K850 Iss8

K850 Critical Point Drier
Instruction Manual

Document Number A4800148
Issue 8 (04/12)

For technical and applications advice plus our on-line shop for
spares and consumable parts visit www.quorumtech.com

QUORUM TECHNOLOGIES LTD
1 & 3 Eden Business Centre
South Stour Avenue
ASHFORD
Kent, UK
TN23 7RS
Tel: +44(0) 1233 646332
Fax: +44(0) 1233 640744
Email: sales@quorumtech.com
Web : http:///www.quorumtech.com

For technical and applications advice plus our on-line shop for spares and consumable
parts visit www.quorumtech.com

Disclaimer
The components and packages described in this document are mutually compatible and guaranteed
to meet or exceed the published performance specifications. No performance guarantees, however,
can be given in circumstances where these component packages are used in conjunction with
equipment supplied by companies other than Quorum Technologies Ltd.

Quorum Emitech is brand name owned by Quorum Technologies Limited. Quorum Technologies Limited is a subsidiary
company of J udges Scientific plc with registered offices at Unit 19 Charlwoods Road, East Grinstead, West Sussex.
RH19 2HL. Registered in England and Wales, company No. 4273003.

Issue Date Details Revised By
1 23/08/2002 Initial Issue PRM
2 29/12/2003 Revision J B
3 06/09/2004 BS No 8 image corrected PRM
4 22/05/2007 Company details amended KJ W
5 11/10/2007 New images and new document layout J LS
6 12/09/2009 New images and updates to section 4.2 J LS
7 10/08/2011 Figure 4.2 added, NCN0138 applies J LS
8 01/04/2012 Revision as to ECR 1186 PRM

K850 - Instruction Manual 3 A4800148-Issue 8

1 Contents
1.1 Section Contents
1 Contents .......................................................................................................... 3
1.1 Section Contents .................................................................................................. 3
1.2 List of Figures....................................................................................................... 4
1.3 List of Tables........................................................................................................ 4
2 Health and Safety ........................................................................................... 5
2.1 Control of Substances Hazardous to Health (COSHH) ........................................ 5
2.2 WEEE Compliance............................................................................................... 5
2.3 Conformity............................................................................................................ 6
2.4 Hazard Signal Words............................................................................................ 6
2.5 Fail Safe............................................................................................................... 6
3 Description ...................................................................................................... 7
3.1 K850 Critical Point Drier ....................................................................................... 7
3.1.1 Features and Benefits............................................................................................... 8
3.2 Specifications ....................................................................................................... 8
3.2.1 Supplied with Unit..................................................................................................... 8
4 Installation....................................................................................................... 9
4.1 Preliminary Checks............................................................................................... 9
4.2 Connections........................................................................................................ 10
5 Operation....................................................................................................... 13
5.1 Display................................................................................................................ 13
5.2 Initial Operating Checks ..................................................................................... 14
5.3 Specimen Preparation........................................................................................ 16
5.3.1 Fixation................................................................................................................... 16
5.3.2 Dehydration ............................................................................................................ 16
5.3.3 Intermediate............................................................................................................ 16
5.3.4 Transitional fluid...................................................................................................... 16
5.4 Specimen Handling............................................................................................ 17
5.5 Critical Point Drying............................................................................................ 18
5.6 Safety Devices.................................................................................................... 20
5.7 Safety Precautions ............................................................................................. 20
5.8 Summary............................................................................................................ 21
6 Service and Maintenance............................................................................. 22
6.1 Maintenance....................................................................................................... 22
6.2 Spares................................................................................................................ 23
6.3 Accessories........................................................................................................ 23
6.4 Fuse Listings ...................................................................................................... 24
7 Appendices ................................................................................................... 25
7.1 World Wide Electrical Supplies........................................................................... 25
7.2 Cylinder Valve Outlet & Hose Connections ........................................................ 26
7.3 Safe Handling..................................................................................................... 27
7.4 Return of Goods................................................................................................. 28
7.4.1 General Introduction: .............................................................................................. 28
7.4.2 Health and Safety Declaration................................................................................ 28
7.4.3 Despatch................................................................................................................. 28
7.4.4 Return Address:...................................................................................................... 28
7.4.5 Declaration of Contamination Form........................................................................ 29
8 Index .............................................................................................................. 30


A4800148-Issue 8 4 K850 - Instruction Manual

1.2 List of Figures
Figure 2-1: WEEE Directive Symbol......................................................................................................... 5
Figure 3-1: K850 Critical Point Drier......................................................................................................... 7
Figure 4-1: K850 Rear Panel.................................................................................................................. 10
Figure 4-2: K850 Gas Connections........................................................................................................ 11
Figure 5-1: K850 Front Panel ................................................................................................................. 13
Figure 5-2: Sample Holder and Insert in Chamber................................................................................. 14
Figure 5-3: Chamber Fill Level ............................................................................................................... 17
Figure 7-1: BS 341 No 8......................................................................................................................... 26
Figure 7-2: CGA 320.............................................................................................................................. 26

1.3 List of Tables
Table 1: Specifications of the K850 Critical Point Drier............................................................................ 8
Table 2: K850 Rear Panel Functions ..................................................................................................... 10
Table 3: K850 Power Requirements....................................................................................................... 12
Table 4: K850 Front Panel Controls....................................................................................................... 13
Table 5: Safety Devices.......................................................................................................................... 20
Table 6: Summary of Operation............................................................................................................. 21
Table 7:- Maintenance Tasks................................................................................................................. 22
Table 8:- Spare Parts for the K850......................................................................................................... 23
Table 9:- Accessories for the K850........................................................................................................ 23
Table 10:- Fuse Listing for the 230 Volt K850........................................................................................ 24
Table 11:- Electrical supplies World Wide.............................................................................................. 25
Table 12: Safe Handling and Storage of Gases in Cylinders................................................................. 27
Table 13: Declaration of Contamination Form........................................................................................ 29



2 Health and Safety
Safety is very important when using any instrumentation.
Quorum Technologies is committed to providing a safe working environment for its
employees and those that use it's equipment and conducts its business responsibly, and in
a manner designed to protect the health and safety of its customers, employees and the
public at large. It also seeks to minimise any adverse effects that its activities may have on
the environment.
Quorum Technologies regularly reviews its operations to make environmental, health and
safety improvements in line with UK and European Community legislation.
Quorum Technologies cannot be held responsible for any damage, injury or consequential
loss arising from the use of its equipment for any other purposes, or any unauthorised
modifications made to the equipment.
All service work carried out on the equipment should only be undertaken by suitably
qualified personnel. Quorum Technologies is not liable for any damage, injury or
consequential loss resulting from servicing by unqualified personnel. Quorum
Technologies will also not be liable for damage, injury or consequential loss resulting from
incorrect operation of the instrument or modification of the instrument.
2.1 Control of Substances Hazardous to Health (COSHH)
The E.C. legislation regarding the Control of Substances Hazardous to Health requires
Quorum Technologies to monitor and assess every substance entering or leaving their
premises. Consequently any returned goods of whatever nature must be accompanied by
a declaration form Health and Safety Declaration form completed. (Appendix -7.4.5 for the
form)
Without this declaration Quorum Technologies reserves the right not to handle the
substance/item. Also in accordance with E.C. regulations we will supply on request hazard
data sheets for substances used in our instruments.

2.2 WEEE Compliance
This product is required to comply with the European Unions Waste Electrical &
Electronic Equipment (WEEE) Directive 2002/96/EC.

Figure 2-1: WEEE Directive Symbol
For full details of our environmental policies including WEEE please visit
http://www.quorumtech.com/environmental_policy.htm



2.3 Conformity
This Equipment of this Design and manufacture and marked CE, conforms with the
requirements of the European Directives EMC 89/336/EEC & LVD 73/23/EEC.

2.4 Hazard Signal Words
The standard three hazard signal words are defined as follows:
DANGER - imminently hazardous situation or unsafe practice that, if not
avoided, will result in death or severe injury.
WARNING - potentially hazardous situation or unsafe practice that, if not
avoided, could result in death or severe injury.
CAUTION - potentially hazardous situation or unsafe practice that, if not
avoided, may result in minor or moderate injury or damage to equipment.

2.5 Fail Safe
This Equipment will fail safe in the presence of excessive RF, Electrostatic Discharge or
Mains Transients. While a loss of function could occur under extreme circumstances the
Equipments operation will be fully recoverable under normal operating conditions



3 Description
3.1 K850 Critical Point Drier
Critical point drying is so named as it includes, as part of its process, the occurrence
known as the continuity of state for which there is no apparent difference between the
liquid and gas state of a medium, the surface tension between this interface reducing to
zero. This occurs at a specific temperature and pressure with resulting density and is
known as the Critical Point. This condition of zero surface tension can be used to dry
biological specimens, avoiding the damaging effects of surface tension.
In biological specimens we are mainly concerned with the removal of water.
Unfortunately, the critical point for water (H
2
O) of +374C and 3212psi is inconvenient,
and would cause heat damage to the specimen. The most common and convenient
transitional medium for Critical Point Drying is Carbon Dioxide (CO), which has its Critical
Point at 31C and 1072psi. However, it is not miscible with water, and therefore we have
to involve a third medium, commonly Acetone, which is termed the intermediate fluid.
We can now convert our transitional fluid, typically CO
2
, from liquid to gas without surface
tension at the Critical Point.
The K850 Critical Point Drier is designed for use with CO
2
having first replaced any water
in the specimen by a series of dehydration, often in the same fluid such as Acetone or
Ethanol, which will also be the intermediate fluid.
(Wet Specimen) - water - Acetone - 30% - 100% - CO
2
- C.P.D. - (Dry Specimen)
The specimens for Critical Point Drying are located in the pressure chamber of the K850.
The chamber is pre-cooled to allow it to be readily filled with liquid CO
2
from a high
pressure cylinder. The chamber is then heated to just above the Critical Temperature
with subsequent Critical pressure being achieved. The CO
2
gas is vented through a
needle valve, to avoid specimen distortion.
The K850 is fitted with electric heating and adiabatic cooling, and temperature control of
+35C on heating with associated pressure on heating of the order of 1250psi. This
ensures the Critical Point is accurately obtained, avoiding excess pressures or
temperatures, or the need to rely on pressure relief valves to control pressure during the
heating cycle. The chamber is vertical, with top loading, to ensure specimens do not
become uncovered during the drying process, and has a side viewing port to locate the
meniscus for the correct level when initially filling the chamber.

Figure 3-1: K850 Critical Point Drier


3.1.1 Features and Benefits
Vertical chamber with top filling and bottom draining - ensures specimens do not
become uncovered during drying
Side viewing port - great visibility
Adiabatic cooling and thermoelectric heating - accurate temperature control
Fine control needle valve pressure let down - precise control of decompression
and avoids potential damage to specimens by uncontrolled pressure release
Built in magnetic stirrer enhanced solvent exchange.
Temperature monitoring and control with thermal cut-out protection.
Pressure monitoring with safety cut-out for over pressure.
Easy to operate valves light finger pressure only is need to open and close
Safe operation every K850 critical point dryer is pressure tested to 2,500psi
and a pressure certificate issued. The K850 is fitted with a safety bursting disc

3.2 Specifications
Specifications of the K850 Critical Point Drier Unit

Instrument Case 450mm Wide x 350mm Deep x 175mm High
Chamber Size 32mm Internal Diameter x 47mm High
Test Pressure 3000psi
Weight 12 Kg
Operating Temperature Normal Operating Temperature 35
O
C
(Critical Temperature 32
O
C)
Operating Pressure 1350psi (Critical Pressure 1172psi)
Pressure Safety Cut-out 1700psi
Site Considerations Requires Space for CO
2
Cylinder
Electrical 230V 50Hz (3A max)
115V 60Hz (6A max)
Table 1: Specifications of the K850 Critical Point Drier

3.2.1 Supplied with Unit
1 x Stainless Steel Specimen Holder (12 compartments: 8mm x 8mm)
10 x PTFE Porous Pots (12.7mm x 15.7mm, pack 10)
High Pressure CO
2
Hose
Operating Manual and Test Certificate


4 Installation

WARNING MAINS LEAD
This Equipment must be Earthed and fitted with the correct lead for
the country of operation. This will normally be achieved from the
correct mains supply socket.

It is important that this Equipment is installed and operated by skilled personnel in
accordance with these Instructions. Failure to do so may result in damage, and impair
protection provided. 'If in doubt - ASK'.
A suitable location should be provided for the unit - either operated on a bench or the
recommended trolley. The total weight of the system is 18Kg. The system operating
environment ambient temperature range is 15
o
C to 25
o
C in a non-condensing relative
humidity of not more than 75%. Sufficient ventilation is required, and positioning should
be out of direct sunlight. The system is rated for continuous operation other than those
supplies specified.
.
4.1 Preliminary Checks
Remove Instrument from packing and place on appropriate operational position. Carry
out visual inspection for any signs of transit damage. Particular attention should be given
to inspecting the high pressure connecting hose for signs of damage.
In choosing an operational position it should be noted that for normal operation the pre-
cooling and heating parameters might be affected by changes in ambient temperature.
The Instrument should not be located near sources of heat or cold, or any other affects
such as direct sunlight. The area should also be of relatively low humidity to avoid
moisture condensation within the pre-cooled chamber when loading specimens. Also
allow for safe venting of gas. The cylinder of Liquid Carbon Dioxide should be located
adjacent to the right hand side of the Instrument, and should be securely located.
Remove Accessory Pack, and check contents against K850 Despatch Certificate.
Ensure that the Independent Test Certificate is with the Instrument as proof of pressure
testing.
Ensure that all areas of the instrument are free of loose packaging material.
Check that the Instrument is of the correct voltage for the Country of operation by
checking the serial number plate and the voltage label on the back of the Instrument.
The Instrument is designed for use with Acetone or Ethanol as the intermediate fluid, and
Carbon Dioxide (via high pressure Liquid CO
2
cylinder) as the transitional fluid.
Research grade Carbon Dioxide should be used and the cylinder fitted with a siphon tube
(usually denoted by a White stripe on a Black cylinder).



4.2 Connections
Connections should only be made in accordance with instructions. Refer To: Figure 4-1,
Figure 4-2 and Table 2.

Figure 4-1: K850 Rear Panel

UNDER NO CIRCUMSTANCES SHOULD ANY OTHER CONNECTIONS OR
OUTLETS/INLETS BE USED FOR ANY OTHER EQUIPMENT OR SERVICES.

TITLE FUNCTION
Rocker switch Main power on to Instrument.
Power in Main power inlet socket
Liquid CO
2
supply High pressure inlet (Liquid Carbon Dioxide)
Exhaust Gas outlet direct from chamber.
Bleed Gas outlet via flow gauge from chamber.
Vent Gas outlet from Adiabatic cooling system.
Earth Earth Tag
Voltage Correct voltage for Country of operation.
Fuse Main power fuse
Table 2: K850 Rear Panel Functions

WARNING
This equipment can produce high voltages and high pressures
In its operation.

Fuse
Liquid CO
2
Supply
Chamber Exhaust
Safety relief
device located
here behind
plastic cover
Bleed
Gas Vent


WARNING EARTH CONNECTOR
This Equipment is normally supplied from 3 pin supply including Earth.
If only 2 pin supply is available a separate Earth must be fitted.
The supplementary Earth stud can be used to facilitate this requirement.

Carry out high-pressure connections to the Instrument with the flexible braid covered
high-pressure hose provided, See connection diagram Figure 4-2 below.

Figure 4-2: K850 Gas Connections

The Instrument connection is common, and is a direct metal contact via a small nipple
located in the CO
2
supply inlet. Tighten up firmly, using the correct size spanner which,
used normally, will ensure the correct torque is applied. The CO
2
cylinder connection will
vary depending on the Country of operation, and the type of gas cylinder used.
CAUTION: Ensure you have correct connection - if in any doubt -do not fit. (Connector
types are given in Appendix 7.2)
The CO
2
cylinder connection uses a fibre washer, which is provided and should be
placed on the end of the flat face of the connector, inside the nut housing, and matched
with the flat surface of the connection on the high-pressure gas cylinder. The nut should
be tightened up using the correct size spanner which, used normally, will ensure the
correct torque is applied.
CAUTION: Ensure that the gas cylinder is secured and the valve turned off.

WARNING INLET/EXHAUSTS
The applications of these 4 gas connections are given in the layout Figure
4-1. The gas supply from high-pressure cylinder must be fitted with the
correct fitting for the cylinder type. The exhaust, vent & bleed - should be
safely vented.



The electrical input to the Instrument is made with the power lead provided. The
Instrument connection is standard and the lead is fitted with the appropriate plug for the
Country of operation.
(Electrical supplies are given in Appendix 7.1)
For fuse ratings and voltages refer to: Table 10 Fuse Listings

Note: - A single phase AC supply with Earth is required - selected to the correct voltage
for the country of operation. Either nominal 240V or nominal 120V. The voltage
and frequency range is:

Nominal 240 Max. Current 4A 200 - 264V 47Hz To 63Hz
Nominal 120 Max. Current 8A 90V - 132V 47Hz To 63Hz
Table 3: K850 Power Requirements
Any outlet gases from the Instrument should be safely vented. The small-bore tubing
provided can be utilized.
The vent and bleed can be connected using the 'T' piece provided. The exhaust has
separate tubing; this is to allow it to be removed more easily when checking of
intermediate fluid purging.



5 Operation
5.1 Display
The diagram below shows the layout of the instrument front panel.

Figure 5-1: K850 Front Panel

TITLE OPERATION FUNCTIONS
Cool Valve (Blue)
Allows controlled flow of gas to adiabatic cooling system - the change in
pressure giving a cooling effect to the chamber - the adiabatic cooling
system does not let gas into the chamber.
Inlet valve (Green) Allows Liquid CO
2
direct to chamber
Exhaust Valve (Black) Allows direct exhausting of gas from chamber
Bleed Valve (Red) Allows bleeding of gas from chamber.
Temperature Gauge Monitors temperature of chamber
Pressure Gauge ** Monitors direct pressure in chamber
Stirrer Switch
Switches on motor, which is located on the base of chamber, this has a
magnetic coupling to a stirrer bar located inside the chamber.
12V DC LED Indicates 12V dc control voltages are present.
Heater Control LED Indicates when heater is on or off under control mode
Heater Switch Switches power on to heater control system
Table 4: K850 Front Panel Controls
**NOTE: This type of pressure gauge is filled with a 'damping' fluid, often evident by a
small bubble in the gauge dial.
Pressure
Gauge Temperature
Display Stirrer
Switch
Heater
Switch
Cool
(Blue)
Chamber Fill
(Green)
Chamber Out
(Black)
Bleed
(Red) Fine Bleed
(Black)


5.2 Initial Operating Checks
(These should be made having become familiar with the controls.)
Ensure that the high-pressure CO
2
cylinder valve is closed. Check that all valves can be
opened and closed freely. Close inlet valve and open exhaust valve. Remove chamber
lid by unscrewing the three thumbnuts.

CAUTION
When the chamber lid is to be removed or refitted - ensure inlet valve is
closed, exhaust valve is open, and pressure gauge is reading zero.

Position the stirrer bar in the bottom of the chamber. Switch on stirrer, and observe
rotation.
Place the sample holder in the chamber followed by the white PTFE chamber insert see
Figure 5-2. Note the purpose of this insert is to ensure the meniscus appears in the
window during the transition through the critical point therefore its orientation is
important.
Refit the chamber lid, ensuring the 'O' ring is not damaged and is correctly seated.
Tighten thumbnuts firmly in even rotational sequence.

Figure 5-2: Sample Holder and Insert in Chamber
NOTE: The front viewing window assembly includes a quartz glass window and a
polycarbonate (Lexan) shield in front of it for additional safety protection.
Removing or refitting should be carried out with the correct replacement parts,
and in accordance with separate detailed Instructions.
Switch on heater. The heater control should illuminate, and the temperature will increase
gradually at approximately 2C/minute. The chamber will feel slightly warm. Switch off
heater when initial indications are that it is operating. Close all valves, and open CO
2

cylinder valve. Check for any obvious signs of leaks.
Open cool valve by a very small amount until a steady hissing of gas is established.
After a short delay, the temperature will start to fall. The cool down rate is approximately
4
o
C/minute. Shut cool valve when indications are that it is operating.
Open inlet valve. The pressure gauge should read approximately 800psi. Close the inlet
valve, and depressurise the chamber firstly by using the bleed valve and then by using
the exhaust valve for quick depressurising. This will also ensure that the system has
been 'flushed through'. Close the bleed valve and the exhaust valve.
Sample holder
chamber insert


TEST RUN
Open cool valve slowly to establish a steady flow.
The chamber, after an initial thermal delay, should cool down from an ambient
temperature of +20C to +5C in approx. 3minutes. At +5C the cool valve can be closed
and the temperature will 'coast' down to approx. +2C. With practice, a cool valve setting
can be achieved which avoids freezing of the valve and internal pipe-work, thus avoiding
the 'spitting' associated with occasional freezing.
Open the inlet valve slowly, taking approx. 1minute to fill the chamber to the correct level
by observing the meniscus in the viewing window. On filling, the temperature may
increase to +5C. If it gets any warmer, and any difficulty is experienced with filling, then
a small amount of cooling can be applied. The chamber should be filled to the centre of
the viewing window to filling mark shown.
IMPORTANT DO NOT over fill the chamber.
Close the inlet valve and switch on the heater.
NOTE: The high-pressure carbon dioxide cylinder valve can also be closed for
additional safety.
After an initial delay the temperature will increase to the control temperature of +35C,
this takes approximately 35 minutes. At this point it will control switching in and out over
the range 32C to 38C and pressure in the range of 1200 to 1300psi. If the meniscus is
observed, it will fall slightly to the lower fill level of the viewing window.
At a temperature of approximately 30C, and a corresponding pressure of 1,100psi the
meniscus will disappear having reached the Critical Point.
NOTE: Subsequent cooling would allow the re-appearance of the meniscus, should
this be of interest for demonstrations.
The system can now be depressurised whilst maintaining the temperature.
For less delicate specimens the exhaust valve can be used at a rate of 100psi/minute,
taking approximately 10 minutes.
For more delicate specimens the bleed valve can be used, for setting a lower de-
pressuring rate of 1000cm
3
/Minute (2 litre/minute) taking approximately 20 minutes.
The heater can now be switched off.
If a run has to be repeated immediately, then the cooling from the operational
temperature of +35
o
C will take somewhat longer.
If the instrument has to be shut down - the carbon dioxide cylinder valve should be
closed. The cool and exhaust valves open to ensure depressurisation of the lines and
the chamber.
Mains power switched off.


5.3 Specimen Preparation
A range of techniques may be used for specimen preparation and the following in only
intended as a general guide.

5.3.1 Fixation
Fixation generally utilizes an Aldehyde, such as Formaldehyde or Glutaraldehyde to
provide a rapid inter and intra-cellular penetration and fixation, followed by Osmium
Tetroxide for further fixation.

5.3.2 Dehydration
The fixed specimen is taken through a series of increasing concentrations of a drying
liquid such as Acetone or Ethanol, ending in a 100% dehydrating liquid of the highest
possible purity. Typically these are steps of 10, 20, 30, 50, 70, 90, 100% at 10 minutes
each, with 3 changes at 100%.

5.3.3 Intermediate
The intermediate fluid, which is miscible with Carbon Dioxide, is typically the dehydration
fluid and therefore an additional step to the intermediate fluid, prior to Critical Point
Drying, is not required. The most common are Acetone and Ethanol.

5.3.4 Transitional fluid
Carbon Dioxide - Critical Temperature 31.1C, Critical pressure 1072psi.



5.4 Specimen Handling
Generally the wire mesh specimen basket is most commonly used when transferring the
smaller specimen. For larger specimens, the porous pots may be used. The specimen
must be maintained in the dehydration fluid immediately prior to use, then quickly
transferred to the K850 chamber.
NOTE: To avoid specimens becoming uncovered when transferred to the K850
chamber, they should only occupy two thirds of the chamber. (See Fig.5-3)

Figure 5-3: Chamber Fill Level

Fill Level


5.5 Critical Point Drying
The following is only a brief outline and guide. For further details consult:-

1. COHEN, A.L..
"Critical Point Drying - Principles and Procedures."
Electron Microscopy 1979 II 303-324.
(Available on Request)
NOTE: Ensure all valves are closed.
a) Pre cool the chamber to +5C using the cool valve as previously described.
b) Transfer the specimen, avoiding any unnecessary delay.
c) The inlet valve is opened and the CO
2
level is filled to the top of sight glass, after
soaking, fresh CO
2
can be added by opening the exhaust draining the unit to the
bottom or even below the sight glass. This is repeated until the solvent exchange
is completed. The Chamber should now be filled for the final time for Critical Point
Drying; it is at this stage that it is IMPORTANT to just fill the CO
2
to the Top of
the upper red line . See image 5.3 but not above the upper small hole behind
the glass. This is to avoid excess pressure when heaters are applied.

NOTE: The high-pressure carbon dioxide cylinder valve can also be closed for
additional safety.
After an initial delay the temperature will increase to the control temperature of +35C,
this takes approximately 35 minutes. At this point it will control switching in and out over
the range 32C to 38C and pressure in the range of 1200 to 1300psi. If the chamber
insert is installed and the meniscus is observed during the heating phase , it may initially
rise out of view of the window and then come back into view fall to the lower level of the
viewing window (this depends on the ratio of liquid to air space in the chamber).
At a temperature of approximately 30C, and a corresponding pressure of 1,100psi the
meniscus will disappear having reached the Critical Point.

NOTE: Subsequent cooling would allow the re-appearance of the meniscus, should
this be of interest for demonstrations.
d) Allow the specimen to soak for approximately 5 minutes (for very large specimens
the soak period should be double) during this period the stirrer may be used to
enhance solvent exchange.
e) The chamber should now be purged for approximately 1 minute. This is achieved
by slowly opening the exhaust valve and observing the meniscus to fall slightly.
The inlet valve should now be opened slightly to compensate and balance the
system thereby replenishing the chamber with 'fresh' Carbon Dioxide.

NOTE: The rotating stirrer should be switched off for the purging, as both Acetone
and Ethanol are more dense so will go to the bottom of the chamber which is designed to
be top filling bottom draining.
f) Ensure the meniscus is at the centre of the viewing window. Repeat the soak as
(d).
g) A further purging should now be carried out as in (e) during the second purging of 1
minute, a check can be made to see that solvent exchange has been achieved:
Remove the plastic pipe from the exhaust outlet. Using a small disc of filter paper,
place into the stream of gas. The presence of a small damp patch will indicate if
solvent is present. If necessary, repeat a soak and purge step.


h) Ensuring meniscus is at the fill the CO
2
to the Top of the upper red line, close
all valves. For added safety also close the carbon dioxide cylinder valve.
i) Switch on heater and allow stable conditions to be reached of approx. 35C and
1250psi. This will take about 35 minutes.
j) The chamber may now be depressurised as described previously.
1. Exhaust Valve at 100 psi/minute.
2. Bleed valve and needle valve (delicate specimen) at 1000Cm
3
/minute flow
rate.
k) Specimen can now be removed and subsequently treated. In all cases, this should
be maintained in dry conditions.
l) The K850 Instrument can now be re-used or shut down, as previously described.



5.6 Safety Devices

SAFETY DEVICES PRESSURE
Chamber normal maximum working pressure 1500psi
Complete unit workshop tested. 2250psi
Quartz viewing window fitted with polycarbonate
shield (Lexan) tested as part of chamber assembly.
NOTE: Chamber and Quartz window have on a
type test been independently tested to 4370psi.
To 2250psi
Temperature controller factory set.
Mid point: 35
o
C range: 32C to
38C. Typical pressure: 1200psi
to 1300psi
Pressure switch non adjustable Set at: 1700psi 50psi
Rupture disc non adjustable Burst at: 1900psi
Table 5: Safety Devices

5.7 Safety Precautions
a) Locate in suitable area in firm position.
b) Ensure correct venting and ventilation.
c) Secure CO
2
cylinder.
d) Avoid trapping or kinking of high-pressure hose and vent tubing.
e) Close cylinder valve when not in use.
f) Open all instrument valves when not in use-switch off at mains.
g) Ensure all fittings are correct on initial installation. IF IN ANY DOUBT - PLEASE
ASK.
h) Wear safety spectacles for additional safety when viewing window direct.
i) Advise with notices all staff of presence and nature of equipment.
WARNING - HIGH PRESSURE EQUIPMENT.
j) Use only correct replacement parts from manufacturer. If quartz window or chamber
lid assembly shows any sign of damage even if instrument appears to be functioning
normally DO NOT USE.
k) Use only Acetone or Ethanol as intermediate fluid.
l) Use only Carbon Dioxide as transitional fluid. (Research grade with siphon tube.)



5.8 Summary

PROCEDURE TEMPERATURE/TIME
PRESSURE
1 Dehydrate specimens Acetone or Ethanol
2 Ensure all valves are closed.
3 Pre-cool chamber using cool valve (Blue). Avoid
excessive flow and freezing up.
+5C - 4 Minutes
4 Load specimens and chamber insert ensure thumb-
screws correctly tightened. Check chamber is
depressurised.

5 Fill chamber, with meniscus to centre of view window
using inlet valve (Green) all other valves closed.
1 Minute
6 Soak (with stirrer if required). +5C - 3 Minutes
7 Purge chamber, maintaining meniscus at least mid
way on view window using slow, steady flow using
balance of inlet valve (Green) and exhaust valve
(Black).
1 Minute
8 Soak (with stirrer if required). If necessary - pre-cool
chamber using cool valve (Blue). All other valves
closed.
+5C - 3 Minutes
9 (Repeat 7). Checking with filter paper at outlet of
exhaust at rear of instrument for damp patch
indicating solvent exchange condition.
1 Minute
10 Fill Chamber to centre of chamber to the Top of the
upper red line Close all valves. Switch on heater.
Allow stable conditions.
+35C - 35 Minutes
1250psi.
11
De-pressurise system:
(a) Exhaust valve (Black) - Non delicate or;
(b) Bleed valve (Red) - Delicate
100psi/Minute +35C 10
Minutes
1000cm
3
/Minute +35
o
C
20 Minutes
12
Repeat run. Pre cooling.
8 Minutes
+35
o
C TO 5
o
C
13 Shut down instrument.
(a) Close CO
2
cylinder valve.
(b) Open exhaust valve (Black).
(c) Open cool valve (Blue).
(d) Switch off mains electricity.

Table 6: Summary of Operation


6 Service and Maintenance
For technical and applications advice plus our on-line shop for spares and
consumable parts visit www.quorumtech.com

CAUTION
Ensure mains electrical power is off during any maintenance and service
activities

6.1 Maintenance
PROCEDURE FREQUENCY
Check chamber lid 'O' ring Weekly
Check chamber studs and thread condition Monthly
Check chamber thumb screws and thread condition Monthly
Check condition of viewing window
Check tightness of viewing window screws. (Only
dismantle and change in accordance with Instructions
supplied with replacement parts)
Weekly
Check high-pressure hose for signs of damage.
Weekly and/or prior to
sustained period of use.
Check high-pressure hose connections at instrument and
cylinder for tightness.
Weekly and/or prior to
sustained period of use.
Check valve-locking nuts for tightness (Only dismantle and
change in accordance with Instructions supplied with
replacement parts).
Weekly
Check condition of mains power cord. Weekly
Table 7:- Maintenance Tasks
NOTE: Consumables and spare items can be obtained from Quorum Technologies Ltd
or approved distributor. Only Quorum Technologies Ltd recommended items
should be used. For technical assistance and advice contact Quorum
Technologies Ltd.



6.2 Spares
The following are available from Quorum Technologies, or your local distributor, and are
featured in more detail in the current Quorum Technologies Consumables Catalogue.
Copies can be sent on request.

SPARES FOR K850 CRITICAL POINT DRIER CATALOGUE
NUMBER
QUANTITY

Chamber Lid 'O' Rings 51000017 5
Knurled Thumb Screws 14700004 3
High Pressure Hose 60200118 1
High Pressure Hose Fibre Washer BS8 60200073 5
High Pressure Hose Fibre Washer CGA 60200074 5
Quartz Window ** 52000001 1
Polycarbonate Protective Shield ** A4800008 1
Viewing Window 'O' Ring ** 51000010 5
Viewing Window Washer ** A4800043 5
Needle Valve 60100008 1
Regulating Valves 60100014 4
Rupture Disc Replacement Kit 60100037 1
Table 8:- Spare Parts for the K850
** NOTE: In the unlikely event that the quartz window cracks or shows any signs of
damage - please inform Quorum Technologies immediately, and ensure the Instrument is
clearly marked: DO NOT USE.

If the polycarbonate protective shield becomes scratched or damaged, it can be replaced
without having to replace the quartz window.
These items should only be changed in accordance with Instructions.

6.3 Accessories
The following are available from Quorum Technologies, or your local distributor, and are
featured in more detail in the current Quorum Technologies Consumables Catalogue.
Copies can be sent on request.

USEFUL ACCESSORIES FOR K850

CATALOGUE
NUMBER
QUANTITY
Porous Specimen Pots P8003 10
Stirrer Bars S8657 3
Safety Spectacles S8656 1
Table 9:- Accessories for the K850


6.4 Fuse Listings
Fuse listing for the K850 Fuse 1

TITLE RATING FUNCTION
240 Volts T630mA Ceramic Mains Power
120 Volts T1A Ceramic Mains Power
Table 10:- Fuse Listing for the 230 Volt K850

Replacement fuses can be supplied by Quorum Technologies Ltd, or the approved
distributor.**

** If an approved distributor is not known - please contact Quorum Technologies Ltd
direct for details.


7 Appendices
7.1 World Wide Electrical Supplies

COUNTRY VOLTAGE FREQUENCY
Australia 240V 50Hz
Brazil 115V/230V 60Hz
Canada 115V 60Hz
Finland 230V 50Hz
France 230V 50Hz
Germany 230V 50Hz
India 230V 50Hz
Ireland 230V 50Hz
Israel 230V 50Hz
Italy 230V 50Hz
Korea (South) 230V 60Hz
J apan 115V 50 / 60Hz
Netherlands 230V 50Hz
Norway 230V 50Hz
Pakistan 230V 50Hz
Portugal 230V 50Hz
Scandinavia 230V 50Hz
Singapore 230V 50Hz
Spain 230V 50Hz
Taiwan 115V 60Hz
Turkey 230V 50Hz
United Kingdom 230V 50Hz
United States of America 115V 60Hz
Table 11:- Electrical supplies World Wide


7.2 Cylinder Valve Outlet & Hose Connections

Figure 7-1: BS 341 No 8

Used in the UK. France, Germany, Italy, Sweden

Figure 7-2: CGA 320

Used in the USA and J apan

CAUTION
It is important to check the Correct Hose Connection to High Pressure
CO
2
Cylinder.
If in doubt - Do not fit - Please ask



7.3 Safe Handling
Safe handling and storage of gases in cylinders

Introduction
The following general practices are recommended for the safe handling and
storage of high-pressure gaseous and liquefied-compressed gases in
transportable containers. Additional precautions may be necessary depending
upon the category to which the gas belongs (corrosive, toxic, flammable,
pyrophoric, oxidant, radioactive or inert), the individual properties of the gas, and
the process in which it is used.
General
Only trained persons should handle compressed gases.
Observe all regulations and local requirements regarding the storage of
containers.
Do not remove or deface labels provided by the supplier for identification of the
container contents.
Ascertain the identity of the gas before using it. Know and understand the
properties and hazards associated with each gas before using it.
Establish and implement plans to cover any emergency situations that might
arise.
When doubt exists as to the correct handling procedure for a particular gas
contact the supplier.
Handling
and Use
Wear stout gloves.
Never lift a container by the cap or guard unless the supplier states it is designed
for that purpose.
Use a trolley or other suitable device or technique for transporting heavy
containers, even for a short distance.
Leave valve protection caps (where provided) in place until the container has
been secured against a wall or bench or placed in a stand and is ready for use.
Never remove valve guards or cages, which permit access to the container valve.
This type of valve protection is intended to be permanently attached.
Where necessary wear suitable eye and face protection. The choice between
safety glasses, chemical goggles, or full-face shield will depend on the pressure
and nature of the gas being used.
Where necessary for toxic gases see that self-contained positive pressure
breathing apparatus or a full-face airline respirator is available in the vicinity of the
working area.
Check for gas leaks using a suitable method. Flammable and toxic gas monitors
are available. Where a gas is toxic check special procedures specified by
supplier.
Ascertain that an adequate supply of water is available for first aid, fire fighting, or
dilution of corrosive material in the event of leakage.
Employ suitable pressure regulating devices on all containers when the gas is
being emitted to systems with a lower pressure rating than that of the container.
Before connecting the container for use ensure that back feed from the system
into the container is prevented.
Ascertain that all electrical systems in the area are suitable for service with each
gas.
Never use direct flame or electrical heating devices to raise the pressure of a
container. Containers should not be subjected to temperatures above 45
o
C.
Never re-compress a gas or a gas mixture from a container without consulting the
supplier.
Never attempt to transfer gases from one container to another.
Do not attempt to increase liquid draw-off rate by pressurising the container
without first checking with the supplier.
Table 12: Safe Handling and Storage of Gases in Cylinders



7.4 Return of Goods
Safety information for the return of Preparation Equipment and Accessories.
7.4.1 General Introduction:
The employer (user) is responsible for the health and safety of his employees. This also
applies to all those persons who come into contact with the Preparation Equipment and
Accessories either at the users or manufacturers premises during repair of service. The
contamination of Preparation Equipment and Accessories has to be declared and the
Health and Safety Declaration form completed. (Appendix -7.4.5 for the form)

7.4.2 Health and Safety Declaration
Those persons carrying out repair or service have to be informed of the condition of the
components. This is the purpose of the Declaration of Contamination of Preparation
Equipment and Accessories..

7.4.3 Despatch
When returning equipment the procedures set out in the Operating Instructions must be
followed. For example:
- Drain the vacuum pumps.
- Neutralise the flushing with gas.
- Remove filter elements.
- Seal all outlets.
- Pack glass components safely.
- Pack loose attachments securely for example stages.
- Seal in heavy duty polythene or a bag,
- Despatch in suitable transport container.

7.4.4 Return Address:
F.A.O.: The Service Manager,
Units 1 & 3 Eden Business Centre
South Stour Avenue,
ASHFORD,
Kent. TN23 7RS



7.4.5 Declaration of Contamination Form

Declaration of Contamination of Preparation Equipment and Accessories.
The repair and/or service of Preparation Equipment and Accessories can only be carried out if a correctly completed declaration
has been submitted. Non-completion will result in delay. The manufacturer reserves the right to refuse acceptance of
consignments submitted for repair or maintenance work where the declaration has been omitted.
This declaration may only be completed and signed by authorised and qualified staff.
1. Description of component
- Equipment type/model: _________________________
- Code No:. ________________________________
- Serial No.: ________________________________
- Invoice No. (if known) ________________________
- Delivery Date.: (if known)________________________
2. Reason for return:
__________________________________________
__________________________________________
__________________________________________
__________________________________________
__________________________________________
3. Equipment condition
- Has the equipment been used? Yes/No
- What type of operating medium was used?
_____________________________________________
- Is the equipment free from potentially harmful
substances? Yes/No
(If Yes go to Section 5)
(If No go to Section 4)
4. Process related contamination of Equipment/
Accessories.
- Toxic Yes/No
- Corrosive Yes/No
- Explosive* Yes/No
- Microbiological* Yes/No
- Radioactive* Yes/No
- Other harmful substances Yes/No

* We will not accept any Equipment/Accessories which have been radioactively, explosively, or microbiologically
contaminated without written evidence that such Equipment/Accessories have been decontaminated in the
prescribed manner.

Please list all harmful substances, gases and dangerous by-products, which have come into contact with the
Preparation Equipment and Accessories.

Trade name
Product name
Manufacturer
Chemical name and
symbol
Danger
class
Precautions
associated with
substance.
First aid measures in
the event of an
accident.
1.
2.
3.
4.
5.

5. Legally Binding Declaration.
I hereby declare that the information supplied on this form is complete and accurate. The despatch will be in
accordance with the appropriate regulations covering Packaging, Transportation and Labelling of Dangerous
Substances.
Name of Organisation: __________________________________________________________________
Address: _____________________________________________________________________________
_____________________________ Post Code: ______________________
Tel.: _____________________________ Fax.: ______________________
Name: _____________________________ J ob Title: ______________________
Date: _____________________________ Company Stamp: ______________________

Table 13: Declaration of Contamination Form


8 Index
A
Accessories...................................................23
Appendices ...................................................25
C
C.O.S.H.H. ......................................................5
Conformity.......................................................6
Connections ..................................................10
Contents..........................................................3
Critical Point Drying.......................................18
Cylinder Valve Outlet & Hose Connections ..26
D
Declaration of Contamination Form..............29
Description......................................................7
Display...........................................................13
F
Fail Safe..........................................................6
Features and Benefits.....................................8
Fuse Listings.................................................24
H
Hazard Signal Words......................................6
Health and Safety............................................5
I
Index..............................................................30
Initial Operating Checks................................14
Installation.......................................................9
Instrument Case..............................................8
K
K850 Critical Point Drier..................................7
L
List of Figures..................................................4
List of Tables...................................................4
M
Maintenance..................................................22
O
Operating Pressure.........................................8
Operating Temperature..................................8
Operation......................................................13
Operation Functions .....................................13
P
Preliminary Checks.........................................9
R
Return of Goods ...........................................28
Despatch.......................................................... 28
General Introduction......................................... 28
Health and Safety Declaration.......................... 28
Return Address ................................................ 28
S
Safe Handling...............................................27
Safety Devices..............................................20
Safety Precautions........................................20
Section Contents ............................................3
Service and Maintenance.............................22
Spares...........................................................23
Specifications..................................................8
Specimen Handling.......................................17
Specimen Preparation..................................16
Dehydration...................................................... 16
Fixation............................................................. 16
Intermediate ..................................................... 16
Transitional fluid............................................... 16
Sputtering Rate.............................................28
Summary.......................................................21
Supplied with Unit...........................................8
W
WEEE Compliance.........................................5
Weight.............................................................8
World Wide Electrical Supplies.....................25

Units 1 & 3 Eden Business Centre
South Stour Avenue
ASHFORD
Kent, UK
TN23 7RS
Tel: +44(0) 1233 646332
Fax: +44(0) 1233 640744
Email: sales@quorumtech.com
Web: http:///www.quorumtech.com

For technical and applications advice plus our on-line shop for spares and consumable parts
visit www.quorumtech.com

Quorum Technologies Limited, company No. 4273003. Registered in England and Wales.
Registered offices:- Unit 19 Charlwoods Road, East Grinstead, West Sussex. RH19 2HL

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