Anton Paar HTK 1200N User manual

Measure
what is measurable
and make measurable
that which is not.
Galileo Galilei (1564-1642)
Reference Guide
HTK 1200N
High-Temperature Oven-Chamber with
CCU 1000 Control Unit

Reference Guide
HTK 1200N
High-Temperature Oven-Chamber with
CCU 1000 Control Unit
Disclaimer
This document may contain errors and omissions. If you discover any such errors or if you would like to see
more information in this document, please contact us at our address below. Anton Paar assumes no liability
for any errors or omissions in this document.
Changes, copyright, trademarks etc.
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process) without prior written permission by Anton Paar GmbH.
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as such. They are the property of their respective owner.
Further information
Published and printed by Anton Paar GmbH, Austria
Copyright © 2018 Anton Paar GmbH, Graz, Austria
Address of the instrument producer: Anton Paar GmbH
Anton-Paar-Str. 20
A-8054 Graz / Austria – Europe
Tel: [phone]
Fax: [phone]
E-Mail: [email protected]
Web: www.anton-paar.com
Date: July 2018
Document number: B40IB006EN-D

Contents
4B40IB006EN-D
Contents
1 Safety Instructions.................................................................................................................................. 7
1.1 General safety instructions ............................................................................................................... 7
1.2 Radiation Safety................................................................................................................................ 8
1.3 Conventions for safety messages..................................................................................................... 8
1.4 Safety Signs on the Instrument......................................................................................................... 9
2 Overview................................................................................................................................................ 10
2.1 Description of the Instrument.......................................................................................................... 10
2.2 Design of the Instrument................................................................................................................. 10
2.2.1 Housing with Safety Switch Box.............................................................................................10
2.2.2 Lid........................................................................................................................................... 11
2.2.3 Sample Holder Flanges.......................................................................................................... 12
2.3 Connector Box................................................................................................................................ 13
2.4 CCU 1000 Combined Control Unit..................................................................................................13
2.4.1 CCU 1000 Front Panel ........................................................................................................... 14
2.4.2 CCU 1000 Rear Panel............................................................................................................ 14
2.4.3 Overheat Protection................................................................................................................ 14
3 Checking the Supplied Parts ............................................................................................................... 15
4 Installation............................................................................................................................................. 17
4.1 Installation Requirements ............................................................................................................... 17
4.1.1 Electrical Power and Computer Interface ............................................................................... 17
4.1.2 Cooling Water Requirements.................................................................................................. 17
4.2 Mounting the Adapter on HTK 1200N.............................................................................................17
4.3 Mounting HTK 1200N on the Goniometer....................................................................................... 18
4.4 Installing CCU 1000........................................................................................................................ 18
4.4.1 Power Supply for the Heater................................................................................................... 19
4.4.2 Thermocouple of Stationary Sample Holder and Sample Spinner ......................................... 19
4.4.3 Connection of Sample Spinner Motor..................................................................................... 20
4.4.4 Connection for Safety Circuit.................................................................................................. 20
4.5 Connecting CCU 1000 with a Computer......................................................................................... 20
4.6 Installing the Cooling Water Circuit................................................................................................. 21
4.7 Installing the Gas Supply................................................................................................................ 21
4.8 Installing the Vacuum Equipment ................................................................................................... 21
5 Putting HTK 1200N into Operation...................................................................................................... 23
5.1 Alignment of the Sample Holder..................................................................................................... 23
5.2 Height adjustment with Rigid Adapter............................................................................................. 23
5.3 Height Adjustment with Motorized Alignment Stage....................................................................... 24
5.4 Adjustment of Chamber Rotation.................................................................................................... 24
5.5 Alignment procedure....................................................................................................................... 24
5.6 Checking the Instrument Condition................................................................................................. 25
5.7 Turning on the Instrument............................................................................................................... 26
6 Operating CCU 1000 ............................................................................................................................. 27
6.1 Front Panel of the Instrument ......................................................................................................... 27
6.2 Keypad............................................................................................................................................ 27
6.2.1 Status LEDs............................................................................................................................ 28
6.3 Display............................................................................................................................................ 28
6.3.1 Navigation Diagram of CCU 1000 .......................................................................................... 29
6.4 Turning the Heater On and Off ....................................................................................................... 30
6.5 Manual Control of CCU 1000.......................................................................................................... 30
6.6 Remote Control of CCU 1000......................................................................................................... 30
7 Handling the Sample Holder and Sample........................................................................................... 31
7.1 Mounting/Demounting the Sample Holder Flange.......................................................................... 31
7.1.1 Exchanging the sample holder body....................................................................................... 32
7.1.2 Matching Sample Holder Height to Sample Thickness........................................................... 33

Contents
B40IB006EN-D 5
7.2 Applying a Sample.......................................................................................................................... 34
7.2.1 Powder Samples..................................................................................................................... 34
7.2.2 Solid Samples......................................................................................................................... 35
7.3 Temperature Validation................................................................................................................... 35
8 Operation............................................................................................................................................... 36
8.1 Before Turning on Power................................................................................................................ 36
8.2 Operation under Air Atmosphere.................................................................................................... 36
8.2.1 Operation at Room Temperature............................................................................................ 36
8.2.2 Operation as Heating Chamber.............................................................................................. 36
8.3 Operation under Vacuum................................................................................................................ 37
8.4 Operation using Various Gases (except air)...................................................................................38
9 Putting HTK 1200N out of Operation................................................................................................... 39
10 Troubleshooting.................................................................................................................................. 40
10.1 Error Messages............................................................................................................................. 40
10.2 General Messages on Display...................................................................................................... 40
10.3 Error Analysis................................................................................................................................ 40
10.4 Technical Support......................................................................................................................... 42
11 Maintenance ........................................................................................................................................ 43
11.1 Routine Maintenance.................................................................................................................... 43
11.2 Check the Functioning of the Flow Controller............................................................................... 43
11.3 Exchanging of Parts...................................................................................................................... 43
11.3.1 Switching off the Instrument ................................................................................................. 43
11.3.2 Replacing the Window Foil................................................................................................... 43
11.3.3 Replacing the Thermocouple................................................................................................45
11.3.4 Replacing the O-rings........................................................................................................... 45
11.4 Checking and Replacing Main Fuses ...........................................................................................45
Appendix A: Technical Data ................................................................................................................... 46
Appendix B: Cooling water..................................................................................................................... 49
Appendix C: Thermal Expansion of the Sample Holder....................................................................... 51
Appendix D: Warranty ............................................................................................................................. 52
Appendix E: Accessories........................................................................................................................ 53
Appendix F: Swagelok tube fittings....................................................................................................... 54
Appendix F.1: Installation instructions .................................................................................................. 54
Appendix F.2: Retightening instructions ............................................................................................... 55
Appendix G: Declaration of Conformity ................................................................................................ 56

Contents
6B40IB006EN-D

1 Safety Instructions
B40IB006EN-D 7
1 Safety Instructions
• Read the documentation before using
HTK 1200N.
• Follow all hints and instructions contained in the
documentation to ensure the correct use and
safe functioning of HTK 1200N.
• The documentation is a part of the product.
Keep this document for the complete working
life of the product and make sure it is easily
accessible to all people involved with the prod-
uct. If you receive any additions or revisions to
the documentation from Anton Paar GmbH,
these must be treated as part of the documenta-
tion.
1.1 General safety instructions
Liability
• The documentation does not claim to address
all safety issues associated with the use of the
instrument and samples. It is your responsibility
to establish health and safety practices and
determine the applicability of regulatory limita-
tions.
• Operate HTK 1200N with CCU 1000
Combined Control Unit from Anton Paar GmbH
only.
• Anton Paar GmbH only warrants the proper
functioning of HTK 1200N if no adjustments
have been made to the mechanics, electronics,
and firmware.
• Only use HTK 1200N for the purpose described
in the documentation. Anton Paar GmbH is not
liable for damages caused by incorrect use of
HTK 1200N.
Installation and Use
• HTK 1200N is not an explosion-proof instru-
ment and therefore must not be operated in
areas with risk of explosion.
• HTK 1200N must not be used with hazardous
(e.g. explosive or poisonous) gases.
• The installation procedure should only be car-
ried out by authorized personnel who are famil-
iar with the installation instructions.
• It is the responsibility of the customer to provide
all the set-up (tubings, valves,..) necessary for
proper work with HTK 1200N.
• Do not use any accessories or wearing parts
other than those supplied or approved by Anton
Paar GmbH.
• Make sure all operators are trained to use the
instrument safely and correctly before starting
any applicable operations.
• In case of damage or malfunction, do not con-
tinue operating HTK 1200N. Do not operate the
instrument under conditions which could result
in damage to goods and/or injuries and loss of
life.
• Check HTK 1200N, especially the sample
holder, for chemical resistance to the samples
and cleaning agents.
• The results delivered by HTK 1200N not only
depend on the correct function of the instru-
ment, but also on various other factors. We
therefore recommend to have the results
checked (e.g. plausibility tested) by skilled per-
sonnel before consequential actions are taken
based on the results.
Maintenance and Service
• Service and repair procedures may only be car-
ried out by authorized personnel or by Anton
Paar GmbH.
Disposal
• Concerning the disposal of HTK 1200N,
observe the legal requirements in your country.
Returns
• For repairs send the cleaned HTK 1200N
(instrument) to your Anton Paar representative.
Only return the instrument together with the
filled out RMA (Return Material Authorization)
and the form "Safety Declaration for Instrument
Repairs". Please download the Safety Declara-
tion form from our website www.anton-
paar.com.
• Do not return instruments which are contami-
nated by radioactive materials, infectious agents
or other harmful substances that cause health
hazards.
Precautions for highly inflammable samples
and cleaning agents
• Observe and adhere to your national safety reg-
ulations for handling the measured samples

1 Safety Instructions
8B40IB006EN-D
(e.g. use of safety goggles, gloves, respiratory
protection etc.).
• Only store the minimum required amount of
sample, cleaning agents and other inflammable
materials near HTK 1200N.
• Do not spill sample/cleaning agents or leave
their containers uncovered. Immediately remove
spilled sample/cleaning agents.
• Make sure that the setup location is sufficiently
ventilated.The environment of HTK 1200N must
be kept free of inflammable gases and vapors.
• Supply a fire extinction unit.
• Ensure sufficient supervision of HTK 1200N
during operation.
1.2 Radiation Safety
• The HTK 1200N High-Temperature Oven-
Chamber represents an open system and is
allowed to be operated only on diffractometers
equipped with a radiation enclosure.
• Before starting the experiment, the user has to
make sure that the radiation hazard equipment
corresponds to the local requirements.
1.3 Conventions for safety messages
The following conventions for safety messages are
used in this document:
TIP: Tip gives extra information about the situation
at hand.
DANGER
Description of risk.
Danger indicates a hazardous situation which, if
not avoided, will result in death or serious injury.
WARNING
Description of risk.
Warning indicates a hazardous situation which, if
not avoided, could result in death or serious
injury.
CAUTION
Description of risk.
Caution indicates a hazardous situation which, if
not avoided, could result in minor or moderate
injury.
NOTICE
Description of risk.
Notice indicates a situation which, if not avoided,
could result in damage to property.
CAUTION
Hot surface
This symbol calls attention to the fact that the
respective surface can get very hot. Do not
touch this surface without adequate protective
measures.
CAUTION
High voltage
This symbol calls attention to the risk of high
voltage. Do not proceed until the indicated con-
ditions for averting this threat are fully under-
stood and met.
CAUTION
X-ray Radiation
This symbol calls attention to the risk of radia-
tion. Do not proceed until the indicated condi-
tions for averting this threat are fully understood
and met.
Wear protective gloves
Wear protective gloves when handling
the HTK 1200N.
Wear safety goggles
Wear safety goggles when handling
the HTK 1200N.

1 Safety Instructions
B40IB006EN-D 9
1.4 Safety Signs on the Instrument
1 CAUTION - Hot surface
Fig. 1: Position of warning signs on the sample holder
flange
1CAUTION
Fig. 2: Safety sign on Instrument
CAUTION
Hot surface
This symbol calls attention to the fact that the
respective surface can get very hot. Do not
touch this surface without adequate protective
measures.
1
CAUTION
This symbol calls attention to the fact that the
instrument must be connected to protective
ground. Service has to be done by qualified per-
sonal only. Always disconnect power cord before
serving.
Wear protective gloves
Wear protective gloves when handling
the HTK 1200N.
Wear safety goggles
Wear safety goggles when handling
the HTK 1200N.
NOTICE
Take care that the warning symbols remain
clearly legible.
1

2 Overview
10 B40IB006EN-D
2Overview
2.1 Description of the Instrument
TheHTK 1200NHigh-TemperatureOven-Chamber
is designed for non-ambient X-ray studies from
room temperature to 1200 °C in different atmo-
spheres.
TheHTK 1200NHigh-TemperatureOven-Chamber
can be easily adapted to most available goniome-
ters.
Due to its environmental heating the temperature
gradientin the sample islowandsamplesof several
mm thickness can be investigated.
The possibility of sample spinning preserves good
statistics of grain orientation distribution even if re-
crystallisation results in large-sized grains. This is
necessary for obtaining reliable diffraction informa-
tion and for subsequent data evaluation like Riet-
veld analysis.
The sample carriers can be easily exchanged and
can accommodate various flat sample forms such
as powders or bulk samples.
Thin films (on thick substrates) can also be studied
with reliably measured surface temperature due to
the environmental heating.
Sample carriers made of alumina provide high
chemical resistance.
In addition to the sample holders for flat powder
samples, a HTK 1200N Capillary Extension is avail-
able. With this extension, the HTK 1200N can be
converted into a capillary heater up to 1000 °C.
To ensure reliable operation of the HTK 1200N
High-Temperature Oven-Chamber, the instrument
must be operated with:
• 135004 CCU 1000 Combined Control Unit
• 164877 Flow controller
TIP: Please refer to Appendix Efor detailed informa-
tion
2.2 Design of the Instrument
The HTK 1200N is a heating stage for powder XRD
with a temperature range from 25 to 1200 °C.
Basically, the HTK 1200N consists of:
1. Housing with safety switch box
2. Lid
3. Sample holder flange with sample holder (sta-
tionary or spinning)
TIP: For detailed information on the materials used
in the HTK 1200N, please refer to Appendix A.
2.2.1 Housing with Safety Switch Box
Fig. 3: Main components of the sample chamber
1 X-ray window
2 Window clamp
3 Height alignment screw
4 Sample holder guiding rods
5 Sample holder flange
6 Base plate
7 Safety switch box
8 Boreholes for adapter
9 Flange fixing screws
All components of the HTK 1200N housing are
made of nickel-plated brass. Both the base plate
and the housing are water-cooled.
The sample holder is inserted through the opening
at the bottom. Two guiding rods provide for exact
centering of the sample holder flange.
At the rear of the instrument is a small safety switch
box that contains two safety switches:
• a bi-metallic thermo-switch that shuts off the
1
2
3
8
6
5
7
94

2 Overview
B40IB006EN-D 11
heater, if the housing temperature reaches
70 °C and
• a contact switch that detects whether the sam-
ple holder flange is mounted and which shuts off
the heater, if it is not.
The adapter, which is used to mount the
HTK 1200N on the goniometer is fixed to the hous-
ing’s base plate. Vertical alignment of the
HTK 1200N versus the goniometer axis is done by
using the height alignment screw or the alignment
stage.
Depending on the type of goniometer used, evacu-
ation can be performed through the adapter or
through the vacuum flange on the lid.
Along the radiation path (entrance and exit of X-
rays), the housing is slotted. The window foil is
pressed against an O-ring by means of two clamps
and covers the window openings. The window foil is
either an aluminium-coated Kapton foil of 125 µm
thickness (for work up to 1000 °C) or a combination
of a graphite foil and a non-coated Kapton foil of
125 µm thickness (for work above 1000 °C).
TIP: The graphite foil and non-coated Kapton foil
are mounted upon delivery.
The oven consists of an electrical heater surround-
ingthe sampleholderand thermalinsulationaround
the heater.
The electrical heater is formed in a special way to
uniformly heat the sample, which is located in the
centerof the heater.Theheating filamentis made of
Kanthal.
The thermal insulation consists of foamed alumina
and provides a very uniform temperature distribu-
tion inside the oven.
TIP: The foamed aluminashell is very porous with a
large internal surface. Even when operated with a
vacuum pump, small amounts of adsorbed gas, in
particular oxygen, are continuously released from
the alumina. If the sample material is very sensitive
to oxygen, this can lead to undesired sample oxida-
tion at elevated temperature.
2.2.2 Lid
Fig. 4: Chamber Lid
1 Current cables for the electrical heater
2 Cooling water inlet
3 Cooling water outlet
4 Gas supply
5 Vacuum flange (DN16KF)
6 Tap holes for HTK 1200N Capillary Extension guiding
rods (optional)
The lid is made of nickel-plated brass and is water-
cooled. It is screwed to the housing and sealed with
an O-ring.
Thelidcontains connectorsforthewatersupply, the
gas supply and the vacuum. The power supply for
the electrical heater is provided by two cables which
have to be connected to the CCU 1000.
Thelid has two tapholesinto whichguidingrods are
screwed when the HTK 1200N is used with the Cap-
illary Extension (optional).
TIP: For more information about the connectors, re-
fer to chapter 4.
For more information about the HTK 1200N Capil-
lary Extension, refer to Appendix Eand to the
HTK 1200N Capillary Extension Instruction Manual.
NOTICE
Risk of damage
At the surface of the Kanthal heater an oxide
layer is formed which protects the wire.
After work in vacuum or inert gas, it is recom-
mended to regularly regenerate this oxide layer
by heating the HTK 1200N up to 1000 °C in air.
This will extend the life time of the heater consid-
erably.
6
3
4
2
1
5

2 Overview
12 B40IB006EN-D
2.2.3 Sample Holder Flanges
Two different types of sample holder flanges are
available for the HTK 1200N:
Stationary sample holder
Fig. 5: Stationary sample holder
1 Sample carrier
2 Fixing ring for sample carrier
3 Sample holder body
4 Thermocouple
5 Temperature shielding with fixing clamp
6 Flange
7 Flange fixing screws (4 pcs)
8 Fixing nut
9 Cable connection between thermocouple and
CCU 1000
Sample spinner
Fig. 6: Sample spinner
1 Sample carrier
2 Fixing ring for sample carrier
3 Sample holder body
4 Thermocouple
5 Temperature shielding with fixing clamp
6 Flange
7 Motor
8 Electronic motor control
9 Flange fixing screws (4 pcs)
10 Cable connection between thermocouple and
CCU 1000
The sample holder assembly consists of the flange
and the actual sample holder, which is fixed to the
flange by a fixing nut.
TIP: The sample spinner is actually not rotating but
oscillating - still providing a good statistics of grain
orientation in the sample.
The sample holder comprises the sample carrier, a
fixing ring and the sample holder body. All these
parts are made of ceramics.
42
3
5
7
6
1
8
9
5
3
1
2
4
6
7
9
10 8

2 Overview
B40IB006EN-D 13
Fig. 7: Sample holder
1 Sample carrier
2 Fixing ring for sample carrier
3 Sample holder body
4 Thermocouple
5 Temperature shielding with fixing clamp
• The sample carrier is fixed to the top of the sam-
ple holder body by a fixing ring. Three different
versions of the sample carrier with different
depth are available: 0.8 mm deep, 0.4 mm deep
and a flat one. Depending on the sample to be
investigated sample carriers made of other
materials are available on request.
• The fixing ring is flexible and is put over the
edge of the sample carrier, allowing quick and
easy exchange of the prepared sample.
• The sample holder body contains a Pt10Rh-
Pt (type S) thermocouple which is used for sam-
ple temperature measurement and control. It is
located right underneath the sample position,
thus providing good correspondence between
the set temperature and the actual sample tem-
perature.
The thermocouple is connected to the connector
box by the cable for sample holder flange (see
also chapter 4.4.2).
The temperature shielding closes the opening of
the alumina insulation and provides a uniform
temperature distribution.
TIP: Please refer to chapter 7 for further informa-
tion.
The sample holder is inserted into the HTK 1200N
chamber with two guide pins and fastened by four
screws.
2.3 Connector Box
The connector box terminates the supply hose of
theHTK 1200N,whichcontainsthecontrolwiresfor
the temperature sensor, flange control and the sam-
ple spinner.
Fig. 8: Connector box
1 Connector cable to the CCU 1000
2 Connector for flange control
3 Connector for thermocouple
4 Connector for sample spinner
2.4 CCU 1000 Combined Control Unit
CCU 1000 is designed to control the sample holder
temperature in HTK 1200N and to guarantee safe
operation of the entire instrument. In order to reach
and maintain the desired sample holder tempera-
ture, CCU 1000 controls the heater inside the sam-
ple chamber.
CCU 1000 can be operated manually by means of
the push - buttons on the front panel, or it can be re-
mote-controlled via a serial RS 232 interface.
NOTICE
Risk of damage
Make sure that the contact surfaces between
sample carrier and top of the sample holder
body are free of dust and sample residues to
provide for a good thermal contact!
1
2
3
5
4
1 2 3 4

2 Overview
14 B40IB006EN-D
2.4.1 CCU 1000 Front Panel
The front panel of CCU 1000 contains all control
buttons, status LEDs and the display.
Fig. 9: CCU 1000 front panel with control elements
1 Mains switch
2 Display and keypad
Allelementsof thefront panelaredescribedindetail
in chapter 6.2.
2.4.2 CCU 1000 Rear Panel
The rear panel of CCU 1000 contains all the con-
nectors of the instrument.
Fig. 10: CCU 1000 rear panel
1 Power connector
2 Connector Heater
3 RS 232 connector
4 LAN connector (currently not used)
5 Connector Flow Sensor
6 Connector OUT1/2 (optional connectors)
7 Connector Sensors/Heater
8 High power module for HTK 1200N
2.4.3 Overheat Protection
HTK 1200N has two devices to prevent overheating
of the instrument. The flow control unit of
HTK 1200N monitors the flow of cooling water
through the housing of the sample chamber. It is a
water flow dependent switch, which is connected to
CCU 1000. If there is not enough water flow,
CCU 1000 switches to Standby mode (heater off),
the Error LED on the front panel starts to flash and
shows an alarm message (E03).
In addition, a thermoswitch is mounted in the safe-
ty switch box for flange control (Fig. 3 (7)) to protect
the device from being overheated in case of a mal-
function. The thermoswitch interrupts the heating
power circuit if the temperature of the chamber
housing exceeds 70 °C. CCU 1000 automatically
switches to Standby mode (heater off) and shows
an alarm (E04).
TIP: A list of all error messages can be found in
chapter 10.1.
12
1 2 3 4 5 6 7 8
CAUTION
Hot surface
When the cooling water supply to the chamber
fails, the housing can have a hot surface.
Carefully check the temperature of the
HTK 1200N housing and make sure the housing
is at room temperature before you touch it.
Make sure that you have found and removed the
cause of the error before you continue operation
of HTK 1200N and CCU 1000.

3 Checking the Supplied Parts
B40IB006EN-D 15
3 Checking the Supplied Parts
HTK 1200NHigh-TemperatureOven-Chamberwas
tested and packed carefully before shipment. How-
ever, damage may occur during transport.
1. Keep the packaging material (box, foam piece,
transport protection) for possible returns or
questions from the transport and insurance
company.
2. Check the delivery for completeness by compar-
ing the supplied parts to those noted in the table
below.
3. If a part is missing, contact the local representa-
tive of your diffractometer manufacturer or
Anton Paar GmbH in Graz, Austria.
4. If a part is damaged, contact the transport com-
pany and either the local representative of your
diffractometer manufacturer or Anton Paar
GmbH in Graz, Austria.
Table 3-1: Supplied Parts
Pcs. Item Cat.No.
1HTK 1200N with stationary sample holder including:
Heating chamber
Stationary sample holder
Sample carrier, 0.8 mm deep (2x)
Fixing ring for sample carrier
Cable for sample holder flange
16407
or
1HTK 1200N with sample spinner including:
Heating chamber
Sample Spinner
Sample carrier, 0.8 mm deep (2x)
Fixing ring for sample carrier
Cable for sample holder flange
16408
1
1
1
2
1
1
1
CCU 1000 Combined Control Unit
Mains cables
Heater cable
Mains fuses
RS232 cable to control PC
USB cable
Connector box
135004
1Stand for sample holder flange
1Cooling water hoses
(already mounted)
1Pressure hose and clamps
(customer-specific part)
1Accessory box
(content specified on label)
1Set of tools
1
1
1
Instruction Manual
Software manual Nambicon
USB flash drive with Nambicon

3 Checking the Supplied Parts
16 B40IB006EN-D
TIP: Check the supplied packages delivered with
the HTK 1200N for completion by comparing the
parts to those listed in the appropriate packing lists.
NOTICE
Risk of damage
Always use the original packing material when
shipping the instrument or parts of it. Store the
packing material carefully for later use!

4 Installation
B40IB006EN-D 17
4 Installation
4.1 Installation Requirements
TIP: When HTK 1200N is ordered together with the
required adapter, the adapter is mounted on the
chamber on delivery.
When HTK 1200N is ordered together with a motor-
ized alignment stage, the adapter is mounted on the
alignment stage.
Operation of HTK 1200N/CCU 1000 requires cool-
ing water supply and electrical power. The corre-
sponding requirements can be found below and in
Appendix A and Appendix B.
4.1.1 Electrical Power and Computer Inter-
face
CCU 1000:
• Mains voltage: AC 230 V ± 10 %
• Mains frequency: 50 or 60 Hz.
• Mains connector (1): IEC 60320 C13
• Mains fuses: 2 x T 8 A H 5 x 20 mm (ceramic
tube)
• Remote control interface: RS 232 C
• RS 232 connector on CCU (2): D-Sub DE-9
(male)
• Cable type: null modem
4.1.2 Cooling Water Requirements
• flow rate: 0.7 to 1.5 l/min
• temperature: 15 to 25 °C
• pressure: max. 4 bar
4.2 Mounting the Adapter on
HTK 1200N
An appropriate adapter is necessary to mount the
HTK 1200NHigh-TemperatureOven-Chamberona
goniometer. For detailed ordering information, refer
to Appendix E.
1 Alignment equipment
2 Allen screw (4 pcs)
3 Adapter (version depends on the goniometer used)
4 HTK 1200N base plate
To mount the adapter, proceed as follows:
1. Remove the alignment equipment (1) from the
rear of the HTK 1200N base plate (4).
2. If required, clean the O-ring at the adapter
flange and lightly coat the O-ring with vacuum
grease.
3. Use the four Allen screws (2) to mount the
adapter to the HTK 1200N base plate (4).
CAUTION
X-ray radiation
The HTK 1200N High-Temperature Oven-Cham-
ber represents an open system. It is only permit-
ted to install the HTK 1200N on diffractometers
equipped with a radiation enclosure.
NOTICE
Risk of damage
Do NOT touch the X-ray window during instal-
lation. When you touch the window, the graphite
foil underneath the Kapton foil will tear.
1
2
3
4

4 Installation
18 B40IB006EN-D
4. Fasten the lower part of the alignment equip-
ment (1) to the adapter using the two screws.
5. Fasten the two upper parts of the alignment
equipment (1) to the HTK 1200N base plate
using the two screws in the front of the upper
part. Make sure that the large screw on the top
of the alignment equipment (1) is surrounded by
the two halves of the upper part.
4.3 Mounting HTK 1200N on the Goni-
ometer
The HTK 1200N High-Temperature Oven-Chamber
(with adapter) is mountedon the goniometer instead
of the standard (ambient) sample holder.
TIP: Make sure that the X-ray beam is properly
aligned before you remove the standard sample
holder (see the Diffractometer Instruction Manual
for detailed information). Good beam alignment is
important, because HTK 1200N is aligned relative
to the X-ray beam.
Make sure that the chamber is mounted centrically
on the goniometer.
Take care that the sample holder is as parallel as
possible to the
 -zero line of the goniometer.
Instructions for mounting the chamber are given in
the instruction manual for your diffractometer
.
4.4 Installing CCU 1000
CCU 1000 Combined Control Unit is prepared for
rack mounting in a 19" 4HE slot.
Mount CCU 1000 either in a suitable slot in the dif-
fractometer or in a rack next to the diffractometer.
Make sure there is enough space (at least 10 cm)
behindthe CCU 1000 for all connectorsandthatthe
slot is sufficiently ventilated to avoid heat accumula-
tion behind the CCU 1000.
The connector for temperature measurement,
flange control and sample spinnerare located in the
connection box described in chapter 2.3.
Theinstrumentisdeliveredtogetherwiththe current
cables for the HTK 1200N heater and the connec-
tion cable for the HTK 1200N temperature sensor.
Connect the electrical cable to the CCU 1000 rear
panel as follows:
• Plug the fix mounted cable on the connector box
to the connector on the rear panel of the
CCU 1000 (see Fig. 10 (7)).
• Make sure the mains switch on CCU 1000 is
OFF and connect the mains power cable to the
POWER connector (see Fig. 10 (1)).
Connect the electrical cable to the sample chamber
as described in the following chapters.
WARNING
Make sure that the system "chamber/alignment
stage/goniometer" is properly earthed. Check
with an ohmmeter if necessary: a low measuring
value means sufficient earthing.
NOTICE
Risk of damage
• When using an adapter with alignment stage:
Detailed mounting instructions are supplied
with the alignment stage.
• A corresponding earthing connector is sup-
plied with the alignment stage.
WARNING
Make sure that the HTK 1200N chamber and (if
applicable) the alignment stage are properly
connected to protective earthing. Refer to the
instruction manual for your diffractometer for
information about suitable terminals for protec-
tive earthing.
CAUTION
Risk of damage
Always make sure that CCU 1000 is turned off
before you connect or disconnect cables on the
sample chamber or the CCU 1000.

4 Installation
B40IB006EN-D 19
4.4.1 Power Supply for the Heater
Power for the heater of the HTK 1200N is supplied
with two high current cables. Plug the cable for the
heater to the heater connector on the rear side of
the CCU 1000 (Fig. 10 (2)). Connect these cables
with the two high current cables at the lid of the
HTK 1200N as described below:
Connecting procedure:
Disconnecting procedure:
4.4.2 Thermocouple of Stationary Sample
Holder and Sample Spinner
For correct installation please follow this instruction:
Stick the plug-in connection (1) of the cable for sam-
ple holder flange into the locknut (2) of the sample
holder at the bottom of the sample holder flange.
Then connect the other end of the cable to the con-
nector "Temperature Sensor" on the connector box
(Fig. 8 (3).
WARNING
Risk of injury
This instrument must be connected to protective
ground.
CAUTION
Risk of damage
Switch off the CCU 1000 and disconnect the
cable for the mains supply, before disconnecting
and connecting the high current cables and the
thermocouple cable.
Connected
Disconnected
12

4 Installation
20 B40IB006EN-D
Whenoperatingthe sample holder flange bewareof
the shape of the thermocouple cable.
Do NOT tear at the cable and prevent a complete
straightening of the cable.
For safe operation with sample spinner preserve a
minimum of four windings (3).
Before demounting the sample holder flange and
changing the sample holder disconnect the cable
from the sample holder at the bottom of the sample
holder flange (4).
4.4.3 Connection of Sample Spinner Motor
The motor of the sample spinner has to be connect-
ed to the connector "Sample Spinner" on the con-
nector box (Fig. 8 (4)).
4.4.4 Connection for Safety Circuit
At the rear of the HTK 1200N is a small safety
switch box for flange control and overheating pro-
tection.Connectthe extensioncablefromthesafety
switch box on the back of the HTK 1200N to the
connector "Flange Control" on the connector box
(Fig. 8 (2)).
4.5 Connecting CCU 1000 with a Com-
puter
The RS 232 serial port at the rear panel of
CCU 1000allows you to connect theCCU 1000toa
computer for remote control (see Fig. 10 (3)).
A null modem RS 232 cable is required to connect
the CCU 1000 to a PC.
PIN assignment:
Fig. 11: RS 232 pins
4
3
Pin
2RX
3TX
5GND
Others not connected
NOTICE
According to EN60950 standards, the RS 232
serial interface represents a SELV circuit which
must therefore only be connected to SELV cir-
cuits.
1