Genevac HT-4X User manual

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

Contents
Introduction..................................................2
Safety............................................................4
Warnings and cautions...................................4
Risk assessment ............................................4
Precautions.....................................................4
Combustible solvents .....................................5
Electrical earthing...........................................5
Emergency shutdown..................................5
Strong acids....................................................5
Low auto ignition point solvents .....................5
Options.........................................................6
Standard equipment .......................................6
HCl resistance ................................................6
Auto defrost and drain....................................6
Condenser flusher ..........................................6
Inert gas purge ...............................................6
High power lamps...........................................6
Remote door open..........................................6
Infinity trolley...................................................7
Sample holders...............................................7
eXalt crystallisation package..........................7
Basic Operation...........................................8
Power up / down.............................................8
Opening / closing the lid...............................10
Stand-by mode .............................................10
Controls ........................................................11
LCD screen...................................................12
SampleGuard™ ............................................13
Selecting a run..............................................14
Starting a run................................................14
Run in progress ............................................15
Stopping a run ..............................................15
End of run.....................................................16
Advanced Operation..................................17
Setting-up a method.....................................17
Run parameters............................................18
Run log .........................................................26
Options menu...............................................27
Controls menu ..............................................27
Menu bar.......................................................28
Data transfer.................................................29
Condenser..................................................30
Automatic defrost 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.......................................... 34
Balancing the rotor....................................... 35
Method guide..............................................36
Pre-programmed runs.................................. 36
Creating new methods................................. 37
Method optimisation..................................... 37
Lyophilisation............................................... 37
Crystallisation .............................................. 38
Acceptable solvents..................................... 39
Solvent mixtures .......................................... 40
Method examples ........................................ 41
Maintenance...............................................44
Recommended practice............................... 44
General cleaning.......................................... 45
Sample holders............................................ 45
IR lamp lens................................................. 46
Planned maintenance and servicing............ 46
Condenser flushing...................................... 46
Delivery and Installation............................47
Installation site............................................. 47
User training................................................. 47
Troubleshooting.........................................48
Audible alerts............................................... 48
Visual alerts ................................................. 48
Faults and errors.......................................... 48
Clearing Errors............................................. 48
Condensation............................................... 49
TFA creep.................................................... 49
Bumping....................................................... 50
Opening the lid without power ..................... 50
Circuit breakers / fuses................................ 51
Other troubleshooting .................................. 52
Technical Data............................................53
Specifications............................................... 53
EC declaration of conformity........................ 54
Warranty statement ..................................... 55
Patents......................................................... 55
Amendment control...................................... 56
Useful Information........................................ 58

Genevac HT-4X Evaporation System
User Manual
204-7415 Issue 1-16 August 2014
Introduction
Genevac HT evaporation systems are designed to provide very high performance coupled
with ease of use. They are simple to set up, easy to operate and very flexible. HT-4X
comprises a built-in cryopump-condenser and a separate vacuum pump.
Programmable 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.
A selection of methods is pre-loaded to allow new systems to be set up quickly; alternatively
methods can be wholly created by the user or can be built up using settings suggested by
the auto-programming software. Once created, methods can be improved or optimised to
provide the best possible performance for specific applications.

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Automatic end of run detection software can be utilised to complete evaporation runs in the
shortest possible time, opening the possibility for two or more runs to be completed in a day
where previously overnight running may have been required.
User interaction is via an easy-to-clean touch-sensitive keypad and data is displayed on a
bright and clear LCD screen. Once set-up, operation is straight forward simply load
samples, select the appropriate run and press start.
Evaporator 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 prevent
initialisation of an evaporation process until the condenser is ready. Waste solvent defrost
and drain can be set up to occur automatically at the end of evaporation or at key points
during the evaporation process. Alternatively, the condenser can be defrosted or drained
manually via the evaporator Select Run screen.
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.

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Safety
Warnings and cautions
This symbol is used within this manual to highlight warnings and cautions.
Warning: highlights a risk of personal injury or material damage.
Caution: highlights a risk of material damage.
Risk assessment
Caution: Carry out a risk assessment for each solvent before use. Consider the
possible consequences of applying vacuum to solvent mixtures, especially
organic solvents. For example, H2O2 gives off O2 under vacuum, creating an
oxygen rich atmosphere.
Precautions
Observe the following safety precautions when using 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 operator
Only use sample holders and / or swings that are approved for use by Genevac
Do not leave the system unevenly loaded, someone may start it
Do not start or restart a system without checking it is evenly loaded
Do not place objects on top of the system
Check the condenser has been drained before starting the system
Refer to the Genevac published list of acceptable solvents for solvent compatibility
information
Clean up any solvent spillage immediately
Dispose of waste solvents in accordance with local environmental regulations.
Caution: Incorrect loading may result in damage to samples and to the system.

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Only allow users who are familiar with all the issues outlined in this User Manual to operate
the equipment. If personnel lack the training or experience to comprehend the hazards that
can arise when operating the system, do not allow them to use it; personnel without such
training require thorough instruction. The information contained within this User Manual may
form the basis of such training.
Any maintenance or repair of this product, other that that which is detailed in this user
manual, must be carried out by Genevac personnel (or approved representatives of
Genevac) using only Genevac approved spare parts.
Combustible solvents
Warning: Risk of vapour ignition. Only operate the system in a well ventilated
environment and consider safety when evaporating any combustible solvents.
Genevac's position regarding the evaporation of such solvents, particularly with
respect to the European ATEX directive, is available on our website, at
www.genevac.com, 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 classification. It
must never be used with any interruption to the safety earth conductor. It is an
installation class II product and is intended to operate from a normal single-phase
supply.
Emergency shutdown
All Genevac evaporators are designed to be safe with respect to samples when they are
switched off in an emergency. The system will automatically vent and the rotor will spin
down slowly when power is removed. To shutdown in an emergency, switch off the power
socket at the wall and unplug (or simply unplug if there is no switch). Users should
familiarise themselves with the location of the connection to the mains supply and make sure
the power socket and plug is always accessible.
Strong acids
Caution: Do not attempt to evaporate, HCl, thionyl chloride, or other acid
chlorides, in non-HCl compatible evaporators.
Low auto ignition point solvents
Warning: Risk of vapour ignition. Do not attempt to evaporate di-ethyl ether,
pentane or other low auto-ignition solvents unless the evaporator is fitted with an
inert gas purge system.

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Options
Standard equipment
HCl resistance
Genevac HT-4X evaporators feature the
following equipment as standard:
Dri-Pure®(including Variable Dri-Pure)
which eliminates sample bumping and
prevents associated problems of sample
loss and cross contamination.
SampleGuard™ for accurate sample
holder temperature control.
Onboard data logging –files can be
transferred via a USB data key (not
included).
In addition, the following optional
specifications can be added at the time of
ordering. Consult your Genevac
representative for advice on any other
requirements.
Auto defrost and drain
AD&D enables the uninterrupted
evaporation of mixtures of solvents with
dissimilar boiling points, including HPLC
fractions. The system facilitates the use of
the Genevac 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 vulnerable parts of the evaporator are
manufactured from inert material. A special
software feature conditions the vacuum
pump by pre-warming before use and
purging harmful vapours after use.
Inert gas purge
Air within the vacuum system is displaced
with inert gas prior to starting the
evaporation run, the system also vents with
inert gas at the end of evaporation. Oxygen
levels within the evaporator are maintained
safely below the minimum concentration
limit for the combustion of solvents.
High power lamps
High power Coolheat IR lamps can
significantly reduce evaporation times when
evaporating solvents with high latent heat of
evaporation (such as water, methanol or
ethanol).
Remote door open
For systems installed in fume cupboards,
the evaporator door can be opened to clear
fumes before opening the fume cupboard.

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Infinity trolley
Infinity Trolley is a modular trolley system.
The lower shelf can be pulled out to provide
access to for maintenance and any number
of units can be bolted together, side by side.
Sample holders
A wide range of swings and sample holders
is available to cover plate, tube, vial and
flask formats, as well as the revolutionary
Genevac SampleGenie™ system. The
illustration shows just a few of the sample
holders available.
Sample 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 distribution for
drying loads.
For further details of sample holders,
contact your local Genevac representative
to request a Genevac Accessories
Brochure or visit the Genevac web site at
www.genevac.com.
eXalt crystallisation package
The package consists of additional software
features plus a tool kit that provides an array
of baffles.
When fitted to vials, the baffles control the
evaporation rate for each individual vial,
allowing a wide range of solvents to be dried
simultaneously at the at the same slow
evaporation rate.

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Basic Operation
Power up / down
Before switching on, make sure the pump control cable is connected as shown, the power
cable is connected to a mains power outlet and 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. Power distribution to the pump is controlled by the evaporator
power switch.
The system powers up in stand-by mode, the LCD screen on the evaporator shows the
evaporator software version.
Pump power switch
Evaporator power switch
Power lead

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To start the system, press the green START
button on the evaporator keypad.
The vacuum pump starts and the
SELECT RUN menu appears on the
evaporator LCD screen.
The condenser also powers up and begins to cool down to its operating temperature. The
system will not allow an evaporation run to commence until the condenser 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
system will allow an evaporation run to commence (this prevents the possibility of solvent
condensation inside the pump). The warm-up time remaining is shown on the screen.
To power down, enter the Select Run screen and press the STOP key. Press Y on the
evaporator keypad when prompted:
Note: If a pump purge sequence begins, allow this to finish before switching off the
evaporator power switch.

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Opening / closing the lid
To open and close the lid, press the button on the front panel.
Note: The lid cannot be opened while the rotor is turning or the
evaporation chamber is below atmospheric pressure.
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 power down.
To restart the system, press the START button.
Note: The system may continue to purge the vacuum pump for a preset time after entering
stand-by mode. The Purge Time remaining is indicated on the screen; do not power the
system down until the pump purge cycle has completed.

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Controls
Frequently used function keys are positioned on the left hand side of the keyboard. The right
side illuminates to accept input for programming via the Run data screen when required.
1. LCD screen: Shows graphical and numerical data.
2. MENU: Press to display the User Menu screen, only operates when the system is idle.
3. DISPLAY: Press to show 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 up or editing runs.
6. USB port: Transfer data (methods or log files) via USB data key.
7. Cursor direction keys:Scroll up and down, move around menu options on the
display.
8. START: Press once to start the selected run or to execute the highlighted option.
9. STOP: When evaporator is operating, press once to stop; when evaporator is idle,
press once to enter standby mode.
10. CLOSE / OPEN: Press to open / close the lid.
1
3
4
5
7
9
6
8
10
2

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LCD screen
The illustration shows the LCD screen as it appears during an evaporation run, the graphical
and numerical information shown relates to evaporation progress.
Other menu screens appear during different operations and are discussed later in this User
Manual.
Run log screen shortly after evaporation has started
1. RUN: 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 Spin Rate.
4. Messages and instructions: Provided instructions if user intervention is required, or
shows summary of current evaporator status.
5. Numerical data: Shows temperatures of evaporation chamber, sample holder, sample,
and condenser; also shows pressure, rotor speed and time elapsed or remaining.
6. ALARMS: Information or warnings regarding errors that occur during operation are
shown here.
2
3
4
6
1
5

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SampleGuard™
The SampleGuard transmitter has two input connectors for SampleGuard probes, these
must be connected for the SampleGurard system to function correctly. The numbers
1 and 2,embossed on the side of the SampleGuard transmitter, correspond to the
SampleGuard channels shown on the LCD screen. The third connector is for a stuffer plug
which should not be removed (this is for use by service engineers only).
The channel 1 temperature probe must always be used, it controls the temperature of the
sample holder.
The channel 2 temperature probe monitors the temperature of a sample. Runs that use
Sample Detection for the automated heat-off or end-of-run options, depend on monitoring
the evaporative cooling effect 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 are available in lengths to suit different types of sample holder.
Caution: Risk to sample integrity; make sure the probes are long enough to allow
the sample holder to swing
channel 1: insert the probe into the small hole (which is provided for this purpose) in
the sample holder.
channel 2: insert the probe into one the central sample tubes (or wells) making sure the
probe rests against the bottom of the tube. During evaporation, the probe is held firmly in
place by centrifugal force.
Channel 1 probe
inserted in hole in
sample holder
SampleGuard
transmitter
Channel 2 probe
in central well of
sample holder
Caution: Risk to sample integrity; the programmed SampleGuard Control
Temperature can only be maintained correctly if the channel 1 SampleGuard
probe is placed in the holder block as shown.

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Note: Significant solvent cooling occurs during evaporation so samples in the central wells
can experience a thermal drain effect due to the greater number of surrounding samples.
For this reason it is advisable to position the channel 2 sample probe near the centre of the
holder as these samples can take longest to dry.
The thermal drain 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 reduces the effect by providing an even
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 Genevac website at www.genevac.com.
Selecting a run
From the SELECT RUN screen, use the cursor direction keys to move the white band up
or down the screen.
Cursor direction keys
The screen displays ten runs at a time and the next ten runs appear when the white band
scrolls off the top or bottom of the screen. Up to 100 runs can be stored in total.
Move the white band until it required run is highlighted.
Starting a run
With the required run highlighted on the SELECT RUN screen, press the START button to
start an evaporation using the selected run.
Note: If the system is not ready, a message appears near the bottom of the screen, the run
will start once the system becomes ready.

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Run in progress
The Run Log screen provides data relating to evaporation progress, information is
presented in numerical and graphical form.
During evaporation, the effect of evaporative cooling (on the sample being monitored) can be
seen in the divergence of the SampleGuard channel 1 and channel 2 traces. 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.
Stopping a run
To manually stop an evaporation run, press the STOP button. The evaporator vents to
atmospheric pressure, once a safe pressure is reached the rotor begins to slow down. The
door cannot be opened until the rotor is stationary and the system is at atmospheric
pressure.
When the rotor comes to a stop, a short sequence of beeps sounds to inform the user (this
repeats periodically).

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End of run
This screen appears after the run finishes.
Select Skip, Drain or Defrost using the numeric keys indicated.
Skip: The evaporator returns to the Run Select screen.
Drain: The system opens the drain valve and pumps any waste solvent into the waste
solvent container.
Defrost: Enter the defrost menu. Select START to begin the defrost cycle.
The evaporator defrosts the condenser until solvent defrost is automatically detected.
Alternatively, press the STOP key to end the defrost cycle.

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Advanced Operation
The evaporator holds a library of up to 100 individual methods (or runs) which can be
accessed using the SELECT RUN screen. Runs 50 to 99 are pre-set at the factory and are
generic; they are designed to get the system up and running quickly. To optimise the system
for specific applications, new methods can be created. For development purposes, existing
runs can be copied to a new location where they can be edited.
Setting-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 an existing method to be overwritten) then press the Settings key to enter
the Run Data screen.
A default set of parameters is shown (or existing parameters if overwriting an existing run).
Press the cursor direction keys to move between the displayed run parameters, then press
the return key to open a field for editing.
Enter a new value for the parameter, then press the return key to save and close the field.
Note: The HELP field, at the bottom of the screen, provides instructions whenever user
intervention is required.

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Run parameters
The following pages describe the function of each run parameter in turn and show the range
of setting options available. Instructions for setting the parameter are also given.
Run Data Protection
The run profile can be protected against accidental alteration. Set the Run Data Protection
field to No before attempting to edit an existing run profile or set to Yes to prevent accidental
changes being made to the run profile. For additional security, a password may also be set
to protect against unauthorised 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 in this
way.
If no link is required, enter 0 (default setting) and the system will stop when the current run
ends.
Note: A never-ending chain will be created if the last run of a chain in linked back to the
first, or if a run is linked to itself. If such a chain is created the only way to stop the
evaporator is to change the setting or to manually press the STOP button.
Run Name
Enter a name (up to 20 characters) which the user can recognise to identify the run profile.
Text entered on the keyboard appears in the lower section of the screen. Press the return
key to enter the text into the Run Name field.