LaboGene CoolSafe Basic 55-4 User manual

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INSTRUCTION MANUAL
CoolSafe Basic & Pro
Size 4-9-15 –Temperature -55-95-100-110

Instruction manual for CoolSafe
06012017QA01
Item No. 700749
CopyRight © 2017
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Symbols used in this manual

Note
Used to direct attention to a special item.
Warning
Used in case of danger of a serious accident or lethal injury.
Caution
Used in case of danger of medium or minor injuries or physical damage.
This document is the original instruction manual in accordance with the current Machinery Directive.
This document is the reference for any translation of this instruction manual. In case of doubts or
uncertainties the text in the original instruction manual is the valid.

Instruction manual for CoolSafe
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Table of contents
1Introduction..........................................................................................4
2Safety precautions ...............................................................................4
2.1 General information................................................................................4
2.2 Safety.....................................................................................................4
3Installation............................................................................................5
3.1 Installation of CoolSafe...........................................................................5
3.2 Installation of vacuum pump...................................................................5
3.3 Installation of accessories.......................................................................6
4Functional description.........................................................................6
4.1 Control panel..........................................................................................6
4.2 Valves and connections..........................................................................7
4.2.1 Power supply and ON/OFF switch..........................................................7
4.2.2 Vacuum pump connection......................................................................7
4.2.3 Electrical vacuum valve ..........................................................................8
4.2.4 Drain valve.............................................................................................8
5Operation..............................................................................................8
5.1 User interface.........................................................................................9
5.2 Error situations, status and error codes...................................................9
5.2.1 Status codes ..........................................................................................9
5.2.2 Error codes ............................................................................................9
5.3 Preparations.........................................................................................10
5.4 Freeze-drying....................................Fejl! Bogmærke er ikke defineret.
5.5 Freeze drying using manifolds..............................................................10
5.6 Freeze drying using chambers..............................................................11
5.7 Stopping the vacuum pump..................................................................12
5.8 Hints, tips and reminders......................................................................12
6Maintenance .......................................................................................13
6.1 CoolSafe freeze dryer...........................................................................13
6.2 Vacuum pump......................................................................................13
6.3 Cleaning...............................................................................................13
6.4 Checking for leaks on the CoolSafe freezer dryer..................................13
7The Freeze-drying process................................................................15
8Technical Specifications....................................................................16
8.1CoolSafe -55 °C ...................................................................................16
8.2 CoolSafe -95 °C and -100 °C................................................................17
8.3 CoolSafe -110 °C .................................................................................18
9Accessories........................................................................................18
10 Declaration of conformity ..................................................................19
11 Annex - Pressure of Aqueous Vapor.................................................20

Instruction manual for CoolSafe
06012017QA01
Item No. 700749
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1 Introduction
This manual covers the CoolSafe models Basic and Pro. The models are:
CoolSafe Basic: 55-4, 55-9 and 110-4
CoolSafe Pro: 55-4, 55-9, 55-15, 95-15, 100-9 and 110-4.
CoolSafe 4-15 l is an outstanding and versatile range of advanced bench-top freeze dryers. They
are the product of more than 40 years’ experience and expertise, and are the ideal choice for
research, process development and small-scale production.
All sizes come with a choice of condenser temperatures and a wide range of high-quality chambers
and accessories. All models offer both simplicity of operation and the highest performance
characteristics to meet the demands of today’s research and development laboratories.
Lowest condenser temperatures of -55°C, -95°C, -100°C or -110°C.
Seamless stainless steel condenser with external cooling coils, heavily insulated to
conserve energy and increase performance Easy removal of water via drain valve.
Easy draining with built-in valve, allowing removal of water after a completed freeze-drying
session.
Very simple to operate.
Widechoice of manifolds, chambers and accessories to suit your sample requirements.
Available with 4-litre condenser capacity and temperature options of -55°C or -110°C and
condenser ice capacity of 2.5 kg/24 hours - max. 3 kg in total.
Available with 9-litre condenser capacity and temperature options of -55°C or -100°C and
condenser ice capacity of 4 kg/24 hours - max. 7 kg in total.
Available with 15-litre condenser capacity and temperature options of -55°C or -95°C and
condenser ice capacity of 6 kg/24 hours - max. 10 kg in total.
If you are not familiar with the freeze-drying process, please read the section “The freeze-drying
process”, which outlines the freeze-drying process.
2 Safety precautions
2.1 General information
Please read this entire manual to fully understand the safe and effective use of this product. Should
you have any comments about this manual we will be pleased to receive them.

Note
If this equipment is used in amanner not specified by the manufacturer, the
protection provided by the equipment may be impaired.
2.2 Safety
All CoolSafe models are electrically protected with an over current circuit breaker.

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All CoolSafe models utilize low temperature refrigeration to -55°C, -95°C, -100°C or -110 °C and
under no circumstances should the cold surfaces of the condenser be touched whilst switched on,
in operation or in the de-icing process.
Do not handle, move or service the vacuum pump whilst in operation or if it is switched off, until it
has cooled down to ambient temperature. (See paragraph regarding maintenance & changing of oil
in the vacuum pump).
It is advisable that safety glasses and personal protective garments are worn by all users of the
equipment.
CoolSafe Basic or Pro models 95-15 and 100-9 are fitted with castors, the front pair being lockable.
Once located in the position conducive to both the safety of the laboratory environment and
personnel, it is advised that the castors be in the locked position.
The safety system is designed according to safety requirements for electric equipment, control and
laboratory use (EN 61010-1), which assumes that two separate faults do not occur simultaneously.
3 Installation
3.1 Installation of CoolSafe
Make sure that themains supply is according to the specifications on the type label placed
on the rear panel.
It is important that free air circulation is available at the air inlet and outlet grills. If the
CoolSafe is positioned against a wall, there must be at least 100 mm free space at the rear
of the unit.
The CoolSafe Basic or Pro 95/55-15 and the CoolSafe Basic or Pro 100-9 are both floor
standing units fitted with castors, the front pair being lockable. Before operating the system
insure that the castors are in the locked position.
3.2 Installation of vacuum pump
A two-stage vacuum pump (with 2-5 m3/h capacity or greater) must be connected to the CoolSafe
Basic or Pro via the connection on the rear of the CoolSafe Basic or Pro cabinet in order to allow
cryo pumping.
On the floor-standing models, the vacuum pump can be installed on the rear of the CoolSafe on a
shelf support delivered with the equipment. On table models the vacuum pump must be placed near
to the freeze dryer.
LaboGene recommends the VacuuBrand RZ2.5 rotary vane pump for which a variety of protection
accessories, against aggressive materials are available. The vacuum pump outlet/exhaust is fitted
with an oil mist filter as standard.

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Check that the mains supply for the pump is according to the specifications on the type
label.
Connect the vacuum hose to the suction side of the pump.
Connect the pump to the vacuum connection pipe on the rear panel of the CoolSafe.
Check the oil level on the pump and fill it if necessary. The oil level sight glass should be
1/2 - 3/4 full.
LaboGene recommends that when the pump is running the gas ballast valve is in the open position.
3.3 Installation of accessories
The CoolSafe Basic or Pro is a basic unit and must be equipped with the necessary accessories to
run a specific freeze-drying process. Select from the wide range of accessories listed in the
accessories section.
Make sure to mount the correct manifold, chamber and shelf arrangements and always check that
all connections are tight.
4 Functional description
The CoolSafe Basic or Pro including a vacuum pump and a chamber or manifold is a standalone
unit.
On the Basic models the chamber temperature is displayed and on the Pro models the chamber
temperature and the chamber pressure is displayed. Further the status of the freeze-dryer is shown
in the display.
4.1 Control panel
The basic models display comprise an AWO-indicator and a two-line alphanumerical display as
shown below.

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The Pro models display is the same with the exception that condenser pressure is displayed as
shown below.
4.2 Valves and connections
The CoolSafe is equipped with several valves and connections that makes the freeze-dryer function
and operate correctly. Each must be set correctly and plugged in correctly to make the CoolSafe
operational.
4.2.1 Power supply and ON/OFF switch
The CoolSafe is designed to be plugged into a standard wall socket with build in earth and minimum
10 A fuse.
The CoolSafe is delivered with a country specific power cable, which is connected to the unit on the
lower left hand side on the back panel. The main ON/OFF switch is placed on the front panel of the
unit.When switched on the switch is illuminated green.
4.2.2 Vacuum pump connection
The connection for the vacuum pump is placed on the back of the cabinet. The connection between
the vacuum pump and the freeze dryer is a vacuum hose, which is clamped to the nozzles on the
vacuum pump and the freeze dryer with the delivered clamps.

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4.2.3 Electrical vacuum valve
All models are equipped with an electrical vacuum valve. It is operated via a switch located on the
front of the cabinet.
Do not open the vacuum valve until the AWO-indicator is green.
4.2.4 Drain valve
The drain valve is placed on the front of the cabinet. After de-icing or cleaning of the ice condenser
it can be drained through the drain valve.
A hose may be attached to the nozzle tominimize spillage. Remember to close the drain valve after
use.
5 Operation
The freeze-drying process is a balance between the heat absorbed by the sample to vaporize the
ice, and the heat removed by the condenser to convert the water vapor into ice.
It is important to remember following factors when trying to obtain efficient utilization of the freeze
dryer system.
The efficiency of the freeze-drying process depends upon:
The surface area and the thickness of the sample.
The temperature of the condenser and the vacuum obtained.
The eutectic point (melting temperature) and the concentration of the sample solution.

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5.1 User interface
On start-up, the display will show the CoolSafe model designation, the software version number and
the total number of hours the unit has run since last reset of the hour counter.
When running the display will show the current status of the unit and the AWO-indicator will either
show constant or blink with the color appropriate (see below).
5.2 Error situations, status and error codes
5.2.1 Status codes
A number of different codes gives information on the current status of the freeze dryer:
AWO
Color
Description
-55 °C
-95 °C
&
-100 °C
-110 °C
OK
The ice condenser temperature is near or at reachable temperature.
The ice condenser is ready for the freeze-drying process. The freeze
dryer will be in Await-state until these temperatures are reached for
the first time after power up. Ice condenser ready.
-40 °C
-90 °C
-90 °C
Wait
Will be shown while the ice condenser is cooling down. Change to
OK-state when the ice condenser reaches this temperature for the
first time. Ice condenser not ready.
-40 °C
-70 °C
-70 °C
Wait
If the temperature in the ice condenser increase to over this
temperature, during the freeze-drying process, the Await-state is
invoked until the ice condenser reaches this temperature again,
where OK-state is returned. Ice condenser overloaded.
-30 °C
-70 °C
-70 °C
Wait
(Alarm)
If the temperature in the ice condenser increase to over this
temperature, during the freeze-drying process, the Alarm-state is
invoked until the ice condenser reaches this temperature again,
where Await-state is returned.
-20 °C
-50 °C
-50 °C
5.2.2 Error codes
The following situations will invoke an alarm that will be shown in the status line on the Basic or Pro
screen:
Displayed code
Description
-55 °C
-95 °C
&
-100 °C
-110 °C
E1
PT-1000 element short circuited.



E2
Not implemented.
-
-
-
E3
PT-1000 element interrupted.



E4
Pressure sensor interrupted or shorted.



E5
Switched on more than 8000 hours.



E6
Supply voltage is too high.



E7
Supply voltage is too low.



E8
Pressure sensor signal is too high.



E9
Pressure switch activated.
N/A



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5.3 Preparations
Check that the CoolSafe ice condenser is free from ice and water, and that all valves i.e. the drain
valve is closed. Check that there is no water in the drain valve.

Note
Do not use any tools to close valves, as they will easily be damaged.
Check that the gas ballast valve on the vacuum pump is open at all times.
Check the oil level in the pump and the oil mist filter. The filter should have only a maximum
10 mm oil level (preferably it should be empty).
Switch on the CoolSafe and the vacuum pump.
The lowest temperature should be achieved within 60 minutes.
The vacuum pump should now be allowed to run for at least 30 minutes to achieve the
lowest vacuum performance. The electrical vacuum valve remains closed until you enter
the freeze-drying modes (opened via the green switch button on the front of the Basic or
Pro cabinets).
5.4 Freeze drying using manifolds
1. The manifold is connected to the conus in the lid. Make sure this connection is tight. Check
that all rubber valves are closed (A) or in vacuum-release position (C), and that the flange
and lid are tight.

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2. Start the creation of vacuum by opening the vacuum valve and check that the AWO-
Indicator stays green indicating OK for freeze-drying.
3. Connect a flask to an appropriatecone on therubber valve. Turn therubber valve toposition
(B). The AWO-Indicator should always be green prior to connecting the next flask. The
freeze-drying process is now in progress.
Freeze drying
Air flow
(B)
4. To stop the freeze-drying process, turn the rubber valve handle 180° to position (C) to
equalise the pressure in the flask, and remove the flask from the cone.
Vacuum release
Air flow
(C)
5. Close the vacuum valve after removal of the last flask.
6. To allow the system to equalise the vacuum in condenser, use the release function.
5.5 Freeze drying using chambers

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Cold shelves
1. Make sure that the vacuum valve is closed.
2. Mount the chamber and shelf arrangement. Check that all connections are tight and the
chamber is closed. If heated shelves are to be used, refer to the controller manual.
3. Open the chamber place the frozen material on the shelves in the chamber. Close the
chamber.

Note
Make sure that both drain valve and release valve are closed.
4. Open the vacuum valve. The freeze-drying process is now in progress.
5. To stop the freeze-drying process, close the vacuum valve and equalise the pressure by
opening the release valve at the back.
6. Remove the material from the shelves.
5.6 Stopping the vacuum pump

Note
Keeping the pump at operation temperature and with open gas ballast valve
minimises the risk for harmful condensation of vapours in the pump.
Caution
Do not stop the vacuum pump during the freeze-drying process!
Close the vacuum valve and let the pump run for a minimum of 45 minutes after the freeze-drying
has ended. This is to avoid any possible condenses remaining in the pump oil.
If the freeze dryer is used regularly during the week, it is recommended that the vacuum pump run
constantly with open gas ballast valve and closed vacuum valve.
5.7 Hints, tips and reminders
The selection of the appropriate samplecontainer is important to ensure samples are dried
efficiently. Freeze drying emanates from the surface area of the sample, so the larger the
surface area in respect to its depth/thickness is a determining factor in the speed of the
drying cycle. “Never let the depth of sample exceeds its diameter” especially in vials, flasks
trays etc.
Maintain the vacuum pump regularly, oil changes must be made as per manufacturer’s
instructions. Poor vacuum performance could mean contaminated oil.
Ensureall seals and surfaces are clean and properly seated to avoid vacuum leaks. Always
start the freeze dryer and the vacuum pump 30-40 minutes before use.
Keep the freeze dryer operational if you expect to use it more than once during the day.

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6 Maintenance
6.1 CoolSafe freeze-dryer
The air-cooled condenser must be cleaned minimum once a year. Use a vacuum cleaner and
remove any dust in the cooling ribs on the front.
Rubber valves, black O-rings and valves on the manifold and black O-rings on chambers should be
greased with an ultra-thin layer of vacuum grease and wiped off with a soft cloth every 3-4 months.
The rubber must appear shiny, smooth and without cracks. All silicone gaskets need only dust
removal (do not use any vacuum grease).
6.2 Vacuum pump
See the vacuum pump instruction manual for maintenance according to supplier’s recommendation.
Maintenance for a vacuum pump in general will be to:
Check the oil volume and colour conditions regularly. The oil should be changed every 400-
500 working hours, more often if aggressive vapours have been pumped. Keep a Log book
Drain the oil mist filter if the oil level is more than 10 mm.
Drain, clean and eventually change the filter insert if smoke comes from the oil mist filter.
6.3 Cleaning

NOTE
When using strong materials such as strong acids or bases, radioactive substances
and volatile organic solvents it must be handled carefully and promptly cleaned up if
spilled.
If a sample is spilled in the concentrator chamber, it must be cleaned up immediately.
Cleaning of acrylic components use only mild detergents solutions NEVER solvents.
Wipe stainless steel surfaces with alcohol and then dry, do not use abrasives.
Thecondenser of the CoolSafe once drained, wipe dry and then lightly cleaned with alcohol,
ensure that the drain valve is open. Do not forget to close the valve once the condenser
has dried.
6.4 Checking for leaks on the CoolSafe freezer-dryer
Always start from the vacuum pump and work forwards towards the chamber.
1. Check vacuum hose connection to the pump. If the pump is fitted with a nozzle and if this is
held in place with a clamp, check that there is a centring ring with seal fitted between the
flange on the pumpandthenozzle. Make sure theclamp istight andthat thehose is pushed
well onto the nozzle, and that the clip on the hose is tight.
2. Check the other end of the vacuum hose where it connects to the CoolSafe, make sure the
clip is tight.
3. The drain valve on the front of the Cool Safe also has tobe checked for leaks. First unscrew
the drain valve (with black knob) all the way until its loose and then pull towards you. The
barrel of the valvethen comes away from the body. On the end of the barrel there is a white
Teflon plug, make sure this is clean and without any scratches, also wipe the inside of the
valve body. Replace the valve barrel into the body of the valve, push in and then screw the
valvecompletely tothe fully closed position. When vacuum is applied check that there is no

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leak from the drain-this can be done placing a finger over the drain spigot, you will feel if
there is a leak.
4. Check the seal on the acrylic plateof the chamber that interfaces with the top stainless steel
part of the CoolSafe. This can be done by squirting or brushing some frothy soap solution
all around, if there is a leak this will be sucked in towards the condenser.
5. If leak(s) are found on the seals, clean both the surface of the s/steel and the seal, using a
clean tissue slightly wetted with alcohol.
6. Check that the lid of the chamber is located correctly, again check that the seal is OK as
previous.

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7 The Freeze-drying process
To understand the freeze-drying process, this section describes the theory for the process in short.
For more detailed information about freeze-drying please consult available literature.
All material in free form will exist in one of three states: Vapour, liquid or solid.
As shown in the diagram for water, the physical state is dependent on the surrounding pressure and
the temperature. The point where all three phases of water co-exist is called the triple point.
Freeze-drying is basically a change in state and properties of the material, (water), that is to be
removed. In principle the process is very simple, but in reality it also can be very complex as the
product can consist of many components, which interact with each other.
Moving from one state to another requires the supply or removal of energy to or from the product.
This energy flux will have an impact on the structure of the material being dried.
Freeze-drying is achieved using equipment that controls temperature and pressure in the
environment of the product and is a 3-step process.
In the first step, the product is frozen solid so that the water present in the material is
converted to ice (pre-freeze).
In the second step, the ice formed in pre-freezing is removed from the product by direct
conversion from solid to vapour. This process is called sublimation. In order to start
removing moisture in the sublimation process, the pressure surrounding the material has to
be brought down to a value below that of the triple point, whilst keeping the temperature of
the product below its freezing point. Thecondenser surface temperature must also be down
to a temperature lower than the temperature of the material handled. When the product is
heated, it will theoretically place itself somewhere on the transition line between the solid
and vapour states. The heating will initiate sublimation of the moisture from the product to
the surrounding environment. The vapour will move to the condenser surface because of
the lower vapour pressure in the condenser.

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In the third step, water that is strongly bound to the solids of the sample (called sobbed
water) is converted to vapour and removed from the product, this process being referred to
as de-sorption. Removing moisture in the de-sorption phase or secondary drying phase, is
done at a higher product temperature and at the lowest possible pressure
8 Technical Specifications
8.1 CoolSafe -55 °C
CoolSafe Basic or Pro 55-4
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes–Proonly
Ultimate temperature at 20°C room temperature
°C
-55
Power requirements
V/Hz
230/50-60
Power consumption
W
500
Insulation
mm
90
Condenser capacity
kg
3
Condenser capacity per 24 hours
kg
2,5
Total volume of Condenser
L
4
Weight net
kg
40
Cabinet dimensions (DxWxH)
mm
500x400x520
Cabinet material
Polyestercoatedsteel
Condenser material
StainlesssteelAISI316
Cooling media
R507
Vacuum Valve
Electrical
Drain tap
Yes
CoolSafe Basic or Pro 55-9
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes –Pro only
Ultimate temperature at 20°C room temperature
°C
-55
Power requirements
V/Hz
230/50-60
Power consumption
W
600
Insulation
mm
50
Condenser capacity
kg
7
Condenser capacity per 24 hours
kg
4
Total volume of Condenser
L
9
Weight net
kg
45
Cabinet dimensions (DxWxH)
mm
500x400x520
Cabinet material
Polyester coated steel
Condenser material
Stainless steel AISI 316
Cooling media
R 507
Vacuum Valve
Electrical
Drain tap
Yes

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CoolSafe Basic or Pro 55-15
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes –Pro only
Ultimate temperature at 20°C room temperature
°C
-55
Power requirements
V/Hz
230/50-60
Power consumption
W
800
Insulation
mm
90
Condenser capacity
kg
10
Condenser capacity per 24 hours
kg
6
Total volume of Condenser
L
15
Weight net
kg
70
Cabinet dimensions (DxWxH)
mm
620x495x745
Cabinet material
Polyester coated steel
Condenser material
Stainless steel AISI 316
Cooling media
R 507
Vacuum Valve
Electrical
Drain tap
Yes
8.2 CoolSafe -95 °C and -100 °C
CoolSafe Basic or Pro 95-15
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes –Pro only
Ultimate temperature at 20°C room temperature
°C
-95
Power requirements
V/Hz
230/50-60
Power consumption
W
1400
Insulation
mm
90
Condenser capacity
kg
10
Condenser capacity per 24 hours
kg
6
Total volume of Condenser
L
15
Weight net
kg
85
Cabinet dimensions (DxWxH)
mm
620x495x745
Cabinet material
Polyester coated steel
Condenser material
Stainless steel AISI 316
Cooling media
R 507/R170
Vacuum Valve
Electrical
Drain tap
Yes

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CoolSafe Basic or Pro 100-9
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes –Pro only
Ultimate temperature at 20°C room temperature
°C
-100
Power requirements
V/Hz
230/50-60
Power consumption
W
800
Insulation
mm
90
Condenser capacity
kg
7
Condenser capacity per 24 hours
kg
4
Total volume of Condenser
L
9
Weight net
kg
75
Cabinet dimensions (DxWxH)
mm
620x495x745
Cabinet material
Polyester coated steel
Condenser material
Stainless steel AISI 316
Cooling media
R 507/R170
Vacuum Valve
Electrical
Drain tap
Yes
8.3 CoolSafe -110 °C
CoolSafe Basic or Pro 110-4
Unit
Item
Digital read-out of temperature
Yes
Digital read-out of pressure
Yes –Pro only
Ultimate temperature at 20°C room temperature
°C
-110
Power requirements
V/Hz
230/50-60
Power consumption
W
1000
Insulation
mm
90
Condenser capacity
kg
3
Condenser capacity per 24 hours
kg
2,5
Total volume of Condenser
L
4
Weight net
kg
55
Cabinet dimensions (DxWxH)
mm
500x400x520
Cabinet material
Polyester coated steel
Condenser material
Stainless steel AISI 316
Cooling media
R 507/R1150
Vacuum Valve
Electrical
Drain tap
Yes
9 Accessories