fume hood sliding doors Close the evaporator doors first to prevent any chance of the evaporator and fume hood doors colliding 10 1562 Issue 2 1 January 2009 Using SampleGuard SampleGuard Transmitter and Probe he k PAR 4 ies i slal 4 Y 1 Sample holder probe hole 10 1562 Issue 2 1 January 2009 Genevac HT 24 Series Workstation 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 C
56. or Speed Elapsed Time eat Off Option sample Detection Heat Off Threshold End of Run Option End of Run Threshold 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 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 Genevac HT 24 series Workstation 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 It detects dryness when evaporative cooling ceases turns off the IR lamps and then stops the run Note
57. oroform is high 3 5 Medium BP Medium BP solvent or mixture of medium Solvents BP solvents Mixtures of medium and volatile solvents with high risk of bumping No solvents should Rapid pre heat of chamber before a high Chamber for be present BP solvent run swings and samples must High BP solvents 56 High BP 140 140 DMF DMAc DMSO High BP solvents 190 C 57 Very High BP 190 C INMP DMI Very high BP solvents Solvents 58 itri 9 fe be removed before this method is used HPLC Fractions Water amp Acetonitrile HPLC fractions or Methanol 5 Aqueous only 100 C meo pe only Remove Any Drying samples which have not been fully stubborn dried using another method The solvents condenser must be empty before this method is used Page s8 oi 60 T Issue 2 1 January 2000 Genevac HT 24 Series Workstation 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 Performance e Increa
58. plied 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 are 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 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 1562 Issue 2 1
59. ree 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 10 1562 Issue 2 1 January 2009 page 49 of 60 Genevac HT 24 series Workstation Planned Maintenance and Service Whilst every effort is made to design and manufacture the HT 24 workstation 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
60. rkstation Convenient pullout sample shelves provide assistance when loading unloading the evaporators Fume Hood Flow Meter Pullout Sample Shelves The evaporator control software offers the facility to auto program run parameters for any recognised 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 Solid state case heaters and Coolheat radiant lamps heat the chamber and samples The control of chamber temperature sample holder temperature vacuum ramping rate chamber pressure rotor speed and run time are all handled by an embedded PC Lyophilisation Freeze Drying may be achieved by freezing samples before loading into an 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 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
61. rly where Series and Series Il evaporators are used within the same laboratory For example some sample holders designed for use in Series Il 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 If 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 Do not exceed the mass limit under any circumstan
62. se evaporation speed for high boiling point solvents by pre heating the aluminium sample holders e Use the link run facility wnen evaporating solvent mixtures with large differences in boiling point See the section entitled Optimising a Run for details 10 1562 Issue 2 1 January 2009 page 39 of 60 Genevac HT 24 series Workstation 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 looped 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 enter 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
63. ss lamp windows as the rotor spins 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 centrifugal acceleration Page 48 o0 UMMA Tssue 2 1 January 2000 Genevac HT 24 Series Workstation 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 A N cause the sample swings to stick
64. station Amendment Control Form FA Reason for Change Date Issued 2 Changes to Declaration of Conformity February 2004 3 Introduction of new Pre Set runs 51 100 within the software 01 March 2004 4 Introduction of Warranty Statement 26 April 2004 5 Introduction of Entrapment Warning 21 May 2004 6 Updated Images 02 June 2004 7 Definition of acceptable Out Of Balance Criteria 14 July 2004 8 Changes to Declaration of Conformity 21 September 2004 9 Updated Waste Container images and change in Height dimensions 08 December 2004 Information on the correct use of cane ae Probes 28 September 2005 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 HT 24 workstation Your attention is drawn in particular to the section entitled Safety qQ The evaporator should not be discarded in your regular disposal stream Contact your Distributor or Genevac for proper disposal instructions Within the EU it is Genevac s responsibility under the WEEE directive to provide for the recycling of their products Pagesoore0SCSCSCS lt lt
65. sure change reduces The temperature of the sample drops due to evaporative cooling Provided there is sufficient vacuum 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 Pagesoore0SCSCS lt lt S S SS OS Issue 21 January 2000 Genevac HT 24 Series Workstation 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 evaporati
66. 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 Once 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 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 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 Access temperature display POwer supply cable connected with Hidden Key
67. ta T 49 Planned Maintenance and Service 50 Moving the SySteM cccccsssseesssseeeeseeeeeees 50 Additional Equipment c sccseeeeeseeees 51 POND e cater E E 52 POCINICA Dala eirpesr 53 EC Declaration of Conformity 55 Warranty Statement ccccceeeeeeeeeeeeees 55 Amendment Control Form 0 0008 56 Useful Information cccccccseeeseeeeeeeeees 58 Genevac HT 24 series Workstation Introduction The HT 24 Workstation provides very high performance occupies the minimum amount of laboratory space and is easy to use The workstation comprises a trolley with the option of an integrated fume hood two condensers a high vacuum Scroll Pump and a Waste Solvent Container The workstation can accommodate the following evaporator combinations Two HT8 SII two HT12 SII a combination of both or one single evaporator This manual refers to the evaporation system on the left hand side as system 1 or position 1 Scroll Pump amp Catch Pot Door Open HT 24 Workstation Front View Two HT12 Sil evaporators installed Complete with optional Waste Solvent Container fume hood Note The fume hood has 3 Sliding doors not Door Open shown for easy access Either evaporator can run independently or both can run together Each evaporator can simultaneously remove a different solvent provided the solvents do not react within the drain circ
68. the system extremely flexible This manual will guide you through the start up requirements set up needs and operation of the system to facilitate the most efficient procedure to protect your product s integrity and to ensure optimum performance at all times 10 1562 Issue 2 1 January 2009 page 5 of 60 Genevac HT 24 series Workstation 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 A 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 Il product and is intended to operate from normal single phase power supplies This evaporator is designed for use in a degree 1 environment no pollution or only dry non conductive pollution Any maintenan
69. ture 30 C Probable cause e Contact Genevac Service for assistance Electrical e No power to any part of the system e Door does not open system powered up Probable cause e Check the circuit breaker on the mains supply to the system and reset if necessary e Check both the pump and evaporator switches are on e Check the leads mains power to pump and pump to evaporator e Ifthe fault persists contact Genevac Service for assistance Page 52060 MM SOD Issue 2 1 January 2000 Genevac HT 24 Series Workstation Technical Data Mechanical Data 1800 1 5 500 Direct drive 65g maximum per system if both in use 6 HT 12 Condenser SSS aaa Vacuum System 0 1200 mbar S O 0 1200 mbar Electrical UK and Europe 3 x 230Vac 10 50 Hz 1 phase Each supply not greater 13A 3 x Schuko for Europe including Switzerland Denmark amp China 3 x 208V ac 10 60Hz 1 phase Each supply not greater 15A Max power requirement peak Approx 6 5 kW with high power lamps 30Amps estimated Fume Hood Extraction In flow velocity min Extraction pressure 25 50 Pa 10 1562 Issue 2 1 January 2009 page 53 of 60 Genevac HT 24 series Workstation Dimensions Width 1346 mm 1420mm with fume hood 1467mm side doors open i e O 817mm Height 1685mm 1915mm with fume hood Weight 700kg approximately REAR 467 REFERENCE 420 REFERENCE W100 REFE
70. uit and waste container Sample processing can also be staggered whilst one unit runs the other can be emptied and reloaded Page 2o60 MMMM oae 2 1 January 2009 Genevac HT 24 Series Workstation Using smart technology integrated with the Genevac V2 evaporator software each condenser is capable of chilling defrosting and draining independently of the other An Automatic pump and drain valve system removes solvent from the condenser pots Note The Waste Solvent Container must be emptied periodically The drain pump only operates if the Waste Solvent Container is fitted and the Waste Solvent Container Door is shut A load cell monitors the amount of fluid in the Waste Solvent Container A buzzer sounds at a predetermined weight limit and a WASTE FULL lamp illuminates on the control panel Note the volume of waste solvent varies according to the specific gravity of individual solvents A static dissipating safety device contacts the waste solvent at all times WASTE FULL LED lIluminates when Waste Solvent Container is full OPEN CHAMBER 1 Press button to open evaporator 1 OPEN CHAMBER 2 Press button to open evaporator 2 OFF button ON button Press to turn off HT 24 and Press to turn on HT 24 and evaporators evaporators EMERGENCY STOP POWER ON LED Press to use Used in an llluminates when HT 24 is emergency to isolate Mains switched on Power to the HT 24 Workstation Control Panel Each evaporator has an LCD scr
71. uto Defrost and Drain this is a full defrost and drain See appendix C for programming details Please contact your local Genevac representative for further details on run times alternatively please e mail Applications Genevac com 10 1562 Issue 2 1 January 2009 page 47 of 60 Genevac HT 24 series Workstation 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 evaporating 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 gla

The Genevac HT-24 Series II Workstation Systems User Manual

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