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User Manual

Genevac HT-4X Evaporation System

04-7415 Issue 1-16 August

2014

39

Acceptable solvents

Carry out a risk assessment for each solvent or solvent mixture before use. Solvents
included in the following table are not damaging to the evaporator providing appropriate
methods are used. Contact your local Genevac representative for advice before using
solvents which are not.

Solvent

Acceptable?

Solvent

Acceptable?

Acetic acid

MeCO

2

H

■

Hydrobromic acid

HBr

■

Acetic anhydride

■

Methanol

MeOH

■

Acetonitrile

MeCN, ACN

■

Methyl teriary butyl ether

MTBE

■

Amonium hydroxide

NH

3

OH

■

N

-Methly-pyrrolidone

NMP

■

1-Butanol

■

Pentane

p

2-Butanol

■

1-Pentanol

■

Butanone

MEK

■

Petroleum ether

pet ether

■

Butyl acetate

■

1-Propanol

■

tert

-Butyl alcohol

tert

-butanol

■

2-Propanal

IPA,

iso

-propanol

■

Chlorobenzene

■

Propanone

Acetone

■

Chloroform

CHCl

3

■

Pyridine

■

Cyclohexane

■

Sodium hydroxide

(aqeous)

NaOH

■

1,2-Dichloroethane

DCE

■

Tetrahydrofruran

THF

■

Dichloromethane

DCM

■

Thionyl chloride

SOCl

2

□

Diethyl ether

p

Toluene

■

Diisopropyl ether

DIPE

■

Trichloroacetic acid

TCA

■

Dimethyl acetamide

■

Triethylamine

Et

3

N

■

N,N

-Dimethyl formamide

DMF

■

Trifluroacetic acid

TFA

■

Dimethyl sulfoxide

DMSO

■

2,2,2-Trifluoroethanol

TFE

■

1,4-Dioxane

■

Water

H

2

O

■

Ethanol

EtOH

■

Water & Acetonitrile

■

Ethyl acetate

EtOAc

■

Water & Methanol

■

Formic acid

HCO

2

H

■

Water & Ammonia

ammonium hydroxide

■

Heptane

■

Water & HCl

□

Hexane

■

Methanol & HCl

□

TFA & DCM

■

■

Solvent may be evaporated in HT-4X.

□

Only compatible if HT-4X is HCl resistant.

p

Only compatible if HT-4X has an inert gas purge system.

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Содержание HT-4X

Страница 1: ...Genevac HT 4X Evaporation System with XDS5 vacuum pump User Manual Original instructions Part number 04 7415 Issue 1 16 August 2014...

Страница 2: ......

Страница 3: ...ost and drain 30 Manual defrost and drain 31 Waste solvent container 31 Loading Samples 32 Sample holders 32 Use of correct accessories 32 Mass limit 33 Sample holders and swings 33 Loading the rotor...

Страница 4: ...grammable software can store up to 100 methods or runs which can be configured independently or can be linked together to form multi stage programmes for a wide variety of solvent removal applications...

Страница 5: ...ator screen and keypad Evaporation progress is shown by a graphical display with plots for temperature and pressure The evaporator features a built in condenser unit with intelligent feed back to prev...

Страница 6: ...sing the evaporation system Only operate the system in a well ventilated space Make sure exhaust ventilation hoses are securely fitted and take solvent vapours away from the equipment and from the ope...

Страница 7: ...om or from your local Genevac representative Electrical earthing Warning Risk of electric shock This equipment must be earthed The evaporation system is a safety class I product according to IEC class...

Страница 8: ...enevac LyoSpeed fast lyophilisation process Condenser flusher For certain solvent applications periodic flushing of the condenser can help to maintain the performance of the evaporation system All vul...

Страница 9: ...e holders are manufactured in solid aluminium and are anodised to improve heat absorption The contact area is maximised to provide good physical support optimum heat transfer and even heat distributio...

Страница 10: ...nd the power is switched on Switch on the system using the evaporator power switch Note The pump power switch is a resettable circuit breaker it should be switched on and left permanently switched on...

Страница 11: ...denser reaches 0 C if an attempt is made to start the run will commence once operational temperature has been reached Note For HCl systems an additional pump warm up sequence must complete before the...

Страница 12: ...ure Stand by mode To enter stand by mode when the system is idle powered up but not evaporating press the STOP button The LCD screen continues to operate with reduced brightness all other systems powe...

Страница 13: ...a graph of the last completed run use the cursor direction keys to show different segments in time 4 SETTINGS Press to display the Run Data screen for the selected run 5 Keypad Enter data for setting...

Страница 14: ...N Currently selected method number 2 Status shows current evaporator status 3 Graphical data Shows progression of evaporation run with data for Channel 1 temperature Channel 2 temperature Pressure and...

Страница 15: ...t on samples therefore these runs require the channel 2 temperature probe to be used For runs that use Heat flow or timed auto shut down the use of SampleGuard channel 2 is optional SampleGuard probes...

Страница 16: ...n heat transfer across the plate For details of the range of heat transfer plates that are available contact your local Genevac representative to request a Genevac Accessories Brochure or visit the Ge...

Страница 17: ...When the traces begin to converge this indicates the sample is approaching dryness Run parameters can be changed whilst the evaporator is operating refer to Advanced Operation Setting up a run Stoppi...

Страница 18: ...eys indicated Skip The evaporator returns to the Run Select screen Drain The system opens the drain valve and pumps any waste solvent into the waste solvent container Defrost Enter the defrost menu Se...

Страница 19: ...up a method The following section describes how to set up a new method the process is similar for overwriting an existing method Begin by selecting an empty slot from the SELECT RUN screen or select...

Страница 20: ...changes Next Run Number Runs can be linked together enter the number of the run that requires to be linked and it will commence when the current run finishes Any number of runs can be linked together...

Страница 21: ...xture Once selected solvents are highlighted in blue Select Done when the solvent or solvents have been selected For solvents that are not listed select Other and enter the solvent name manually no mo...

Страница 22: ...amme the remaining run parameters Auto programmed run parameters are shown in blue but can be manually overwritten in which case they revert to being shown in white Alternatively select N No to contin...

Страница 23: ...emperature SampleGuard Control Channel Channel 1 is the default setting The option to change to channel 2 is provided only to allow continued operation should a fault arise with channel 1 or its assoc...

Страница 24: ...for the vacuum chamber to cool before evaporating volatile solvents or mixtures that may be prone to bumping this is unnecessary for most applications function Automatic Control To optimise the cryo...

Страница 25: ...automatically if Dri Pure is selected see Pressure Control Regime Low Samples are subject to lower centrifugal force approximately 350 G This should be used for applications that do not require high r...

Страница 26: ...in the sample holders at control temperature When sample dryness is detected the system automatically turns off the IR lamps and performs a final drying stage before stopping the run Sample Detection...

Страница 27: ...Pure ramp Select this setting if bumping is anticipated Variable Dri Pure As Dri Pure but with added flexibility as settings for Dri Pure Start Pressure Dri Pure End Pressure Dri Pure Ramp Time and Fi...

Страница 28: ...1 probe Channel 2 Temperature SampleGuard channel 2 probe Chamber Temperature temperature of vacuum chamber wall Condenser Gas Temperature temperature of the condenser coolant gas Pressure vacuum cham...

Страница 29: ...End of Run Beeps On Off turns off repeating end of run alarm Options enable Auto Shutdown and Pre Run Checklist Maintenance for engineer use only Status displays information for fault diagnostics Fil...

Страница 30: ...ing any of the other menu options START starts the highlighted run EDIT alternative route to the Run Data screen GRAPH shows the graph of the last completed run CLEAR clears the highlighted run profil...

Страница 31: ...created on the data key before copying files to it To transfer data go to the OPTIONS menu and select FILE TRANSFER then select one of the following options COPY ALL METHODS FROM DATAKEY All methods...

Страница 32: ...MSO are almost impossible to evaporate in one operation but using automatic defrost and drain methods can be set up to perform multiple operations without the need for manual intervention between stag...

Страница 33: ...T and press the START button The defrost cycle will continue until the system senses that all solvent in the condenser pot is liquid or can be stopped manually by pressing the STOP button To drain liq...

Страница 34: ...dance at all times Only use swings and sample holders that are approved for the system it is particularly important to check this if more than one Genevac system is in use Only use the tubes or vials...

Страница 35: ...tions Do not exceed the mass limit under any circumstances In most cases with normal solvent volumes loaded Genevac sample holders will fall within this limit If in any doubt load up a swing and weigh...

Страница 36: ...sample holder wells If using separate swings make sure the sample holders are located correctly in the swings If partially loading the rotor make sure sample holders swings are placed in a balanced co...

Страница 37: ...st to redistribute the samples into four holders to help distribute the heat flow evenly between samples and to reduce mechanical stress on the rotor Alternatively two empty swings can be placed on th...

Страница 38: ...SELECT RUN screen Runs 61 through to 98 are associated each run having a venting procedure linked to the end of the evaporation process which helps to remove residual vapours from the chamber Note Ru...

Страница 39: ...te for fast lyophilisation methods it will also indicate when the monitored sample has frozen and when the lyophilisation process ends Use the data to optimise the method for example if it can be prov...

Страница 40: ...ser to enter control parameters for pressure reduction cycles Select Crystallise and enter values for Pressure reduction mbar Pressure reduction time MM Atmosphere Vent Time MM The software feature is...

Страница 41: ...one MEK Petroleum ether pet ether Butyl acetate 1 Propanol tert Butyl alcohol tert butanol 2 Propanal IPA iso propanol Chlorobenzene Propanone Acetone Chloroform CHCl3 Pyridine Cyclohexane Sodium hydr...

Страница 42: ...sed to evaporate a mixture of DMSO and DCM Specific method settings would depend on variables such as volume mixture ratio and the type sample holder used 1 Select Variable Dri Pure and set a ramp fro...

Страница 43: ...olume ml Your Volume Your Volume Your Volume Solvent MeOH H20 MeOH H20 MeOH H20 SampleGuard Control Temp C 40 40 40 SampleGuard Control Channel 1 1 1 CoolHeat Enable Pressure mbar 50 50 50 Chamber Tem...

Страница 44: ...eOH H20 SampleGuard Control Temp C 40 0 0 40 SampleGuard Control Channel 1 1 1 1 CoolHeat Enable Pressure mbar 50 50 50 50 Chamber Temperature control c preheat to 25 preheat to 0 preheat to 0 preheat...

Страница 45: ...Volume Your Volume Your Volume Solvent DMSO or DMF DCM DMSO or DMF DCM DMSO or DMF DCM SampleGuard Control Temp C 40 40 40 SampleGuard Control Channel 1 1 1 CoolHeat Enable Pressure mbar 50 50 50 Cha...

Страница 46: ...ain cycle manually Periodic maintenance Check the condition of the exhaust hose and waste solvent drain tubes Make sure the exhaust hose takes solvent vapours away from the system safely Avoid forming...

Страница 47: ...e sample holder wells Spilled solvent can cause debris to stick to the sample holders causing high points that stress the glassware Clean off any adhered dirt or debris by washing the sample holders i...

Страница 48: ...pressure of 16 mbar using a sample control temperature of 40 C Caution Purging with acetone is not recommended as vacuum seals within the evaporation chamber will be exposed Whilst every effort is mad...

Страница 49: ...and a safe distance from any breakable objects or areas where entrapment could occur If required the evaporator can be bolted to the bench or trolley by its five mounting feet using M10 high tensile...

Страница 50: ...hat an error occurs that that could affect the physical condition of the evaporator or its ability to safeguard the integrity of the samples a critical error the system will stop automatically A descr...

Страница 51: ...cetonitrile or methanol Check the sample swings are able to move freely Clean the quartz glass using a suitable solvent such as methanol or acetone and a lint free cloth or paper towel Clean the swing...

Страница 52: ...amples by reducing the pressure in the vacuum chamber by gradual increments Evaporation begins progressively and samples are contained due to the higher centrifugal force In the event of power failure...

Страница 53: ...replaced by suitably trained personnel If a fuse blows repeatedly contact Genevac service for assistance Evaporator The evaporator fuse is located on the lower right hand side of the evaporator back p...

Страница 54: ...opposing holders are balanced with 10 g IR lamp blown or cooling fan failed Contact Genevac Service No SampleGuard temperature display No SampleGuard signal Wait until rotor reaches full speed Note S...

Страница 55: ...condensing Altitude Sea level to 1600 m Ventilation air gap 50 mm Ingress protection rating IP30 The evaporator is designed for use in a pollution degree 2 environment normally only no conductive poll...

Страница 56: ...wing standards BS EN 61010 1 2010 Safety requirements for electrical equipment for measurement control and laboratory use General requirements BS EN 60204 1 2006 A1 2009 Safety of machinery Electrical...

Страница 57: ...out as detailed in the Maintenance section of this User manual Power leads supplies with the system are for use with that system only If items are replaced by the owner only Genevac approved parts may...

Страница 58: ...Aug 13 1 7 Display button description correction Connection diagram correction Sample holder image update Data transfer changed to Copying methods data 12 Nov 13 1 8 HCl option required for thionyl ch...

Страница 59: ......

Страница 60: ...ng to press and may be subject to change without notice Some of the features and software functions described within this user manual may not apply to equipment manufactured before this manual s publi...

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