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The Genevac HT12 & HT8 Series II Evaporation Systems User Manual

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1. Run Ho 91 Last Used Hot yet used Run Data Locked Hext Run Humber CA for none Run Hane Sanple Holder Type ALTO PROGRAX ai Auto Progranne remaining paraneters YLesl NLol 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 LTD SOLVENT Acetonitrile ACH Annoniun Hydroxide CNHSO0H Chloroform TCE DCH Diethyl Ether DEE DHF DHI DHSO Ethanol EtOH Ethyl Acetate CEtAc Hexane Hex Hethanol He0H HHP TFA THF Toluene PhHe Hater H20 Other C lear Done HELF tL EHTER 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 07 03 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 Chamber 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 No QO Example Deep W
2. January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Optimising a Run This section describes the general principles by which the Series Il control software can optimise evaporation rates Limiting the Chamber Pressure Pressure control can be used to significantly increase the evaporation rate for aqueous mixtures of greater than 30 water when contained in glass tubes and beakers When evaporating these mixtures at pressures of less than 4 mbar ice forms extending the evaporation time By controlling the evaporator at a pressure of 6 mbar ice formation is prevented and the time required for evaporation can be reduced by up to 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 successiv
3. 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 04 4541 Issue 3 1 January 2009 Page 35 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Dispense the DMSO samples into the vials and place the sample holders into the sample swings Load the sample holders and swings into the evaporator ensuring that the vials sample holders and sample swings are correctly and securely located Refer to the 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 Close the evaporator door and press the START key 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 SampleGuard Probe Location Hole Some time can be gained by preheating solid aluminium sample holders to
4. 40 C in an oven Other evaporation run profiles are suggested in the section entitled Optimising a Run The Evaporation Process This section examines the process that occurs within the evaporator during the run When the previously described evaporation run starts the pressure drops steadily as air is evacuated from the chamber and condenser The CoolHeat lamps operate when the pressure reaches 100 mbar and because the chamber is pre heated to 40 C the sample holders quickly reach the pre set temperature The SampleGuard maintains the 40 C temperature ceiling As solvent starts to evaporate the rate of pressure change reduces The temperature of the sample drops due to evaporative cooling Provided there is sufficient 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 Page 36 of 58 04 4541 Issue 3 1
5. 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 04 4541 Issue 3 1 January 2009 Page 47 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems 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 met
6. Il Evaporating Systems Select Run Screen The Select Run screen lists a library of up to 100 evaporation run profiles Unused run locations remain blank and are available for creating new runs Press the Cursor Direction up and down keys to scroll through the run profiles Run profiles are displayed on the screen 10 at a time SELEC No Name Solvent Vol Holder T 1 Oligosynthesis Annonia e2ml DEEP WE 35 2 Oligo Purification Water ACH Onl DEEP WE 3H 3 PCR Purification Hater ACH im DEEP WE 38 4 RNA Purification Hater 110ml 44 15 4 5 Oligo Production Aqueous Hixture dnl SH ml T 48 H 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 paraneters stored m Press the Settings key to enter the Run Data screen see the section entitled Run Data Screen for details START Press the START key to execute the highlighted option Note the Run Log screen is shown when the run starts Press the cursor direction left and right keys to highlight the options on the horizontal menu bar near the bottom of the screen Press the up and down keys move the white band cursor Note The default position for the horizontal menu bar cursor is with START highlighted Press the cursor direction left and right keys to return the cursor to START after using any of the other menu options 04 4541 Issue 3 1 January 2009
7. Page 23 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Functions of the Menu Bar e START Starts the highlighted run e EDIT Alternative route to the Run Data screen e GRAPH Alternative route to the graph displayed by the display key e CLEAR Clears the highlighted run profile e COPY TO The highlighted run profile may be copied to a different location This feature is useful if several similar run profiles need to be created Copy and edit a profile instead of creating each one from scratch 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 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 24 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Run Data Screen Each of the method profiles shown on the Select Run screen is generat
8. Weight Temperature max low 153kg 180kg 45 C HT4 SII 45 C HT4 SII 50 C HT4X SII 50 C HT4X SII 60 C 60 C 1 5 litres HT4 SII 1 5 litres HT4 SII 2 3 litres HT4X SII 2 3 litres HT4X SII 0 4 litres 0 4 litres No No 316 Stainless steel 316 Stainless steel Stainless steel PTFE Stainless steel PTFE Temperature max high Vacuum pot capacity Exhaust pot capacity Condenser level detector Condenser chamber Condenser drain valve Pressure resolution 1 1000 mbar 1 1000 mbar Vacuum control 1 1000 mbar 1 1000 mbar Dri Pure Yes Yes Auto vacuum vent valve Yes Yes Rapid defrost Yes Yes Ultimate system vacuum 0 4 mbar 0 4 mbar Vacuum Pump Serol Weight 28kg 28kg Maximum vacuum 0 15 mbar 50Hz 0 15 mbar 50Hz 0 12 mabr 60Hz 0 12 mabr 60Hz Flow rate Bem Bem Vacuum pump CVP Weight 52 zo 52 zo Maximum vacuum 0 15 mbar 0 15 mbar Flow rate 3 6 mh 3 6 mh Evaporator W xD x H 562 x 700 x 828 older build 660 562 x 700 x 828 Condenser 515 x 590 x 425 515 x 590 x 425 Scroll pump 530 x 305 x 398 530 x 305 x 398 CVP oa S ooo m x 290 x 405 D x 290 x 405 Power ee single phase 9A i lt 50Hz sam 50Hz AE 60Hz e 60Hz Operating Environment Ambient temperature 15 sceso to 30 C 15 scese to 30 C Relative humidity 10 60 10 60 Altitude Sea level to 12 000m Sea level to 12 000m Storage Environment Ambient temperature 10 C to 60 C 10
9. a lt e N Ez a ees wi Sample Holder correctly seated The Series 1 design is easy to distinguish The corners are not welded MAX MASS FOR SERIES 1 9009 a Ang la oa ANGLE x Sample Holder on edge of swing SZ 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 Page 12 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Balancing Sample Holders and Swings Opposite pairs of swings must be balanced within 10g and the swings must be of the same A type and version Please note that there are several versions of Side Bridge Swings in circulation with a static weight ranging from 375g to 445g Place swings of the same static weight in diametric opposition on the rotor ideally use the same version of swings in all four positions of each rotor level Genevac systems have some inbuilt tolerance for imbalance and a safety system which stops the rotor if the out of balance is unacceptably high However to minimise noise nuisance and wear and tear the balance limit should always be observed If the evaporator is to be partially loaded always fill the top rotor level first Then fill the second level then the third third level applies to HT12 SIl evapor
10. clear the error from the screen RUN 91 Example RUN 91 Channel 1 Temperature C Channel 1 Temperature C Channel 2 Temperature C Channel 2 Temperature C Chamber Temperature C Chamber Temperature C Condenser Gas Temp C Condenser Gas Temp C Pressure mbar Pressure mbar Spin Rate rpn Spin Rate rpm 1666 Total 66 63 64 This Stage 66 03 44 Total 66 45 43 End of Run 46 82 32 pinning 00 Lheat 2pinning pill 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 04 4541 Issue 3 1 January 2009 Page 31 of 58 The following screen appears after the run finishes RUN 91 Exanp le ALARMS Channel 1 Temperature C C TxD Channel 2 Temperature C TxD Chamber Temperature Condenser Gas Temp Pressure Crmbar Spin Rate Crpn c Cc 26 c Cc 24 1137 4 Total 44 46 15 End of Run 44 44 4A Channel 2 Pressure Spin Rate MM mbar RUN FINISHED 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
11. outwardly similar to the HT12 SIl but may be distinguished by a two tier rotor where the HT 12 SIl has three tiers Solid state case heaters and Coolheat radiant lamps heat the chamber and samples The control of chamber sample holder and sample temperature vacuum ramping rate chamber pressure rotor speed and run time are all handled by an embedded PC Page 2 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems The system 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 Evaporator Screen and Keypad The status of the system is shown on an LCD screen Programming input is via a keypad and simple to use up down controls enable the run time rotor and chamber temperatures to be set in an instant Lyophilisation Freeze Drying may be achieved in LyoSpeed enabled systems fitted with an Auto Defrost amp Drain condenser Samples must be frozen before loading into the evaporator Automatic end of run shut down may be programmed manually with a simple time setting or may be achieved by automatic end of run prediction using Heat Flow or Sample Detection methods The Run Progress screen has a fully featured graphical display providing annotated plots for
12. 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 Page 28 of 58 04 4541 Issue 3 1 January 2009 OoOo o o E B a 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 Lou 50g SampleGuard Control Temperature C SampleGuard Control Channel CoolHeat Enable Pressure mbar Chamber Temperature Control C AUTO Cool to 32 C
13. 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 the system extremely flexible This manual will guide you through the requirements for setting up operating and maintaining the system It will facilitate the most efficient procedures to protect your product s integrity and ensure optimum performance at all times 04 4541 Issue 3 1 January 2009 Page 3 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Safety Safety Symbols The following safety symbols are used throughout this manual and are defined as follows Hazards that can be harmful to health or lead to serious damage or injury Possible risk to sample integrity Genevac Evaporators and Combustible Solvents Please note it remains the responsibility of the user to consider safety when evaporating any combustible solvents and to place the system in a well ventilated environment Genevac s position regarding evaporation of such solvents particularly with respect to the European ATEX directive is available on our website or from your local sales representative Electrical Safety Important the system must be earthed This evaporation system is a s
14. the defrost menu Select START to begin the defrost cycle VARIABLES 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 ie Defrost __ Completed when 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 Issue 3 1 Jan Enter the Select Run screen and press the STOP key SELECT RUN No Nane 50 lvent Vol Holder T xt 91 Example Etc Hex iml Deep We 40 0 gz 93 PURIFICATION WATERSACETONITRILE 10m 18 X 15 94 SOLID PHASE SYNTH TFASDCH eml DEEP WE 95 COMPOUND f CONFIRM REQUEST 396 OLIGO SYN Shut down evaporator Are you sure CYH 9 SOLUTION amp 96 SOLUTION PHASE 2 DCHNME THANOL iml DEEP WE 99 MAINTENANCE TEST 1 Om MAINTENANCE TEST 2 Om GENEVAC LTD MENU vie EDIT GRAPH CLEAR COPY TO DRAIN DEFROST FLUSH OPTIONS HELP select Run with Tl Menu Item with gt keys press START to e
15. 0 40 for MeCN Dri Pure End Pressure E ao for MeOH Dri Pure Dri Pure Ramp Time Time Final Control Pressure 40 boa MeCN 45 for MeOH Notes Remove organic Remove most of the Remove final phase aqueous phase stubborn solvents Page 52 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Fast Lyophilisation of HPLC Fractions a HPLC Fractions Run Data Locked O N N OO O ON OK Next Run Number 2 B 4 O Oo oe Lyo part Lyo part Neal Lyo part Fractions Lyo Sample Holder Type rrr Holder rr Holder Geeta Holder couse Holder Sample Volume ml Your Volume Volume Your Volume Volume Your Volume Volume Your Volume Volume Solvent MeCN or MeOH MeCN or MeOH MeCN or MeOH MeCN or MeOH ooo a H20 oo H20 mooo H20 mn H20 aee a e Temp C 40 40 e Channel 1 1 1 1 procure boo Pressure Seer eas pated fant pat control preheat to 25 preheat to 0 preheat to O preheat to 30 Rotor Rotor Speed sits High is High Heat Off Option Elapsed Time Elapsed Time Elapsed Time Elapsed Time Heat Off Elapsed Time lask for time 0 00 _ 00 00 05 00 End of Run Option Elapsed Time Elapsed Time Elapsed Time Elapsed Time End of Run Elapsed Time ask for time 0 30 01 00 10 00 Auto Defrost amp Drain es ee ee caer ett Se puvacum cam Regime Variable Dri Pure Pressure Full Vacuum Full Vacuum eee a a a mbar 175 a a moa 45 for MeOH Dri Pure Dri Pure Ramp Time Time Final Control Pre
16. 5 September 2006 2 13 Drain Converted to print A5 Booklet 08 December 2006 2 15 Add Maintenance of Rotor Swings and Sample Holders 09 April 2008 2 16 Update page footers 04 June 2008 Reformat layout remove mega references default to current build 3 1 version amp include old builds as variances 26 January 2009 Update Statement of Conformity Update sample holder images 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 HT8 or H1I12 Sll evaporation system Your attention is drawn in particular to the section entitled Safety The evaporator should not be discarded in your regular disposal stream Contact your Distributor or Genevac for proper disposal a instructions Within the EU it is Genevac s responsibility under the WEEE directive to provide for the recycling of their products 04 4541 Issue 3 1 January 2009 Page 57 of 58 Genevac Limited The Sovereign Centre Farthing Road Ipswich IP1 5AP United Kingdom Sales and Service Hotlines Service Hotline 44 0 1473 243000 Sales Hotline 44 0 1473 240000 Fax 44 0 1473 461176 Email mailto salesin
17. 53 54 56 57 58 59 Page 38 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Getting the Best from the System Routine Checks For high boiling point solvents such as DMSO NMP DMF and DMI the best evaporation rates are achieved at pressures better than 0 5 mbar Carry out the following checks regularly to ensure optimum vacuum performance Check security of all clamped joints Drain the condenser pots before every run Check the pump exhaust catch pot regularly and drain as necessary Keep a log of the time taken for your system to reach full vacuum and use it to indicate deterioration of performance due to seal ageing and wear Tips for Improving System Performance e Increase 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 Further Notes for CVP Pumps Check the pump oil level weekly Ensure the oil level is within the notch on the dipstick Top it up if necessary using the correct grade of silicon oil Correct Oil level centre of dipstick notch Pump Type Part Number CVP100 CP SCF025 AS1616 1 litre CVP100 CPC Crylin 614 AC2310 1kg Do not apply vacuum to a recently defrosted condenser containing traces of liquid DMF DMSO or NMP This is likely to cause pump
18. C to 60 C Relative humidity 10 80 10 80 Altitude Sea level to 12 000m Sea level to 12 000m 04 4541 Issue 3 1 January 2009 Page 55 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems EC Declaration of Conformity We Genevac Limited declare that this product Series Il Evaporating System Complies with the relevant Essential Health and Safety Requirements of the European Machinery Directive 98 37 EEC the EMC Directive 89 336 EEC and the Low voltage Directive 73 23 EEC Conformity is demonstrated by compliance with the following specifications EN 60204 1 2006 Safety of machinery Electrical equipment of machines Pt 1 General Requirements EN 249 1992 Safety of machinery Safety distances to prevent danger zones being reached by upper limbs EN 1088 1995 A1 2007 Safety of machinery Interlocking devices associated with 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 general requirements Warranty Statement This product is guaranteed for period of 12 months from the date of delivery to site In the unlikely event of any defect arising due to faulty materials or construction resulting in system failure the unit w
19. Off Turns off the key press beep response User Intervention Beeps On Off Turns off the user intervention beep response End of Run Beeps On Off Turns off repeating end of run alarm Press the ESC key to leave these menu screens Page 34 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Starting a Run This section describes the steps required to carry out a typical evaporation run for DMSO In this example two sets of eight 28 x 60 mm scintillation vials each containing 5 ml of DMSO are placed in solid aluminium sample holders Switch on the HT8 or HT12 SIl evaporation system select the Run Data screen go to an unused run location and input the following data Run Data Locked ccc cceccceeeeeeeeeeeeeneeeenes No Next Run Number cccccccseeeceeeeeeeeeeeeeneeees 0 Run Name 0c00 DMSO 28 x 60 mm tubes Sample Holder Type Solid Aluminium 28 x 60 Sample VoOlUMe cccccc cece seeeeeeeeeeeeeteeeaeeanes 5 S10 12 en ee eee eee DMSO SampleGuard Control Temperature 40 SampleGuard Control Channel 0 0000 1 CoolHeat Enable Pressure cccccseeeee 100 Chamber Temperature Control 40 Rotor Speed Ss ieiisncissnessdecnvendavenscisdpenndcsnienennumerions Low Heat Off Elapsed Time ccccceeeeeeees
20. The evaporator monitors the sample temperature It detects dryness when evaporative cooling ceases turns off the IR lamps and then stops the run Note Two temperature probes are required for Sample Detection See Using the SampleGuard for details Note Evaporators with IR temperature control have no sample guard transmitter and do not offer the Sample Detection option for of end of run detection Set the IR Control Temperature in the same way as the SampleGuard Control Temperature End of Run Defrost and Drain Select yes to defrost and drain condenser at the end of the stage See 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 Page 30 of 58 04 4541 Issue 3 1 Januar
21. afety 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 II 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 maintenance 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 The HT8 SII and HT12S Il evaporation system 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 Page 4 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Options Available options include e Bump protection Dri Pure and Variable Dri Pure e High power Coolheat lamps e Low UV lamp lenses Data Logging is available The easy to use package provides the data needed for process and quality control Hardware Required e PC running Windows 95 98 NT 2000 or XP e Around 5Mbytes of free space on your hard drive e Serial Port on the PC or USB to Serial Adapter e Serial Cable to connect the PC to the Evaporator Contact
22. age 20 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems 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 Press the START and STOP keys to start and stop the selected run Press the Cursor Direction Keys to move around the screen in the direction of the arrows Press the Enter key to open or close fields in the Run Data screen for inputting or amending data Note the START key acts Enter as an enter key when the keyboard is not illuminated Press the Menu key to display the User Menu screen This only operates when the rotor is not spinning and the chamber is at Menu atmospheric pressure Press the Display key to show the graph from the last completed run This function only operates when a run has been completed Display Press the Cursor Direction Keys to show different segments of the graph Press the Settings key to display the Run Data screen for the selected run Note the Run Data screen can also be accessed Settings from the View Edit Details option on the SELECT RUN screen WE Bop 04 4541 Issue 3 1 January 2009 Page 21 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Control Screens an Overview There are thr
23. al 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 sample loss damage to equipment and could A 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 4 a m k PA 4 rs y MTAMA ces Awaba t Con 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
24. arts in the field is complex and demands a high level of skill To this end Genevac offers a range of preventative maintenance service and breakdown contracts Moving the System Refer to the section entitled Positioning the Evaporator Refer also to the following notes if it is necessary to move a system to a new location Address the following key points before moving an HT8 or HT12 SIl evaporation system e Clear sufficient bench of fume cupboard space to accommodate the system at the new location e Ensure there is access to a power supply two separate mains sockets are required e Ensure there is adequate ventilation e Make provision for the drainage of waste solvents 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 e Remove and retain all the clamps seals tubes cables and instructions 04 4541 Issue 3 1 January 2009 Page 45 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Additional Equipment Genevac supply a range of swings and sample holders which may be utilised to adapt existing systems for new applications All sample holders are of a solid aluminium construction and are black anodised to improve heat absorption Solid aluminium tube holders provide even heat distribution for uneven drying loads Maximum contact areas provide good physical support optimum heat transfer and even heat
25. at 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 04 4541 Issue 3 1 January 2009 Page 25 of 58 Run Ho Run Data Locked Hext Run Number CH for none Run Hane Solvent Sanple Holder Type Sanple Vo lune Hicrotitre 7 Last Used CHot yet used Last Changed CNew entry SAHPLE HOLDER Select Sample Holder Plate Deep Hell Plate Tube Yial Holder SanpleGuard Control Temperature C SanpleGuard Control Channel CoolHeat Enable Pressure mbar Hininum Chamber Temperature C CIJ Rotor Speed Heat Off Option Heat Off Elapsed Time CHH HH End of Run Option End of Run Elapsed Time CHH HHIJ Pressure Control Regime Dri Pure Final Controlled Pressure Cmbar GENEVAC LTD High Elapsed Tine HH 48 Elapsed Tine HH 48 Dr i Pure H HELP tl to select ENTER to accept ESC to cancel Sanple holder type to be entered Select a sample holder type from the window that opens If the required sample ho
26. at the condenser drain connectors are accessible Connect the heated inlet tube to the condenser heated inlet using an appropriate clap and centre ring Connect the other end of the heated inlet tube to the evaporator vacuum inlet Plug the heated inlet power lead into the heated inlet power socket on top of the condenser Screw the Pressure head into its connector on top of the condenser Connect the sensor cable from the condenser and secure it using the screw supplied Connect suitable pipes not supplied except for LyoSpeed systems to the spigots of the condenser drain outlet Place the other end of the drain pipes in a suitable waste solvent container not supplied Ensure the end of the drain pipes cannot be submerged in the waste solvent Heated inlet tube Do not submerge waste solvent pipes Connect the condenser cable to the socket on the side of the evaporator Connect the other end of the cable to the socket on the condenser Note The condenser cable has 19 way QM connectors a male connector at one end a female connector at the other end and only connects to the corresponding sockets in the correct orientation Fit the pump control box to the pump using the connectors clamps and fasteners supplied Fit the exhaust catch pot bracket and catch pot assembly to the pump Push the exhaust outlet adapter into the pump exhaust outlet and connect the pipe supplied from the exhaust outlet to the catch pot Connect the 25KF
27. ators 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 8mls per well On the other swing the reverse is true The two swings now weigh the same However if placed opposite each other in on a rotor would be imbalanced This is because when the swings rotate to their operating attitude the centre of mass of one is at a different radius to that of the other MULL lable slaan aalala I 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 04 4541 Issue 3 1 January 2009 Page 13 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Good Procedur
28. ature C Chanber Tenperature c Condenser Gas Temp L C3 Pressure nbar Spin Rate rpn Total 66 63 84 This Stage 46 83 84 Spinning 00 nea Eva pora ti ng Page 22 of 58 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 whilst 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 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series
29. ay also be thrown onto the side of the chamber and the Quartz glass lamp windows as the rotor spins oe a a aM Whilst the solvent evaporates the product becomes carbonised by the heat from the lamps and forms sites where crack propagation can occur Inspect the lamp glass at regular intervals and clean with a lint free cloth and acetone Contact Genevac Service if the contamination becomes excessive and carbonised as shown A range of specialised sample holders is available to protect the Quartz lenses Contact Genevac Sales for details Bumping Bumping can also cause product to deposit on the glass lenses as previously described It is unpredictable and may occur with any solvent or mixture it is also a potential source of cross contamination between samples Avoid bumping by selecting the Dri Pure option from the Pressure Control Regime drop down menu on the Run Edit screen This option sets a high rotor speed and avoids super heating the samples by reducing the pressure in the vacuum chamber by gradual increments Evaporation begins progressively and samples are contained due to the higher centrifugal acceleration 04 4541 Issue 3 1 January 2009 Page 43 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Maintenance Refer to the section entitled Getting the Best from Your System for details of routine maintenance checks This section describes some further proactive maintenance procedures Excessive build up o
30. convoluted vacuum tube to the pump vacuum inlet with an appropriate clamp and centre ring Connect the other end of the convoluted vacuum tube to the condenser vacuum inlet Connect a length of exhaust tube to the spigot on top of the pump catch pot assembly and secure it with a pipe clamp Cut the pipe to an appropriate length and connect the other end of the exhaust tube to horizontal spigot of the condenser exhaust inlet Cut a length of exhaust tube approximately 300mm and connect it to the top vertical spigot of the condenser exhaust inlet Secure it with a pipe clamp Connect the other end of the pipe to a spigot of the T piece Page 8 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Cut another short length of exhaust tube approximately 200mm and connect it to the condenser exhaust outlet secure it with a pipe clamp Connect the other end of the exhaust tube to s spigot of the T piece Connect the remaining exhaust hose to the T piece Connect the other end of the exhaust tube to an appropriate laboratory fume extraction system See the diagram entitled Pipe Connection Overview for details Connect the pump control cable to the pump control cable socket on the pump Connect the other end of the pump control cable to the pump control cable socket on the side of the evaporator Note The pump control cable has 8 way QM connectors a male connector at one end a female at the other end a
31. ctivity 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 particularly 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 not
32. distribution The following accessories are an example of the many ways in which Genevac can assist in developing your system for the future For further information or to discuss any requirements please call Genevac Sales using the contact details on the back cover of this User Manual Side Bridge FastStack for shallow well plates FastStack for deep well plates Flask holder One piece holder for 50m lTubes Sample Genie Page 46 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Auto Defrost Drain Auto Defrost and Drain is a condenser option for the Genevac HT4X HT8 and HT12 series 2 evaporation systems and is standard on the HT 24 Workstation Auto Defrost and Drain enables the system to e Automatically drain the condenser of volatile solvent s between method stages e Automatically drain the condenser at the end of the method The Auto Defrost and Drain system requires no user intervention When performing an intermediate drain i e mid method the system also performs a short defrost in case residual solvent from a previous use is frozen in the outlet pipe of the condenser The intermediate drain removes volatile solvents which do not freeze at temperatures above 50 C Benefits of Auto Defrost amp Drain The principal benefit of the Auto Defrost and Drain function is to eliminate volatile solvent s from the condenser The volatile component of a mixture boils off fi
33. e For evaporators equipped with infra red temperature control set IR Control Temperature instead of SampleGuard Control Temperature ji 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 03703703 Kun Data Locked No Next Run Number 0 for none 0 Run Name Example sample Holder Type Deep Well Plate sample Volume ml 0 70 50 l vent Et c Hex sanpleGuard Control Temperature 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 Automatic Control Heat Off Threshold End of Run Option End of Run Threshold Not Applicable End of Run Defrost and Drain Yes Pressure Control Regime Controlled Pressure Controlled Pressure mbar 10 GENEVAC LTD HELP Tl to select ENTER to accept ESC to cancel Chamber temperature controlled to suit
34. e 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 Run Name BP Solvent Examples Application Number Range 51 Volatiles not 60 90 C Ethyl Acetate or Single volatile solvents with no risk of DCM Methanol bumping Very Volatile amp 40 90 C IDCM Methylene Volatile solvent mixtures and DCM DCM Chloride or Methylene chloride where risk of bumping Chloroform is high Medium BP 90 DMF or Toluene Medium BP solvent or mixture of medium Solvents 155 C BP solvents Med BP amp 40 DMF amp DCM Mixtures of medium and volatile solvents Volatile 155 C Methylene Chloride with high risk of bumping 55 Pre heat No solvents should Rapid pre heat of chamber before a high Chamber for be present BP solvent run swings and samples must be removed before this method is used solvents High BP 140 140 DMF DMAc DMSO High BP solvents 190 C Very High BP 190 C NMP DMI Very high BP solvents Solvents HPLC Fractions Water amp Acetonitrile HPLC fractions or Methanol fee only 100 C meo pe only Any Drying samples which have not been fully stubborn dried using another method The solvents condenser must be empty before this method is used 52
35. e Genevac HT12 amp HT8 Series i Evaporation Systems User Manual Issue 3 1 January 2009 Part Number 04 4541 Contents INTOGUCHON setinecinncmancanaieianasevetadsuwseimedeentxesuns 2 By ess ise on E A Safety SYMbOIS cccccccsseeeeeeseeeeeeeeeeeeseeeeeeens 4 Genevac Evaporators and Combustible SOIVENIS aine E e ee ee 4 Electrical Safety ccccccsssseeccsseeeeesseeeseeeees 4 Limitations Of USC ccceccceecceseeeeeeeeeeeeeeenseees 4 RN OURS soriman 5 Delivery and Installation cccceeeeeeees 6 Checking the Delivery ccccccesseeeeeeeeeeees 6 Arranging COMMISSIONING 0ccecseeeeeeneeeees 6 ERMC wientiia ne parti T E 6 Positioning the Evaporator cccceeceeseeeeeees 6 Pipe Connection Overview ccceeeeeeeeeeeees 6 Identifying the parts ccccceeeceesseeeeeeeeeeeeeeees 7 SAY 2 06 2 0 earn ene eee eee ee ee eee en T 5161 6 PUMO erreia a nee eee ne 7 ISS OE oiri des sete tecins aedins Nee madera anes 7 Installing the System ccccececesseeeeeeseeeeeeeaees 8 Intsallation Variations Lyospeed Systems 9 Installation Variations CVP Vacuum Pump 9 Safe Loading of Rotor General Document PE A EE aban An Sine Ran E 10 Nomenclature cece cece ceececeeeeseeeeeeeeeeeeeseeees 10 Use of Correct Accessories 0 ccceseeeeeee ees 11 Adherence to Mass Limit ccccseeeeseeeeee
36. e runs can be linked at reduced SampleGuard temperatures and different pressures Some experimentation is necessary to ensure that safe sample temperatures are not exceeded Pre programmed Runs HT8 and HT12 SII evaporators are pre programmed with a number of evaporation methods These runs are located at 51 to 60 of the RUN selection screen Desired runs can be copied to other locations using the copy to function Runs 61 through to 98 are all associated with these pre programmed methods and runs 99 and 100 are for use by Genevac service engineers please do not alter them The pre programmed runs are designed to cover a group of solvents such as high boiling point The following table provides a guide to the correct run 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 04 4541 Issue 3 1 January 2009 Page 37 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems The pre programmed runs are designed to make use of all the appropriate features of the system and to provide optimal evaporation conditions All methods make use of the automatic end of run detection feature so that run times do not need be set the system stops when all the samples ar
37. e 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 circumstances 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 04 4541 Issue 3 1 January 2009 Page 11 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Loading Sample Holders into Swings and series Il equipment is used in the same f This information is applicable where Series 1 laboratory There are two possible ways in which a sample holder may be miss loaded into an older type of swing One is to rotate the sample holder such that its corners rest on the edges of the swing The other is to place the sample holder so that one side rests on the edge of the swing Diiss Sample Holder rotated Both these modes of miss loading are possible with a Series 1 open or standard swing but are virtually impossible with a Series Il swing Care must still be taken when loading the samples i z amp lt a
38. e the door so that the screen may be viewed but do not lock it This prevents any chance of inadvertently starting the rotor with the power supply cable connected 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 The SampleGuard system will not operate without the Stuffer Plug fitted Page 19 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems The Condenser The condenser starts automatically a short time approximately 3 minutes after the evaporator is switched on There is a further short delay before the condenser reaches operating temperature Drain the condenser defrost first if necessary before each run and at the end of each day Access the DEFROST DRAIN CYCLE for the condenser via the HT8 or HI12 SIl Select Run Screen Manual Defrost and Drain To start the defrost cycle move the cursor to the DEFROST DRAIN CYCLE using the up down cursor keys and press the ENTER key The DEFROST VALVE opens and the defrost cycle begins The required frequency of defrosting a
39. ed 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 CHew entry Hext Run Number CH for none Run Hane Solvent Sanple Holder Type Sanple Vo lune SanpleGuard Control Temperature C CI SanpleGuard Control Channel CoolHeat Enable Pressure Cobar Hininun 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 HA BA Pressure Control Regine Controlled Pressure Controlled Pressure Cnmbar GENEVAC LTD HELP Tl to select ENTER to edit MENU ESC to exit Press the cursor direction up or down keys to move between fields Press the Enter key to open a field Enter a new value for the relevant parameter and press the Enter key again to close the field Run Parameter Details Run Data Protection The run profile may be protected against accidental alteration Set the Run Data Protection field to No before attempting to edit an existing run profile Set the Run Data Protection field to Yes to lock the profile Next Run Number Runs may be linked together Enter the number of the run th
40. ee main control screens The information on this page is a brief overview of what the screens do Detailed descriptions are provided in following sections 1 Select Run Screen No Name Solvent Vol Holder T 1 Oligosynthesis Ammonia 2ml DEEP WE 35 2 Oligo Purification Water ACN Onl DEEP WE 3 3 PCR Purification Hater ACN inl DEEP WE 3 4 RNA Purification Hater inl 24 X 15 4 dni 58 nl T 46 5 Oligo Production queous Mixture GENEVAC LTD NENU START EDIT GRAPH CLEAR COPY TO DRAIN Magui FLUSH OPTIONS HELP Select Run with tl 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 Hun Data Protection No Next Run Number O for none 8 Run Name Sample Holder Type Sample Volume ml Solvent 8 0 IR Sensor Control Temperature C 28 168 Wait to cool to 20 High CoolHeat Enable Pressure mbar Chamber Temperature Control C Rotor Speed Heat Off Option Heat Off Elapsed Time HH MM End of Run Option End of Run Elapsed Time IHH MM End of Run Defrost and Drain Pressure Control Regime Final Controlled Pressure mbar Elapsed Time 66 68 Elapsed Time No Dr i Pure 0 0 GENEUAC LTD HELP t to select ENTER to edit MENUVESC to exit R Dat rotection Select level of Run Data 3 Run Log Screen RUN 91 Example Channel 1 Tenperature C Channel 2 Tenper
41. eeeeeeeeneeeeeees 33 Options Menu c ccccceeeeeeeeeeeeeeeeeeeeeeees 34 Starting a PRU iccsecccceetsencttenraesiecreisevericuepescce 35 The Evaporation Process ccceseeeeeees 36 Optimising a PUM aie ietercetinteicecctccdeecsercain 37 Limiting the Chamber Pressure 0005 37 TG RUNS ve antancrananlannccestansichsornavtinataxesoiun 3 Pre programmed RUNS cccsccccseeeeeeeeeeeeees 37 Getting the Best from the System 39 Routine Checks 1 00 ccceecceceeececeeeeeeeeeeeeeeeeenes 39 Tips for Improving System Performance 39 Further Notes for CVP Pumps 008 39 Run Parameters Quick Reference 40 Problem Prevention ccsccsscsssseeeeseeenees 43 CONCENSATION ccccecceceececeeeeeceeeeeeeeeeeseeees 43 TFA Creep Ree ne een eee eee eee 43 BUMPING ecreis 43 MaintenanCce ssssssnsnssnnnnnnnnnnnnnnnnnnnnnnnnnnne Ad Cleaning the Sample Holders and Swings 44 Cleaning the Chamber Rotor and Swings 44 Scroll PUMP sereine iaae 44 Planned Maintenance and Service 45 Moving the System cccecseeeeeeseeeeeeaeeeenens 45 Additional Equipment ccceeeeeeees 46 Auto Defrost Drain ccscceseeeeeeeeeeeeees 47 Benefits of Auto Defrost amp Drain 0 47 8 16 ee nC ee ee ee ee 47 HOW WV OV ICS osercee cetescecstatanee Ainan EER 48 When to use Auto Defrost a
42. ell Plate 0 7 Etc Hex 4E 1 200 AUTO Cool to 324 Control at 20 Low Heat Flow Not Applicable Not Applicable Not Applicable Yes Controlled Pressure 9 5 GENEUVAC LTD HELP Tl to select ENTER to edit MENUYESC to exit Temperature to maintain using SampleGuard The screen shows the automatically programmed run parameters in blue These parameters may be overwritten manually Manually overwritten parameters are shown in white Note There are a couple of restrictions to 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 f ue 3 1 January 2009 Page 1 4 Issue 3 9 age 27 of lt Genevac HT8 amp HT12 Series Il Evaporating Systems The following details relate to the remaining run profile fields when the Auto Programme function is not used SampleGuard Control Temperature Enter a temperature value between 20 and 70 C The system heats the sample holders to this temperature Not
43. ems Note Significant cooling and possibly freezing occurs during evaporation the extent is dependant upon the solvent It is advisable to position the sample probe in a sample near the centre of the holder Since the central wells are surrounded by other frozen or cold wells there is a significant thermal drain during evaporation This effect is particularly prevalent when using microtitre plates Under these conditions dryness may occur in the outer wells whist the central samples remain in solution or frozen The use of Genevac Heat Transfer Plates is beneficial in reducing this effect by providing an even heat transfer across the plate When positioning the sample probe always ensure that the probe tip is located firmly at the bottom of the well vial or tube 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 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 Clos
44. enser and spoil the level of vacuum achieved in the latter stages of the run Page 48 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems When not to use Auto Defrost and Drain There are certain circumstances when Auto Defrost and Drain should not be used This is to protect the system and or samples from solvent damage Do not use Auto Defrost and Drain in the following circumstances e 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 defr
45. f debris on the pivoting faces of the sample swings and rotor can AN cause the sample swings to stick in the out position when the rotor stops This can cause unrecoverable sample loss Cleaning the Sample Holders and Swings Regular inspection and maintenance of swings and sample holders should be performed at least monthly The following inspection routine is mandatory following any tube breakage or solvent spillage Never use wet swings or holders in an evaporator Visually inspect the sample holders monthly Clean off any debris especially in the sample holder wells as this may cause high points that lead to stress in the glassware resulting in breakage The main cause of repeat glassware breakage is fragments from a previously broken tube Solvent can stick the glass fragments to the holder making it difficult to remove Residual solvent or sample material must be cleaned off Superficial surface damage e g scratches do not affect the performance of a holder or swing However if there is any structural damage if any part of the holder swing or rotor is bent or deformed do not use it 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 t
46. fo genevac co uk Web site http www genevac com Genevac Inc SP Industries 815 State Route 208 Gardiner NY 12525 United States of America Sales and Service Hotline 1 845 267 2211 Fax 1 845 267 2212 Email salesinfo genevacusa com Useful Information lf you need to contact Genevac for assistance use either the telephone or fax Hotlines shown It always helps Genevac Service if you have the serial numbers at hand for the components of your system lf you need to contact Genevac Sales for information on Service Contracts or products use the telephone or fax Hotlines shown Alternatively Email or visit our web site These instructions are subject to change without notice No part of these instructions may be reproduced in any form or be processed duplicated or distributed by electronic or optical means without the written permission of Genevac Limited All rights reserved Genevac Limited Read these operating instructions before using the Genevac HI12 SlIl Evaporating System Keep them near the system for easy reference Your attention is drawn in particular to the section entitled Safety
47. 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 arun The solvents with an N against them must be entered using the Other option and the rest of the data entered manually 04 4541 Issue 3 1 January 2009 Page 15 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Getting Started CVP pump power switch Evaporator power switch Software Control Screen Page 16 of 58 The following notes provide basic instructions for starting up the evaporation system Refer to the relevant sections of this manual for detailed information on specific steps Switching on the Pump Connect the pump to the mains and switch on the mains Switch on the pump power switch Note The pump does not start until the evaporator is switched on Switching on the Evaporator Switch on the evaporator power switch There is a short delay while the imbedded PC completes its boot up sequence The display shows the Software Control screen The system is now in stand by mode Press the START key to start the system e The pump starts e The display shows the Run Select screen e The condenser starts after a delay of approximately three minutes Note The system is not available for use until e The pump reaches its operating temperature CVP pumps o
48. he third connector for normal system operation Insert the Channel 1 control channel temperature probe into the small probe hole in one of the sample holders Insert the Channel 2 temperature probe into a sample tube vial well etc Press the SETTINGS key to display the Run Data screen Use the cursor keys to select the SampleGuard Control Channel field and select channel 1 as the control channel Note Only use the option to select channel 2 as the SampleGuard Control Channel if there is a fault with channel 1 or its associated temperature probe In this instance insert the channel 2 probe 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 04 4541 Issue 3 1 January 2009 Sample Guard Stuffer Plug Access temperature display with Hidden Key Comparison Thermometer 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Syst
49. hod the system a full defrost and drains the condenser automatically When to use Auto Defrost and Drain Auto Defrost and Drain has two main functions 1 To automatically drain the condenser mid process to eliminate volatile solvents enabling the system to reach full vacuum in the later stages of evaporation This allows the system to achieve better final drying of the sample and to get better evaporation of mixtures of solvents with 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 cond
50. holders supplied with the system or that are specified for use with the system Never use non Genevac approved sample holders Genevac Ltd will not accept responsibility for any loss or damage incurred by improperly or excessively loaded rotors Page 14 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Solvents Common Acceptable Solvents Autoprogram Available Density g cm Density Temp C Acetonitrile ACN Ammonium Hydroxide NH3OH _ 2 Dichlroetine OGE T a0 Diehioromethane OGM fg fg eee ou 0 94 Dinetylemine OMA oe a0 a a a a a a e E 1 10 Ehenol OH 0 Ethyl Acetate Em o a yv Hexane He y w Y S Isopropanl ON Methanol MeQH Dw y Y SOS N Methyl 2 pyrrolidone NMP 1402 J o 5 S Y O S NN Tetrahydrofuran THF ose w2 Y O Toluene PhMe o o o o S S Tri Ethyl Amine TEA On S w Y S Trifluoroacetic acid TEA ooo o a S D Y Water ooo o o y awa Y SYS HCI Thionyl Chloride or Di Ethyl Ether compatibilities are not available tt j O gt O S a 3 O D CO lt lt lt ZI lt lt lt z2 z lt lt lt 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
51. igots on top of the pump catch pot seal the connection with a pipe clamp Connect another length of exhaust tubing to the second catch pot spigot seal with a pipe clamp Cut this tube to an appropriate length and connect the CVP Pump vacuum inlet free end to the condenser exhaust inlet Seal the connection with a pipe clamp Note Early build versions of the CVP pump require a different pump control cable which connects to the pump via a plastic Buccaneer connector Do not attempt to exchange a CVP pump for a scroll pump This operation requires a set up in the system software that may only be carried out by Genevac Service personnel or a trained representative of Genevac 04 4541 Issue 3 1 January 2009 Page 9 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Safe Loading of Rotor General Document Genevac are obliged to include the following information in its entirety irrespective of the system type As with all centrifuges Genevac centrifugal evaporators must be loaded correctly to remove the risk of damage Failure to correctly load a system can lead to unrecoverable loss of samples and damage to the system This guide is intended for new users and also as a reminder for more experienced users The principles outlined apply to all Genevac evaporators The following instructions deal with various aspects of loading Use of correct swings and sample holders Observation of weight limits Safe loading of sam
52. ill 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 Sample Guard thermocouple probes control fuses Failure to adhere to the above may result in the costs of repairs being charged Page 56 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Amendment Control Form Issue Reason for Change Date Issued Integration of The Importance of Safe Loading Document Introduction of new Pre Set runs 51 100 within the software 01 March 2004 2 8 Introduction of Scroll Pump 2 9 2 9 Introduction of Warranty Statement 26 April 2004 Change to EU Declaration of Conformity 21 September 2004 Information on the correct use of SampleGuard Probes 28 September 2005 Introduction of Auto Defrost and Drain Option 21 August 2006 Introduction of Annex A Getting the best from Auto Defrost and 1
53. l Evaporating Systems Lyophilising HPLC Fractions The best optimised evaporation method has the following stages 1 2 Follow stage 1 of the Drying HPLC Fractions method to remove the organic solvent Cool the samples concentrating some of the water without any heat input Set the controlled pressure to 8mbar to boil away some of the water without any heat input this cools the holders and helps achieve good freezing in the next stage 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 tem
54. lder option is not available select other and enter the details no more than 31 characters Enter a value for Run Ho Run Data Hext Run Run Hane Sanple Holder Type Sanple Vo lune 91 Last Used Hot yet used Locked Humber CA for none DCH DHF DHI DHSO Ethanol EtOH SanpleGuard Control Temperature C C SanpleGuard Control Channel CoolHeat Enable Pressure mbar Hininum Chamber Temperature C CIJ Rotor Speed Hexane Hex the volume of sample in each individual well tube vial SOLVENT Acetonitrile CACHI Annoniun Hydroxide CHH30H 1 Chloroform CICE Diethyl Ether DEE Ethyl Acetate CEtAc Hethanol MeOH HHP TFA THF Toluene PhHe Hater H20 Other 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 C lear Done GENEVAC LTD HELF TL ENTER to select deselect Done ENTER to accept ESC to cancel Select a solvent from the window that opens mixture of solvents More than one solvent may be selected if using a Selected solvents are highlighted in blue Select Done when the solvent or solvents have been selected Alternatively select Other and enter the solvent name no more than 31 characters a
55. n 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 a a cr ee eae 04 4541 Issue 3 1 January 2009 Page 29 of 56 Genevac HT8 amp HT12 Series Il Evaporating Systems Select one of the following options for End of Run and or Heat Off Elapsed Time Enter independent times for heat off and for end of run The evaporator turns off the IR lamps when the heat off time elapses and allows the system to run without heat input until the end of run time elaspes This feature enables the protection of thermally sensitive samples as they approach dryness while ensuring that all samples are dried completely Heat Flow The system monitors the rate of evaporation by looking at the demand for heat input that is required to maintain the SampleGuard control temperature When sample dryness is detected the system turns off the IR lamps and allows a final drying stage before stopping the run Sample Detection
56. nd Drain 48 When not to use Auto Defrost and Drain 49 Drying HPLC Fractions cccceeseeeeneeeeeees 49 Lyophilising HPLC Fractions 0000008 50 Notes on Lyophilisation cccccceceeeeeeeeees 50 Drying Mixed High and Low Boiling Point Sie f 8 Senne ne eee 51 Programming Guides cccsceseseeeeeeeeees 52 Drying HPLC Fractions cccceeseeeeseeeeeees 52 Fast Lyophilisation of HPLC Fractions 53 Mixtures of High and Low Boiling Point Solvents A EEE AE E E E EA E E T 54 Tecnica Dala uunie a 95 EC Declaration of Conformity 0008 56 Warranty StateMent ccccccecceceeeeeeeeeee ees 56 Amendment Control Form s 0008 57 Useful Information cccccceseeeseeeeeeeeees 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Introduction The Genevac Series Il range of evaporation systems provide very high performance coupled with ease of use The systems are simple to set up easy to operate and very flexible The HT8 SII and HT12 SIl evaporation systems are comprised of an evaporation chamber and rotor with an external cryopump condenser unit Vacuum is provided by a Scroll Pump although other types of vacuum pumps can be used Scroll Pump HT 12 VC3000D Condenser Note Earlier build variants of the HT8 SIl system may have a smaller shorter vacuum chamber The current production versions appear
57. nd draining the condenser depends on the volume and nature of the evaporated solvents The maximum defrost period should be no longer than two hours Defrost and drain the condenser after each run to obtain optimum performance from the condenser Before opening the condenser drain valves ensure that pipes connect the two valves to a suitable waste solvent container Auto Defrost and Drain Ensure that a suitable waste solvent container is connected to the condenser drain pipe at AN all times Draining occurs automatically even after the run has completed Ensure that the end of the drain hose remains above the level of waste solvent in the container Flushing the Condenser Use the condenser flusher if fitted to clean traces of volatile solvent from the condenser before evaporating a less volatile solvents the condenser operates most efficiently when it is drained and clean Always drain the condenser before using the condenser flusher Select FLUSH on the HT12 SII or HT8 SII Menu Bar and press the START key Wait until the system vacuums down to approximately 5mabr Pour approximately 100 ml of acetone into the flushing funnel and open the flushing valve Close the flushing valve after use Stop the system and allow it to vent to atmospheric pressure Drain the flushing solvent from the condenser vacuum pot Repeat the flushing procedure as necessary Never use the flushing valve to vent the system Flushing Valve P
58. nd only connects to the corresponding sockets in the correct orientation To connect the control cable push the connector into the socket and twist the knurled grip clockwise until it clicks into place Connect a mains power cable to the pump mains power connector Connect the second mains power cable to the secondary mains power connector on the side of the evaporator Connect the mains power cables to two separate suitable mains power outlets Note The primary power to the evaporator is delivered via the pump control cable The mains cable to the evaporator supplies power to the infra red lamps and chamber heaters only The system is now ready to switch on Carry out an inspection to ensure all parts are fitted correctly and securely Read the rest of this manual before operating the system Intsallation Variations Lyospeed Systems Connect the single solvent drain pipe to the drain outlet manifold of the LyoSpeed condenser system Ensure the end of the drain pipe cannot be submerged in the waste solvent Installation Variations CVP Vacuum Pump Install the CVP pump in the same way as the scroll CVP Pump exhaust outlet pump the following additional instructions apply Cut a length of exhaust tubing approximately 250mm and connect it to the pump exhaust outlet seal the connection with a pipe clamp Place the pump exhaust catch pot next to the pump adjacent to the Pump Exhaust Outlet Connect the other end of the short tube to a sp
59. nly e The system Pump Warming delay times out HCL systems with a scroll pump only e The condenser temperature cools below 0 C 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Locking and Unlocking the Door Press the Open key on the front panel to unlock the door and open the door manually Hold the door closed and press the Close key to lock the door A beep indicates when the door is closed and the door lock status is shown when the Run Log screen is displayed Note The door can only be unlocked when the rotor is stationary and the system is at atmospheric pressure 04 4541 Issue 3 1 January 2009 Page 17 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Using SampleGuard SampleGuard Transmitter and Probe k L i PAE A i MS PAMAN 44 a Sample holder probe hole Page 18 of 58 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 t
60. o move freely Clean the Quartz Glass using a suitable solvent such as methanol or acetone and a lint free cloth or paper towel Clean the swings and rotor in the same manner Take care to avoid solvent contact with the outside paintwork and accessories of the chamber Scroll Pump Check the pump exhaust catch pot regularly and empty it as necessary No further routine maintenance is required Page 44 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Planned Maintenance and Service Whilst every effort is made to design and manufacture the HT8 and HT12 SIl evaporation systems to the highest build quality and to provide assured reliability there will be some degree of wear and ageing of the seals and bearings of the chamber condenser and pump The extent of wear and ageing depends on the utilisation of the system the severity of temperature cycling and the nature of the solvents used Some solvents may eventually cause pin hole corrosion in the connecting tubes resulting in a decline in performance A gradual decline in system performance may not be noticed if it occurs over a period of time Monitor the system performance by keeping a weekly log of the time taken for the system to reach full vacuum and the full vacuum achieved In order to maintain peak performance and avoid costly and unscheduled down time Genevac strongly recommend implementing a schedule of planned maintenance Changing p
61. oil contamination The pump must have an adequate supply of cooling air and a minimum 300mm of free space adjacent to the heat exhaust Do not place the pump in a space with restricted airflow such as a cupboard 04 4541 Issue 3 1 January 2009 Page 39 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Run Parameters Quick Reference Run Data Locked Set to Yes to protect the run data from inadvertent changing Press the ENTER key to toggle between Yes and No lock the data after completing the run entry Next Run Number Enables the creation of multistage runs by linking runs in any order Enter the number of the run that is required to follow the current run Runs may also be ooped by linking to themselves this makes the run cycle repeatedly until interrupted by a press of the STOP key Run Name Identifies the run profile Sample Holder Type Select the sample holder type from the drop down menu or select OTHER and enter the holder name Sample Volume Enter the volume of the individual samples in mls Solvent Select the solvent from the drop down menu or select OTHER and 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 SampleGuard Control Tempera
62. ontrol 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 GENEYVAC 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 70 350 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 Rotor Speed Elapsed Time eat Off Optio
63. ost in case a small amount of water is frozen in the drain port The system then drains the organic solvent from the condenser allowing high vacuum levels to be achieved later in the run c Consult your local Genevac representative for advice on the evaporation time for this stage However a good rule of thumb is that for 50 50 Acetonitrile water the overall length of this stage should be approximately 1 3 as long as the length of stage 2 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 a2 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 04 4541 Issue 3 1 January 2009 Page 49 of 58 Genevac HT8 amp HT12 Series I
64. perature place probe 2 in a central sample to monitor the process This is essential during method development It indicates when the sample freezes and when the lyophilisation process ends Fill all positions of the sample holders when performing lyophilisation samples in partially filled holders may not freeze Do not use this method to attempt lyophilisation of samples that are grossly insoluble in water These samples crash out once the 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 Page 50 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Drying Mixed High and Low Boiling Point Samples The actual method required depends on the solvents in the mixture A mixture of DMF or DMSO and DCM is outlines in this illustration For other details of mixtures please contact Genevac 1 2 Select Variable Dri Pure to prevent bumping Ramp from 750mbar to 70 mbar in 55 minutes Evaporate the DCM at 65mbar and collect it all in the cold trap Select Auto Defrost and Drain this is a sho
65. ple 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 Tube Holder and Side Bridge Swing Sample holders requiring a separate swing or bucket may also be used Each of these swing types lifts straight out of the rotor The ideal swing type depends on the sample holder required A large range of sample holders is available Load the tubes vials beakers or flasks into the sample holders then place the sample holders in the swings Page 10 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Use of Correct Accessories Genevac supply a wide range of sample holders to cover a variety of plate tube vial or flask formats Where no holder is available custom units can be made To ensure that bespoke holders are suitable and approved for use new sample holders may be designed in collaboration with the Genevac R amp D department Criteria for approval Mass within prescribed maximum limit Matched sample holder mass within a set Correct centre of gravity Good thermal condu
66. r 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 liquid phase Requires both SampleGuard p
67. robes 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 04 4541 Issue 3 1 January 2009 Page 41 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems End of Run Elapsed Time Select the elapsed time after which the run is stopped This can be in the range of 1 minute to 99 hours 59 minutes End of Run Defrost and Drain Select Yes or No Only available on LyoSpeed or automated systems Typically used to remove mixed solvents Pressure Control Regime Select from the following options e Full Vacuum Reduces the chamber pressure to the maximum vacuum capability of the pump e Controlled Pressure Reduces the 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 Variable Dri Pure As Dri Pure b
68. rst and is collected in the condenser To remove the higher boiling point solvents low pressures must be applied later in the process However reducing the pressure causes the previously condensed volatile solvent to re boil in the condenser generating a very large volume of vapour which must exit through the pump Until all this vapour is pumped away which can take several hours the system cannot achieve a lower pressure The volatile solvents 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 Evaporators equipped with the Auto Defrost and Drain facility are identified by a Lyo Speed Enabled label The Auto Defrost and Drain option also appears in the run menu when programming methods Flexibility A Genevac evaporator enhanced with Auto defrost and Drain functionality can be used as part of the LyoSpeed process In addition it can also deliver improved results when working with any mixture of solvents with differing boiling points
69. rt defrost and drain to remove the organic solvent from the condenser allowing high vacuum levels to be achieved later when drying the high boiling point solvent Evaporate the high boiling point solvent Select full vacuum end the method using heat flow Dry any stubborn leftover solvent Select full vacuum and let it run for 1 hour Select Auto Defrost and Drain this is a full defrost and drain See appendix C for programming details Please contact your local Genevac representative for further details on run times alternatively please e mail Applications Genevac com 04 4541 Issue 3 1 January 2009 Page 51 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Programming Guides The programming guides on the following pages show examples of run profiles for some common applications Drying HPLC Fractions ___ving HPLC Fractions Run Data Locked NINN NextRunNumber _ __ _ p B o b Run Name Fractions_ _ Fractions part2 Fractions part3 MeCN or MeOH amp MeCN or MeOH amp MeCN or MeOH amp SampleGuard Control Tempe 40 40 SampleGuard Control Channeli hooo a CoolHeat Enable Pressure 5050 D a a Heat Off Elapsed Time ask fortime 0100 0300 End of Run Option Elapsed Time Elapsed Time End of Run Elapsed Time ask for time 01 00 03 00 Auto Defrost amp Drain Pressure Control E ee o Dri Pure Pressure Vacuum Dri Pure Start Pressure Dri Pure Start Pressure mbar 475
70. s 11 Loading Sample Holders into Swingg 12 Balancing Sample Holders and Swings 13 Good Procedural Practice ccseceeeeneeeees 14 Loading the Rotor cccsccsscssesseeeeeeeeeeees 14 Ste a gE E E E 15 Common Acceptable Solvents 060 15 Genevac and the ATEX Directive 15 Getting Started cccteeeceeeseeeseeeseeeeeeeeees 16 Switching on the PUMD ccccesseeeeeeeeeeees 16 Switching on the Evaporator cccseeeee 16 Locking and Unlocking the Door 04 17 Using SampleGuard 0 eeeeeeeeeeeeeeeees 18 Verifying the Sample Guard Calibration 19 The COndensSe cccccececeeeseeeseeeseneeeeeeenes 20 Manual Defrost and Drain cccceseeeeees 20 Auto Defrost and Drain cccccccseeeeeeeeeees 20 Flushing the Condenser cccceeeeeeeeeeeeees 20 Evaporator Controls ccsecseeeeeeeeeeees 21 Control Screens an Overview 00 22 Select RUN Screen cccccscceseseeesseeeeeeeeees 23 Functions of the Menu Bar c seeceeeeeees 24 Entering Control Data cccccseeeeeeeeeeeeeees 24 Run Data Screen ccccecscsececacsccccececeeeeeecees 25 Run Parameter Details ccccceeeeeeeeeees 25 Run Log SOIC IN aacceescaseccctecesctesicicceciesscice 31 PAVING E E N E E E E EE 31 Shutting DOWN cccccceceseeee
71. ssure T D MeCN 45 for MeOH Notes Remove MeCN Cool the water Freeze the water Lyophilise the water 04 4541 Issue 3 1 January 2009 Page 53 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Mixtures of High and Low Boiling Point Solvents Drying High Low Mixtures Runnumber O n o S e B Run Data Locked 2 2 ff Next Run Number Run Name High Low Mix Solvent DMSO or DMF amp DMSO or DMF amp DMSO or DMF amp DCM DCM DCM SampleGuard Control Temp C40 o Mo Ci o oO SampleGuard Control Channel 40 1 1 CoolHeat Enable Pressure 50 Chamber Temperature control preheat to 15 preheat to 40 preheat to 30 Rotor Speed a Heat Off Elapsed Time laskfortime b 000 End of Run Option Elapsed Time b Elapsed Time End of Run Elapsed Time laskfortme b 0mo a a Auto Defrost amp Drain 40 1 50 Pressure Control Regime Variable Dri Pure Full Vacuum Full Vacuum Dri Pure Start Pressure mbar T 50 Dri Pure End Pressure mbar 70 Dri Pure Ramp Time C S Notes Remove MeCN Dry high BP solvent Final Drying Page 54 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Technical Data Mechanical data HT8 SIil HT12 SIil 1300 Low speed 1300 Low speed 1750 High speed 1750 High speed 300 500G 300 500G Direct Direct 85g 85g 8x1 5kg 500G 4x1 5kg 500G 4 6 Max rotor speed Max force Drive system Operational imbalance Max load IR lamps number
72. the same distance clear of any breakable objects or areas where entrapment could occur If this positioning requirement is impractical the evaporator should be bolted to the bench or trolley by its four mounting feet using M10 high tensile bolts Consult Genevac for advice on any other positioning requirements Pipe Connection Overview CATCH PUMP To Fume Hood or Extraction System Page 6 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Identifying the parts Evaporator Vacuum a Inlet Pump Control Cable Socket and Secondary Mains Power Connector Evaporator Pump Vacuum Inlet Pump Control Box mw lt Catch pot Assembly a F Scroll Pump Pump Control Cable Mains Power Connector Socket Pressure Head Heated Inlet Power Exhaust Inlet Outlet Sockets Condenser Vacuum Heated Inlet Temperature Display Condenser NS Condenser Drain Outlet not shown Condenser Status Indicators 04 4541 Issue 3 1 January 2009 Page 7 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Installing the System The following instructions refer to the installation of an HT8 SII or HT12 SIl evaporator with a scroll pump Details follow showing the differences that may be encountered on earlier build variants Place the Evaporator and Condenser in their intended location The condenser must be placed to the right of the evaporator so th
73. ture Enter the maximum temperature to which the samples holders are heated during evaporation The system s ability to control the sample holders at lower range temperatures is dependant upon the solvent boiling point i e Evaporative cooling and the ambient temperature within the vacuum chamber This can be set within the range 20 to 70 C The default setting is 30 C if no other value is entered Note this is not available for very low rotor speed Sample Guard Control Channel Channel 1 is assigned as the control channel by default channel 1 probe is placed in the sample holder channel 2 probe is optionally placed in the sample Assign control to channel 2 and place the channel 2 probe in the sample holder only if a fault affects channel 1 or its associated probe CoolHeat Enable Pressure Enter the pressure below which the lamps turn on This can be in the range of 5 400 mbar The default setting is 400mbar if no other value is entered Page 40 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems 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 Note do not set the Wait for Chambe
74. ut with additional user settable parameters for the ramp start pressure the ramp end pressure the ramp duration Bumping the violent and uncontrolled boiling of solvents resulting in cross contamination of samples Note The Coolheat function is disabled during the Dri Pure cycle Page 42 of 58 04 4541 Issue 3 1 January 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Problem Prevention Condensation Solvent condensation within the evaporator occurs when the chamber walls are cooler than the solvent vapour This is most likely to occur with high boiling point solvents such as NMP DMI DMSO and possibly DMF Pre heat the evaporator chamber to prevent this happening To do this enter the Run Data screen set the Minimum Chamber Temperature field to 40 C and start the run The chamber takes approximately 20 minutes to reach this temperature Note the CoolHeat lamps do not operate during this pre heating cycle If condensation occurs unexpectedly switch off the lamps by entering O into the Heat off Elapsed Time field on the Run Data screen Do not pre heat the chamber when 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 m
75. xecute 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 om U g D wf I Q Ul D Ow WW O h January 2009 Select Options on the horizontal 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
76. y 2009 Genevac HT8 amp HT12 Series Il Evaporating Systems Run Log Screen The Run Log screen shows information relating to sample drying progress Relevant system status information is shown with key parameter values represented graphically to reveal change trends in real time Numerical values are shown for Channel 1 Temperature SampleGuard channel 1 probe connected to sample holder Channel 2 Temperature SampleGuard channel 2 optional probes Submerged in sample Chamber Temperature Temperature of vacuum chamber wall Condenser Gas Temperature Temperature of 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 If an error is encountered a description of the problem is shown in the ALARMS field Safety critical errors cause the evaporator to stop and report the reason for stoppage non critical errors allow the evaporator to continue with compromised performance and alert the user to the fault Note Rectify the problem and switch the evaporator off to
77. your sales representative for purchase and installation details 04 4541 Issue 3 1 January 2009 Page 5 of 58 Genevac HT8 amp HT12 Series Il Evaporating Systems Delivery and Installation Installation and commissioning by Genevac personnel is an option available with every new Genevac HT system Installation instructions are provided should the commissioning option not be selected Checking the Delivery Check the contents of the delivery against the delivery note as soon as possible Notify Genevac Ltd immediately if any parts are missing or damaged Refer to the back cover for contact details Arranging Commissioning If your system is to be delivered separately Genevac Ltd will contact you prior to delivery to agree a convenient date to commission your system Training Commissioning normally includes training in the basic operation of the system Further in house training is recommended to fully exploit the flexibility of the system The HT8 Sil and HT12 SII evaporation system must not be operated by personnel who AN lack the training or experience to comprehend the hazards that can arise when using the system Personnel without such training require thorough instruction These operating instructions should form the basis of this instruction Positioning the Evaporator The evaporator and condenser must be sited on a level and sturdy work surface Position AN the system least 300mm away from the edge of a bench and

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