Genevac Rocket 4D User manual

Genevac Rocket ™
4D
Evaporation System
User Manual
Original instructions
Part number 04-7848 Issue 2-4 August 2014

Contents
Overview ......................................................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
Basics...........................................................6
Power up.........................................................6
Standby mode ................................................6
Controls ..........................................................7
LCD screen.....................................................8
Opening the lid ...............................................9
Baffles...........................................................10
Getting Started...........................................11
Batch mode ..................................................11
Feed mode ...................................................11
Starting the evaporator.................................12
Stopping........................................................12
Pausing.........................................................12
Evaporation vessel .......................................13
Draining the condenser ................................14
Pouring stand ...............................................14
Menu overview .............................................15
Method guide.............................................16
Factory loaded methods...............................16
Method select ...............................................17
Single solvent feed sequence ......................17
Mixed solvent feed sequence.......................17
Method edit...................................................17
Acceptable solvents......................................18
Advanced Features....................................19
File transfer...................................................19
Log files ........................................................20
System info...................................................20
Options menu...............................................21
View last method graph................................21
About menu ..................................................21
Reduce odour...............................................22
Re-dissolve...................................................22
System Information.......................................22
System Optimisation.................................23
Condenser....................................................23
Delta T..........................................................23
Coolant stabilisation .....................................23
End of stage trigger point .............................24
Final stage....................................................24
Method optimisation .....................................25
Adjustable method parameters ....................25
Special methods...........................................25
Maintenance...............................................26
Recommended practice............................... 26
System test.................................................. 27
Vacuum chamber reservoir water................ 27
Periodic maintenance .................................. 28
Consumable items....................................... 28
Planned maintenance & servicing ............... 28
Outer lid seal................................................ 29
Inner lid seal ................................................ 29
Inner lid feed seal ........................................ 30
Anti-overfill tube........................................... 30
Evaporation vessel spout seal..................... 30
Rotary joint seals ......................................... 31
Feed system ................................................ 32
Hoses........................................................... 32
Feed sensor................................................. 32
Software upgrade ........................................ 32
Re-circulating coolant .................................. 33
Draining the re-circulating coolant............... 33
Unpacking and Setting Up.........................35
Packaging.................................................... 35
Lifting ........................................................... 35
Installation site............................................. 36
Chiller........................................................... 36
Waste solvent .............................................. 36
Hose connections ........................................ 37
Electrical connections.................................. 43
Vacuum chamber water reservoir................ 45
Final checks................................................. 45
Waste solvent full detect.............................. 45
Connecting power........................................ 45
Priming the cooling system.......................... 46
Troubleshooting.........................................47
Opening the lid without power ..................... 47
Error messages ........................................... 47
Error rectification.......................................... 48
Fuses........................................................... 49
Other troubleshooting .................................. 50
Options.......................................................51
Auto feed...................................................... 51
Infinity trolley................................................ 51
Pouring standfor evaporation vessel ........... 51
Technical Data............................................52
Specifications............................................... 52
EC declaration of conformity........................ 53
Warranty statement ..................................... 54
Returning equipment to Genevac................ 54
Chiller warranty and service ........................ 54
Model / serial number .................................. 55
Ordering spares........................................... 55
Patents......................................................... 55
Amendment control...................................... 56
Useful information........................................ 58

Rocket 4D Evaporation System
User Manual
2 04-7848 Issue 2-4 August 2014
Overview
1
4
3
14
11
12
13
10
9
8
5
6
7
2

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04-7848 Issue 2-4 August 20143
Item
Feature
Function
1
Main lid
Automatically unlocks when safe to open. Manually
lift to access the vacuum chamber and inner lid.
2
Lid coupling
Connect the feed line to the evaporation vessel
when the main lid is closed (feed systems only).
3
Inner lid
Turn the thumbscrew and lift the inner lid to open
the evaporation vessel.
4
Rotary joint
Enables gradual feeding of large volumes of
product solution (feed systems only).
5
Evaporation vessel
Product solution capacity up to five litres solution
when used in batch mode.
6
Batch baffles
Fit to the hub of the evaporation vessel to use
batch mode (remove and insert a feed baffle to
use feed mode or to evaporate a very small
volume in batch mode).
7
Lifting points
Insert lifting handles to lift evaporation vessel out of
the evaporator.
8
Waste container vent inlet
Vapour from the waste solvent container is
expelled via the system exhaust.
9
Waste solvent drain outlet
Connect a hose to a waste solvent container for
fully automatic draining.
10
USB port
(Under control panel.) Data log files may be
transferred to, method files may be transferred to or
from, a USB data key
11
Start, stop, pause buttons
Control the evaporation process using the selected
method.
12
LCD screen
Menus allow quick access to everyday functions
and intuitive guidance to advanced features; at-a-
glance system status information is shown during
the evaporation process.
13
Select control
Twist to highlight menu options on the screen,
press to select.
14
Condenser
Waste solvent is recovered by a highly efficient cold
trap which is powered by coolant from a
re-circulating chiller or external chilled water source.
Solvent is drained from the cold trap automatically.

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User Manual
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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
Carry out a risk assessment for each solvent before use. Consider the volumes of solvents
to be used and 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 ventilated space.
Make sure exhaust / ventilation hoses are securely fitted and take solvent vapours
away from the equipment and from the user.
Product solution and rinse solvent is drawn into the vacuum system by atmospheric
pressure, do not pump liquids into the evaporator or pressurise the feed containers.
Do not place objects on top of the evaporator.
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.
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.
It is recommended that physical operations, such as removing the evaporation vessel,
should be practiced with a dry system or with dummy samples before operating with real
samples.
Note: It is the user’s responsibility to ensure that all equipment installed complies with local
regulations for the handling of large solvent volumes.

User Manual
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04-7848 Issue 2-4 August 20145
Combustible solvents
Warning: Risk of vapour ignition. Only operate the system in a ventilated
environment and carry out a risk assessment before 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. For
systems with multiple power leads, each lead requires a separate earth
connection and must be plugged into a separate power socket which is
connected directly into the laboratory electrical supply; do not use extension
leads.
This equipment is an installation class II product and is intended to operate from a normal
single-phase supply.
Emergency shutdown
To shutdown in an emergency, switch off the power socket at the wall and unplug (or
simply unplug if there is no switch). All Genevac evaporators are designed to be safe,
with respect to samples, when switched off in an emergency. The system will
automatically vent and the rotor (evaporation vessel) will spin down slowly when power is
removed. 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 diethyl ether,
pentane or other low auto-ignition solvents.

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Basics
Power up
Before switching on, check that power cables are connected (two to the rocket 4D and one
to the re-circulating chiller) and all other cables and hoses are connected as shown in:
Service connections. Switch on the Rocket4D power switch and switch on the chiller.
After a short boot-up sequence, the Method Select menu appears on the Rocket4D
screen. If Commissioning or Sys use check lists appear, follow the instructions and
press the select control to confirm each check is completed (check lists can be enabled or
disabled in the Options menu).
Note: After switching off, wait at least 10 seconds before powering up again. Repeated
switching off and on should be avoided where possible.
Standby mode
While the Rocket4D is idle, press the stop button to enter
standby mode. The screen brightness reduces (the
Rocket4D logo and software version are shown) and all
other systems are powered down.
To restart, press any button.

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Controls
Menu screens interact with the controls for programming, selecting methods and
operating the evaporator.
1. Screen: Menus allow quick access to everyday functions for method selection and
alteration, and an intuitive guide to advanced features. At-a-glance system status
information is shown during the evaporation process.
2. Start button: Press to start the evaporator using the highlighted method.
3. USB port: (Below the control panel.) Plug in a USB mass storage device (data
key) to copy methods to or from the Rocket or to transfer data log files from the
Rocket. Software updates may also be transferred via data key.
4. Pause button: Press to temporarily interrupt the evaporator, evaporation may be
resumed later.
5. Stop button: Press to stop the evaporator.
6. Select control: Turn to highlight options in menus on the screen, press to select
the highlighted option.
1
2
3
6
4
5

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LCD screen
Graphical and numerical information relating to system status and evaporation progress is
shown during evaporation.
1. Selected method
2. Power save function enabled
3. Sample temperature
4. Inner (rotor) chamber pressure
5. Coolant temperature
6. Delta T (T )*
7. Elapsed time or time remaining
8. USB device connected
9. System status
10. Progression of feeding sequence
11. T trigger point
12. T graph
13. Rotor spinning
14. Current method stage
*For details , see System Optimisation, Delta T.
Single Solvent Feed
d (1/ 2)
rT
+38.8°C
33 mbar
-1.0 °C
+9.15 °C
#00:43.01
Feed Stage 1(Feed 2/3)
0 time 1:00
8
6
4
2
0
5
6
7
8
3
4
1
2
13
12
9
11
14
10

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Opening the lid
Using the handle, manually lift the lid to the
fully open position.
Note: The main lid cannot be opened when
the power is switched off or when the
evaporator is operating.
Lift handle to open lid
Turn the thumb screw counter clockwise and
lift the inner lid away from the evaporation
vessel.
Inner lid thumb screw
A lid stand provides safe storage for the lid
while samples are being loaded or
unloaded.
Lid stand
To refit the inner lid, lower it onto the
evaporation vessel hub, making sure the
feed tube is inserted under the rim of the
evaporation vessel. Tighten down the
thumb-screw until light resistance is felt,
then tighten a further 1½ turns.
Feed delivery tube
Caution: Do not over tighten
the inner lid thumb screw.
Manually close the main lid and press
down firmly to ensure it seals.
Note: Should an error message relating to
vacuum appear (see: Troubleshooting,
Error messages) when the evaporator is
started, check the lid and inner lid are
properly fitted. Push down on the back of
the lid to ensure it is fully seated all the
way round.

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Baffles
For feed enabled Rocket 4D evaporators, two types of baffle are supplied. To ensure even
distribution of liquid around the evaporation vessel, it is important the correct baffle is used.
Batch baffles
Feed baffle
Two batch baffles are supplied for use when
operating the Rocket 4D in batch mode.
These must be fitted to the hub of the
evaporation vessel.
Fit one baffle and make sure it locks into
place before fitting the second baffle. Check
the second baffle also locks into place.
Batch baffles
To remove the batch mode baffles, push
inwards towards the hub and lift away from
the vessel.
For feed enabled systems, a single
feed baffle is supplied for use when
operating the Rocket 4D in feed mode.
The feed baffle is not fitted or secured to
the vessel; it is placed loosely and is
sufficient to ensure even distribution of the
small volumes of product solution in the
vessel during feed mode operation.
The feed mode baffle may also be used for
smaller batch volumes (two litres or less)
and may yield better results when using
re-dissolve.
The batch baffles must be removed from
the vessel before inserting the feed baffle.
Feed baffle
The feed baffle can be removed from the
evaporation vessel using a magnet (not
supplied).
Note: Make sure the correct baffle is fitted
for the method being used, do not operate
the Rocket 4D with batch baffles and a
feed baffle at the same time.

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04-7848 Issue 2-4 August 201411
Getting Started
Batch mode
Feed mode
To start Rocket 4D in batch mode:
1. Check / top-up the chamber water level.
2. Load the evaporation vessel into the
evaporator (do this before adding
product solution).
3. Fit the batch baffles.
4. Pour the product solution into the
evaporation vessel. Take care to avoid
product solution entering the holes in the
hub.
5. Fit the inner lid seal.
6. Fit the inner lid.
7. Close the main lid.
8. Make sure a waste solvent container is
connected and has sufficient capacity.
9. Select the appropriate batch mode
method and press the start button .
Note: For smaller volumes (two litres or less)
the feed baffle may be used instead of the
batch baffles.
To start Rocket 4D in feed mode (feed
enabled systems only):
1. Check / top-up the chamber water level.
2. Load the evaporation vessel into the
evaporator.
3. Place the feed baffle in the evaporation
vessel (batch baffles should not be
fitted).
4. Fit the inner lid seal.
5. Fit the inner lid.
6. Close the main lid.
7. Pour the product solution into the
product solution reservoir.
8. Insert the product solution feed hose
into the product solution reservoir, make
sure the hose weight reaches the
bottom of the reservoir.
9. Pour the rinse solvent into the rinse
solvent reservoir.
10. Insert rinse solvent feed hose into the
rinse solvent reservoir, make sure the
hose weight reaches the bottom of the
reservoir.
11. Check a waste solvent container is
connected and has sufficient capacity.
12. Select the appropriate feed mode
method and press the start button .

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Starting the evaporator
Stopping
When a method is selected and the start
button is pressed, the screen displays the
method settings momentarily whilst the rotor
spins up.
If Pre Run Checks appear on the Screen,
complete the checks as prompted and press
the start button to confirm each check has
been performed.
Note: Pre Run Checks can be enabled or
disabled from the Options menu.
Evaporation methods consist of multiple
stages which follow on automatically. Whilst
evaporation is in progress, the screen shows
the current status; for example:
Stage 1: system safety check
Stage 2: controlled vacuum ramp
Stage 3: evaporation stage
Stage 4: final drying stage.
Method settings may be changed whilst
evaporation is in progress
The evaporator stops automatically when
the evaporation process is complete.
To stop manually, press the stop button.
The evaporator vents to atmospheric
pressure and rotor slows down and stops.
Pausing
Press the pause buttonto stop the
evaporator temporarily. Once the rotor
comes to a stop, samples may be
inspected. The evaporation process may
then be resumed if required.

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Evaporation vessel
Insert a lifting handle into each of the two
lifting points to prepare the evaporation
vessel for lifting out of the Rocket 4D.
Lifting handle release button
Rotate the vessel so the drain spout is at the
back of the evaporation chamber.
Keep fingers and thumbs away from the
lifting handle release buttons and lift the
evaporation vessel clear of the hub, tilt
towards the back of the evaporator and lift
out of the evaporator.
Avoid solvent contact with the inner lid seal
wherever possible. If necessary, remove the
lid seal from the vessel before lifting.
Place the vessel on the bench (or optional
pouring stand) and press the release buttons
to remove the lifting handles.
Tilt the evaporation vessel to elevate the
pouring spout above the liquid level before
removing the stopper from the spout; then
pour the contents from the vessel.
If required, a hose-tail connector may be
fitted to the pouring spout.
Alternatively (with the inner lid seal
removed) pour the contents over the rim of
the evaporation vessel.
Refit the inner lid seal only after the
evaporation vessel has been cleaned.
Dried product may be removed from the
evaporation vessel using a plastic spatula.
Note: The material of the evaporation
vessel is 316 stainless steel. The
compatibility and suitability of samples for
drying in a stainless steel vessel, from the
point of view of corrosion of the vessel and
the potential for metal contamination of the
sample, should be evaluated.
Note: At the end of an evaporation
process, the volume of liquid in the
evaporation vessel should be manageable
and operation of lifting the vessel out of the
evaporator, straight forward. If there is
excess liquid in the vessel, siphon it off or
select a batch mode method and
evaporate the solvent from the vessel. Do
not attempt to lift the vessel with a large
volume of liquid in it.

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Draining the condenser
In normal operation, draining is fully automatic and requires no user intervention. However,
if manual draining is required, go to the Method Select menu, select the Drain Condenser
option then press the start button .
Observe the condenser to make sure all solvent has drained, then press any button to close
the drain valve (after six minutes the condenser drain valve closes automatically).
Make sure the waste solvent container is empty before starting the evaporator. Do not
disconnect the waste solvent container while the evaporator is operating as the drain valve
may open without warning.
Pouring stand
For easy pouring of concentrated product from the evaporation vessel rotor, place on the
pouring stand with the spout positioned as shown. Lift the front of the stand and remove
the stopper from the spout, then lift the back of the stand to pour.
Evaporation vessel (bowl rotor) with pouring stand
Warning: Entrapment hazard, keep hands away from the sides of the pouring
stand when raising or lowering.
Drain Condenser
Drain Will Commence On
Next Key P ress…
Please Ensure Waste Connected
to Start, to Return

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Menu overview
The menus allow quick access to everyday functions and to advanced features. Select
<BACK> or press the stop button to return to a previous menu (some menus revert
automatically after a short period).
If required, alter method
parameters before
starting the Rocket
Press stop button to
enter standby mode, any
button to restart
Use select control to
select required function

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Method guide
The Rocket 4D can store up to ten individual methods which can be accessed from the
Method Select menu. Factory loaded methods are described below (methods on your
Rocket may differ if they have been over-written).
Factory loaded methods
Feed enabled system
Number
Method
Mode
Solvent group
01
Feed Low BP
Feed
Single solvent or
Mixture of solvents with boiling points (within 20°C)
02
Feed Medium BP
Feed
Solvent boiling point > 90°C (including DMF)
03
Feed Aqueous
Feed
Water
04
Feed HPLC
Feed
Mixtures of solvents with dissimilar boiling points (more
than 20°C difference)
05
Batch Low BP
Batch
Single solvent with boiling point below 90°C
Mixed solvents: all boiling points within 20°C and below
90°
06
Batch Medium BP
Batch
Solvent boiling point > 90°C
07
Batch Aqueous
Batch
Water based solutions where freezing at 0°C is
anticipated
08
Batch HPLC
Batch
Mixtures of solvents with dissimilar boiling points (more
than 20°C difference)
09
No Method Loaded
10
No Method Loaded
Non-feed-enabled system
Number
Method
Solvent group
01
Batch Low BP
Single solvent with boiling point below 90°C
Mixed solvents: all boiling points within 20°C and below
90°
02
Batch Medium BP
Solvent boiling point > 90°C
03
Batch Aqueous
Water based solutions where freezing at 0°C is
anticipated
04
Batch HPLC
Mixtures of solvents with dissimilar boiling points (more
than 20°C difference)
05
No Method Loaded
06
No Method Loaded
07
No Method Loaded
08
No Method Loaded
09
No Method Loaded
When custom methods are loaded, unused method slots may be used. Alternatively the
factory pre-loaded methods may be over-written.

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Method select
In the Method Select menu, turn the select
control to highlight the desired method on the
screen. Press the control to select it.
Feed methods consist of a sequence of feed
and evaporation and drain cycles.
Single solvent feed sequence
These methods consist of a single stage with
periodic feed intervals. The number of feeds
is calculated to deliver the maximum volume
of solvent that the condenser can hold. The
condenser is then drained and the process
repeats until the feed reservoir is emptied.
The end of each feed interval is detected
when ∆T drops to the trigger point (refer to:
Condenser Delta T and End of Feed
Interval Detection).
Some method parameters can be adjusted to
optimise the evaporator for specific
applications. For details, refer to: System
Optimisation, Adjustable method
parameters.
Mixed solvent feed sequence
These methods have two stages with a drain
in between. The first stage consists of
several feeds and removes volatile
components from the mixture. The
condenser is drained after the first stage and
(without feed) the second stage removes the
less volatile component(s).
On completion of the second stage the
process repeats from the beginning until the
feed reservoir is emptied.
The second stage only then repeats as
required to evaporate any remaining
solvent from the evaporation vessel.
Method edit
Adjustable method parameters may be
changed at any time (including when the
evaporator is operating) changes are
stored and will apply to future use of the
method.
To edit method settings:
1. Go to the Method Select menu and turn
the select control to highlight the desired
method.
2. Press the select control to enter the
Method Edit menu.
3. Select the parameter to be edited.
4. Use the select control to scroll through
the available setting options and select
the required value.
5. Select <Back> to return to the Method
Select menu.

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Acceptable solvents
The solvents listed in the following table will not damage the evaporator, providing
appropriate methods are used. Contact your local Genevac representative for advice
before using any solvent which is not listed.
Solvent
Recommended method
Acceptable?
Acetic acid
MeCO2H
Aqueous
■
Acetic anhydride
Medium BP
■
Acetonitrile
MeCN, ACN
Low BP
■
Amonium hydroxide
NH3OH
Requires special method
□
1-Butanol
Medium BP
■
2-Butanol
Medium BP
■
Butanone
MEK
Low BP
■
Butyl acetate
Medium BP
■
tert-Butyl alcohol
tert-butanol
Aqueous
■
Chlorobenzene
Medium BP
■
Chloroform
CHCl3
Very Low BP
■
Cyclohexane
Low BP
■
1,2-Dichloroethane
DCE
Low BP
■
Dichloromethane
DCM
Very Low BP
■
Diisopropyl ether
DIPE
Low BP
■
N,N-Dimethyl formamide
DMF
Medium BP
■
1,4-Dioxane
Aqueous
■
Ethanol
EtOH
Low BP
■
Ethyl acetate
EtOAc
Low BP
■
Formic acid
HCO2H
Aqueous
■
Heptane
Low BP
■
Hexane
Low BP
■
Methanol
MeOH
Low BP
■
Methyl teriary butyl ether
MTBE
Low BP
■
1-Pentanol
Medium BP
■
Petroleum ether
pet ether
Low BP
■
1-Propanol
Low BP
■
2-Propanal
IPA, iso-propanol
Low BP
■
Propanone
Acetone
Low BP
■
Pyridine
Medium BP
■
Sodium hydroxide (aqueous)
NaOH
Aqueous
■
Tetrahydrofruoran
THF
Low BP
■
Toluene
Low BP
■
Triethylamine
Et3N
Low BP
■
Water
H2O
Aqueous
■
Water & Acetonitrile
HPLC
■
Water & Methanol
HPLC
■
Water & Ammonia
Requires special method
□
TFA & DCM
Low BP Mix
■
■
Solvent may be evaporated using Rocket
□
Requires special method
Before evaporatingDMF, pre-heat the evaporator by running the Medium BP method
with no solvent for 15 minutes.