Linkam Scientific Instruments CCR1000 User manual

CCR1000
Catalyst Cell Reactor
Linkam Scientific Instruments
USER GUIDE

2
Contents
Before Setting Up Your Equipment……………………………………………………………………………..…...3
Important Notice ............................................................................................................... 4
Warranty........................................................................................................................... 4
Technical Support.............................................................................................................. 4
Equipment Maintenance..................................................................................................... 4
Pressure Warning .............................................................................................................. 4
Safety Precautions ............................................................................................................. 5
Symbol Reference.............................................................................................................. 5
Feedback .......................................................................................................................... 5
Introduction ...................................................................................................................... 6
Stage Anatomy ............................................................................................................ 6
Mounting Stage to Microscope with Dovetail Substage ......................................................... 7
Set Up the CCR1000 .......................................................................................................... 8
Electrical Cable Connectors........................................................................................... 8
Connection to T95 System Controller ............................................................................ 9
Connect the ECP Water Circulator Pump.......................................................................10
Connect the Gas Lines ................................................................................................10
Pressure Warning...........................................................................................10
Load a Sample..................................................................................................................11
Remove Sample Holder ...............................................................................................11
Load Sample Filter ......................................................................................................12
Warning .........................................................................................................12
Important Note Before Heating Sample ...........................................................12
Load Sample into Sample Holder .................................................................................13
Load Sample Holder into CCR1000...............................................................................14
Appendix..........................................................................................................................15
Spares and Accessories ...............................................................................................15
Contacts Details................................................................................................................16

3
Before Setting Up Your Equipment
Please register your products by going to www.linkam.co.uk and click on the
product/software registration button.
You will need to register your equipment with us to:
 Activate your warranty and technical support
 Access the online setup videos
 Permanently unlock the Linksys32 software (if purchased)
If you have purchased Linksys32 software, please install the software first. This pro-
cess will guide to register all of your products.
See Linksys32 manual for further installation instructions.
A CD with a setup videos is supplied with your system.

4
Important Notice
Please check that your Linkam equipment has not been damaged during transport. If there is any evidence
of external damage DO NOT SWITCH ON ANY ELECTRICAL ITEMS.
Contact LINKAM SCIENTIFIC or their appointed distributor immediately. Your warranty may be im-
paired if Linkam is not informed of any transport damage within 7 working days of delivery.
NO attempt should be made to repair or modify the equipment in any way, as there are no user replaceable
parts.
No attempt should be made to open the case except by qualified personnel as hazardous voltages are pre-
sent.
Please contact Linkam for custom modifications for specific applications.
In order to use this equipment successfully, please take time to read this manual all the way through before
starting to work.
Warranty
This equipment has a warranty against defects in material and workmanship for a period of 12 months.
Linkam will either repair or replace products that prove to be defective. For warranty service or repair,
this product must be returned to Linkam or a designated service facility.
The warranty shall not apply to defects resulting from interfacing, unauthorized modification or misuse,
operation outside of the environmental specifications for the product, or improper site preparation or
maintenance.
Technical Support
Any technical questions or queries should be addressed to the Technical Support Department at the ad-
dress shown on the back of this manual.
Equipment Maintenance
The programmer does not require any regular maintenance. If for any reason it is necessary to check the
electronic calibration then a set of standard resistances can be supplied, which simply plug into the pro-
grammer in place of the stage, and indicate known temperature values. The standards are traceable to
NAMAS (National Accreditation of Measuring and Sampling)
Before cleaning the case or front panel of the programmer, remove the mains lead from the wall outlet.
Use a small quantity of isopropyl alcohol with a soft cloth and gently wipe the surface.
Pressure Warning
The CCR1000 has been tested to 5bar pressure using 22mm quartz windows of 1mm thickness. Windows
must always be inspected with magnifying lens to check there are no microscopic cracks or scratches
before using the stage under pressure. Never stand within 1m of CCR1000 when using high pressure
between 2-5bar.
Linkam cannot guarantee pressure with IR transparent windows due to the inconsistent mechanical
strength of the windows.
Contact Linkam if there is any concern with pressurizing this stage.

5
Safety Precautions
1) Read this guide before using the equipment. Save these instructions for later use.
2) Follow all warnings and instructions which may be placed on the programmer or stage.
3) If for any reason the mains fuse needs to be replaced then it must be replaced by one of the same
type and rating as shown in the equipment ratings.
4) To prevent electric shock, do not remove the cover of the controller or associated electronics.
5) Never use the equipment if a power cable has been damaged. Do not allow any heavy objects to
rest on the power cables. Never lay the power cables on the floor.
6) Do not obstruct any ventilation holes. Do not attempt to insert anything into these openings.
Provide adequate ventilation of at least 75mm all around the equipment.
7) Do not expose the equipment to water. If for any reason it gets wet then unplug it from the mains
and contact Linkam Scientific Technical Support.
8) The equipment is not intended to be used outdoors.
9) Each product is equipped with a 3-wire grounded (earth) mains plug or a free-end 3 wire
mains lead. The plug only fits into a grounded-type outlet. The free-end mains lead should be
connected to a correctly grounded 3-wire mains outlet. Do not defeat the purpose of the grounded
(earth) type plug.
Free - end mains leads are colour coded as follows :
Colour Function
Brown Live
Blue Neutral
Green/Yellow Earth (Ground)
10) If any problems occur then unplug the equipment from the mains outlet and contact Linkam Sci-
entific Technical Support.
11) Do not remove the cover from the equipment unless the mains inlet has been removed. Any
servicing should be carried out by qualified service personnel.
Symbol Reference
Caution:
This safety symbol is on the back panel of the equipment and warns:-
The user must not make or remove any connections while the unit is powered on.
To avoid electric shock do not remove the cover. Refer servicing to qualified service personnel.
Caution:
This warning symbol indicates that the surface labelled with this symbol may be hot.
Feedback:
Your feedback will be greatly appreciated, please go to www.linkam.co.uk to fill in the Feedback form.

6
Introduction
Thank you for purchasing the CCR1000 High Temperature Catalyst Cell Reactor. Please take the time to
read through the manual as it will help you to make the most out of the equipment.
The Catalytic Cell Reactor system consists of a removable ceramic sample holder which is heated by a
resistance coil. Samples are placed on a highly porous ceramic cloth filter. Gas is introduced via a high
pressure valve and is then heated by sample holder before passing through the sample. A high pressure
outlet valve can be connected to various gas analysis equipment. All materials used in the CCR1000 stage
have been carefully selected to be as un-reactive as possible.
Either quartz windows for standard brightfield microscopy, fluorescence and Raman or IR grade windows
such as zinc selenide and Barium Fluoride for IR work (pressure range dependent on type of window
used).
Stage Anatomy

7
Mounting Stage to Microscope
with Dovetail Substage
The CCR1000 is designed to work with an up-
right microscope using reflected light only.
The following description is for mounting the
stage on to microscopes which have a circular
dovetail substage assembly.
Attach the curved stage clamps (part no. 9548) to
the base of the stage using the supplied hex
screws and the outer most holes in the base plate.
Adjust the two positioning screws (1) and the
thumb screw (2) so that approximately 5mm of
thread is exposed on the inside edge of the clamp.
This will roughly position the stage in the centre
of the dovetail (3).
Place the stage onto the dovetail then tighten the
thumbscrew (2) to fix the stage in place.
For other types of microscope sub-stages, refer to
the diagram included with the stage adaptor.
Curved Clamps Set 9548
1
3
2

8
Set Up the CCR1000
Please check that all of the following parts have
been supplied with the CCR1000.
1. CCR1000
2. Green Temperature Sensor Cable
3. Power Cable
4. Stage Connection Lead
Electrical Cable Connectors
Plug in the green Temperature Sensor cable to
stage.
Make sure the ’+’ and ’-’ markings on the cable
and connector match and push the cable firmly in
place.
1
2
3
+-
4

9
1
Connection To T95 System Controller
From the stage: connect the green Temperature
Sensor cable to the Stage Socket (1) and connect
the Stage Connection Lead to Stage Connection
Socket (2).
Refer to the T95-LinkPad Manual for more de-
tails.
2

10
Connecting the ECP Water Circulator
Pump
Note: An ECP pump filled with cool water, 15-
18°C, has large enough capacity for upto 2 hours
operation of the stage at 1000°C or over. It is not
recommenced for longer term work at these tem-
peratures.
Connect the Inlet and Outlet tubing from the ECP
to the CCR1000 as shown.
Refer to the ECP, Water Circulator Pump Manual
for more details.
Connect the Gas Lines
The gas connectors are standard size fittings that
require 1/16inch peak or stainless tubing. High
pressure peak ferrule can also be use to seal into
the stage body.
Unscrew the hexagonal stainless steel gas con-
nectors by hand. Insert your gas line into the
connector so that a couple of millimetres extend
beyond the end of the connector.
Relocate the gas line and connector into the stage
body. No force is necessary. Now screw in the
connector until it stops, using only fingers. No
spanner is necessary (unless using stainless steel
tubing).
Note: The CCR1000 is designed to flow reactive
gases over the sample. Make sure the GAS IN
and GAS OUT lines are connected correctly as
shown by the arrows. Use a flow rate of less than
50cc/min.
Pressure Warning
The CCR1000 has been tested to 5 bar pressure
using 22mm quartz windows of 1mm thickness.
Windows must always be inspected with magni-
fying lens to check there are no microscopic
cracks or scratches before using the stage under
pressure. Never stand within 1m of CCR100
when using high pressure between 2-5bar.
Linkam cannot guarantee pressure with IR trans-
parent windows due to the inconsistent mechani-
cal strength of the windows.
Contact Linkam if there is any concern with pres-
surizing this stage.
Inlet Outlet
Gas In
Gas Out
Gas Flow

11
Load A sample
Remove Sample Holder
Before removing the sample holder please ensure
that the heater assembly has cooled to room tem-
perature. When using the Loading Tool, care
must be taken as the heater assembly is very
fragile.
Remove lid by unscrewing anti clockwise.
Remove the 22x1mm quartz window.
Use the Sample Holder Removal Tool (1) as
shown in the picture.
Carefully lower the Sample Holder Removal Tool
over the Sample Holder (2).
The next step requires great care and minimal
force. Once the tool is axially aligned with the
sample holder it will need to be pressed over the
outer diameter of the Sample Holder. Rotate the
tool slightly to make this easier. The tool will
come to a stop after approximately 1.5mm. No
further force is required otherwise the user risks
damaging the heater assembly. Gently pinch the
tool with a thumb and fore finger. This will allow
the tool to grip the outer diameter of the sample
holder.
Lift the tool vertically away from the CCR1000.
If the sample holder is lifted out at an angle it
could break.
1
2
Lift Vertically

12
Load Sample Filter
The sample filters come as a sheet of alumina /
silica (Al2O3 96%/SiO2 4%) Non-Woven Fabric.
A small disc of this fabric is needed to place the
sample on. The following procedure must be
used to load the filter into the Sample Holder.
Warning: The above mater ial is harmful by
inhalation and when in contact with skin. Possi-
ble risk of irreversible effects. Wear suitable
protective clothing. Wear suitable gloves, eye/
face protection or work in a fume cupboard. This
material is NON-CARCINOGENIC.
Important Note Before Heating Sample: The
Alumina/Silica Fabric filter on which the sample
is loaded should be heated up to 600ºC before
doing a sample run. Either heat the fabric in an
autoclave or using the CCR1000. Remove the lid
window and run gas through the stage during the
heating phase. This is so that any dust or debris
in the stage or fabric filter is burned off and car-
ried away before start of experiment.
Turn the Sample Holder upside down and with a
forefinger and thumb gently rest it over the alu-
mina/silica fabric (1). Once the sample holder is
in position, apply a very light force and rotate the
sample holder into the alumina/silica Non-Woven
Fabric. This will cut the fabric to fit the sample
holder.
Gently lift the sample holder away from the fab-
ric. The filter will now be the perfect size for the
sample holder.
The filter is not yet low enough in the sample
holder and needs to be pressed into position. This
can be achieved by the using the Filter Load/
Removal Tool (2).
The filter should be in the sample holder and
ready to be pressed into position as shown above.
Make sure that the tool is round the correct way to
press the filter into the sample holder.
Note: To remove the filter, the tool can be used to
push it out of the sample holder. Balance the tool
on a flat surface so that the smaller diameter of
the tool is protruding upwards. Hold the sample
holder over the tool (the Filter Load/Removal
Tool can be supported by hand if required). Gen-
tly lower the sample holder over the filter load/
removal tool.
2
1

13
Load Sample into Sample Holder
Place the Sample Loading Base (1) on a flat sur-
face and hold the Sample Holder (2) above it.
Gently press and rotate the Sample Holder into
the central hole in the sample loading base until
resistance is felt. Excessive forces are not needed
as the sample holder should slide into the sample
loading base.
Place the Sample Loading Funnel (3) on top of
the sample holder and the sample loading base as
shown below.
The sample can now be easily guided through the
top of the funnel into the sample holder.
123

14
Load Sample Holder into CCR1000
Carefully pick up the top of the Sample Holder
and hold it over the heater assembly.
Very carefully lower the Sample Holder into the
heater assembly. Rotate the sample holder to
make sure that it is axially aligned with the heater
assembly.
Once the sample holder is positioned in the heater
assembly place a fore finger on top of the sample
holder. Gently press down and rotate the sample
holder so that it sits firmly in place.
Replace the quartz window.
Replace the Lid.

15
Appendix
Spares and Accessories
Here is a list of spares you may require in the future. Contact your Linkam representative for other spare
parts that are not listed below.
Part No. Part Name Part Description
9848 CCR1000 KIT Replacement Spares Kit
CCR-SLK Sample Loading Kit
CCR-CC Ceramic Cloth for Sample Loading (6x3.5cm) x4
CCR-CPF Cole Palmer Fitting with Ferrule x4
W22Q1 22mm Diameter Quartz Window, 1mm thick x2
CCR-ALSH Alumina Sample Holder
RING O Ring ID18.0 x CS1.5 Viton x2
WTK Water Tube Kit: 3x WVC Hose Valve, 3x Clear PVC 3x6mm Tubing
CCR-SP Micro Spatula
Part No. Part Name Part Description
9754 CCR-BCeramic Heating Element including S-Type Thermocouple

16
Linkam Scientific Instruments Ltd
Tel: [phone]
Fax: [phone]
Email: [e-mail]
Unit 8 Epsom Downs Metro Centre
Waterfield, Tadworth, Surrey, KT20 5LR, UK
www.linkam.co.uk
Version: 1.05.29.10