ThermoFisher Scientific Thermo Scientific ARL EQUINOX 100 Operation and maintenance manual

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Thermo Scientific ARL EQUINOX 100
X-Ray Diffractometer
Instruction Notice
AA83838 - C • March 2019

Chapter | Revision Table
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PN AA83838 | Revision C | 11-Mar-2019
ARL EQUINOX 100
Page 2
1 Revision Table
Revision
Date
ECO number
Description of Changes
A
04-JUN-2018
SDR14163
Initial Release
B
21-JUN-2018
SDR15489
Minor update done.
C
11-MAR-2019
SDR17946
SDR18055
Appendix 5 - Gandolphi sample holder removed.
Co X-Ray limit changed from 0.2 mA to 0.3 mA.
Note This document is original manual.
The information in this document is subject to change without notice.
We assume no responsibility for any errors that may appear in this document.

Contents
1Revision Table...................................................................................................2
2Introduction.......................................................................................................5
3Safety.................................................................................................................6
3.1 General Safety Guidelines...................................................................................6
3.2 Hazard Statements and Symbols.........................................................................7
3.3 Symbols on the Instrument ..................................................................................7
3.4 Emergency Stop..................................................................................................8
3.5 Electricity.............................................................................................................8
3.6 High Voltage Generator.......................................................................................8
3.7 Protection Enclosure and X-Ray Tubeshield........................................................9
3.8 Security Beacons.................................................................................................9
3.9 Gas....................................................................................................................10
4General Information........................................................................................11
4.1 ARL EQUINOX 100 Front View .........................................................................11
4.2 ARL EQUINOX 100 Rear View..........................................................................12
4.3 ARL EQUINOX 100 Inside View ........................................................................13
4.4 Front Panel Information .....................................................................................14
4.5 Power Supply for Sample Holders .....................................................................14
4.6 Selector Switch with Key....................................................................................15
5Connection Specifications.............................................................................16
5.1 Electrical Connection.........................................................................................16
5.2 Cooling Fluid......................................................................................................16
5.3 Gases................................................................................................................16
5.3.1 Specifications of the Detector Gas..........................................................17
5.3.2 Gas Impurities Specifications .................................................................18
5.3.3 Environment...........................................................................................18
6Installation.......................................................................................................19
6.1 Location.............................................................................................................19
6.2 Assembly Instructions of Diffractometer's Parts.................................................19
6.3 Gas Line Installation..........................................................................................20
6.4 Connection Specifications..................................................................................21
6.4.1 Computer Communication......................................................................21
6.4.2 Electrical Power Supply Connection.......................................................22
6.4.3 Connection Gas......................................................................................22
6.4.4 Installation of an External Gas Cylinder..................................................23
6.5 Additional Documentation..................................................................................24
7Operation.........................................................................................................25
7.1 Start Up.............................................................................................................25

7.2 Shut Down.........................................................................................................26
7.3 Emergency Stop................................................................................................26
7.4 Sample Holder...................................................................................................26
7.5 Sample Preparation Procedure..........................................................................29
8Maintenance and Cleaning.............................................................................30
8.1 Replacing the Gas Cylinder ...............................................................................30
8.2 Replacing the Cooling Fluid...............................................................................32
8.3 Cleaning and Replacing the Water Filter............................................................33
8.4 Checking the Emergency Stop Button ...............................................................33
8.5 Replacing the Main Power Supply Cord.............................................................34
8.6 Replacing the Fuses..........................................................................................34
8.7 Cleaning ............................................................................................................34
9Troubleshooting..............................................................................................35
10 Appendix 1: Conformity Certificate...............................................................36
11 Appendix 2: Cleaning and Replacing the Water Filter.................................37
12 Appendix 3: Optical paths of X-Rays in ARL EQUINOX 100 .......................38
13 Appendix 4: Periodic Preventive Maintenance.............................................39
14 Appendix 5: Sample Holders for ARL EQUINOX 100...................................41
15 Index ................................................................................................................43

Chapter | Introduction
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ARL EQUINOX 100
Page 5
2 Introduction
ARL EQUINOX X-Ray diffractometers are designed for measuring of crystalline samples
(powder, bulk, metals, thin layers, etc...), phase identification, nanoscale structural analysis,
non-destructive quality control, as well as for many other applications.
This instrument is intended for professionals. The user is advised to read the following
instructions and any other additional information supplied by Thermo Fisher Scientific before
operating the instrument.
Thermo Fisher Scientific declines all responsibilities for improper use by unauthorized
personnel or non-authorized operation of the instrument.
For any additional information, contact Thermo Fisher Scientific.
Supplied Items
Before the shipment, ARL EQUINOX X-Ray diffractometers are tested and packed carefully.
However damage can occur during the transport.
If the instrument or any additional supplied item has been damaged during transport, or if you
notice any signs of a possible damage, please contact both the transport company
representative and the Thermo Fisher Scientific representative as soon as possible.
Furthermore, if you notice that any part is missing or you have any questions about
the delivered items, contact the Thermo Fisher Scientific representative.
Storage
The storage where the instrument is stored has to meet following ambient specifications:
Temperature: 0 –50°C, relative humidity: < 95% (without condensation).
Assistance
The Thermo Fisher Scientific worldwide technical support network consists of highly trained
field service engineers, technical support specialists and service coordinators who are ready
to quickly assist the customers with answers and solutions to service needs and application
questions. If you need any help, please contact the local Thermo Fisher Scientific
representative.
Manufacturer
Thermo Fisher Scientific Brno s.r.o.
Vlastimila Pecha 12, Brno 627 00
Czech Republic

Chapter | Safety
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3 Safety
3.1 General Safety Guidelines
•Before using your ARL EQUINOX X-Ray diffractometer, read this instruction manual
completely and understand it. Please take notice of all warnings, cautions and notes to
ensure the correct and safe functioning of the instrument.
•Never place the instrument near an open flame or in an excessively hot environment. The
instrument must not be installed in an ATEX explosive hazard area.
•Never place the instrument in locations where excessive moisture or corrosive materials
are present.
•The instrument construction provides protection against the risk of electrical shock by
grounding the appropriate metal parts. The protection may not work properly unless the
power cord is connected to a properly grounded socket. It is customer's responsibility to
assure that a proper ground connection is provided.
•Never use flammable or corrosive fluids with this unit.
•Never use gases other than described in specifications.
•Never block the fan grid or the bottom of the instrument to allow a proper ventilation.
•If the instrument is used in a manner not specified by the Thermo Fisher Scientific, the
protection provided by the instrument may be impaired.
•Only accessories that comply with Thermo Fisher Scientific specifications are allowed to
be used with ARL EQUINOX X-Ray diffractometers.
•Transport of the instrument should be done with extreme care and should be done with an
appropriate lifting system, ideally a forklift truck with forks height not exceeding 115 mm.
•Never operate a damaged or a leaking instrument.
•Always turn the instrument OFF and disconnect the power cord from the power source
before performing any service or maintenance tasks, or before moving the instrument.
•Never operate the instrument with a damaged power cord.
•Never turn the instrument ON without a proper cooling fluid.
•Install the instrument on an appropriate table and make sure that the instrument can not
move horizontally.

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3.2 Hazard Statements and Symbols
The following messages are used throughout the manuals to highlight information.
Note A Note message indicates the information in it requires special attention.
CAUTION!
A Caution message indicates a potentially hazardous situation that, if not avoided,
may result in moderate or minor injury. It may also be used to alert against unsafe
practices.
WARNING!
A Warning message indicates a potentially hazardous situation that, if not avoided,
may result in death or severe injury.
DANGER!
A Danger message indicates an imminently hazardous situation that, if not avoided,
will result in death or severe injury.
WARNING!
Radiation danger –Indicates that X-Rays hazard may be present. Take necessary
precautions.
SERVICE!
A Service message indicates that the described procedure should be performed by
qualified personnel only.
3.3 Symbols on the Instrument
Note The symbol of electrical danger is located on the rear panel.
DANGER!
A danger of a potential risk of electrical shock in case of operation made on
components placed behind the rear panel. Any task must be performed by qualified
personnel only.

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3.4 Emergency Stop
In case of any problem (electrical, radiation or mechanical) there is an emergency stop button
located on the front panel of the instrument. Pushing the emergency button immediately
removes the power to the instrument, including the X-Ray generator. Be aware, that pushing
the emergency stop button will result in communication loss between the control computer
and the instrument.
CAUTION!
The emergency stop should not be used for routine shut down of the generator since
repeated rapid power shut downs may dramatically reduce the lifetime of your X-Ray
tube and damage the X-Ray generator.
3.5 Electricity
The symbol of electrical danger is present on the left of the appliance inlet on the rear
panel.
The switch disconnecter located on the rear of the ARL Equinox 100 allows disconnecting the
power supply from the mains. The position “0” “Off “means that the system is disconnected
from the mains. The position “I” “On” means that the system is connected to the mains.
3.6 High Voltage Generator
DANGER!
DANGER OF DEATH BY ELECTROCUTION:
Any tasks on the electrical equipment (high voltage generator, electronics...) must be
performed by certified and qualified personnel only.

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All energized parts are accessible with specific tools only. Any service tasks must be
performed only when the instrument is unplugged and by qualified personnel only. All
conductive parts are usually insulated from the energized parts and are grounded to each
other.
A safety beacon indicates that the X-Ray generator is in operation.
3.7 Protection Enclosure and X-Ray Tubeshield
WARNING!
WARNING IONIZING RADIATION:
X-Ray is ionizing radiation which has effects on living tissue and on the organism.
While the X-Ray generator is in operation and the shutter is open, no access inside
the enclosure is permitted.
Both the enclosure and the tubeshield of the ARL X-Ray diffractometer fulfill the function of a
protection shielding against the ionizing radiation. The enclosure surrounds the instrument
and helps to attenuate the diffused radiation emitted by the X-Ray tube. The X-Ray tube is
mounted in a tubeshield which is the most important part of the X-Ray protection. The optics
and collimation enable forming the X-Ray beam aperture to a directional beam. Never use the
instrument with a damaged enclosure, tubeshield or optics line!
Control circuits are designed to monitor the state of the shutter (opened or closed) and adjust
them accordingly while the generator is running.
Safety interlocks located on the enclosure's door enable to lock the door during the emission
of X-Rays in the analysis area.
3.8 Security Beacons
The ARL Equinox 100 X-Ray diffractometer is equipped with two security beacons located on
the right side of the front cover. The orange beacon "X-RAY" indicates that the X-Ray
generator is in operation and emitting X-Ray radiation. The red beacon indicates that the
shutter is opened and the X-Ray radiation is emitted inside of the enclosure.
Additional red LEDs to indicate the state of the shutter are located on the shutter as well (red
LEDs ON represents an opened shutter).
In case of a malfunction of the safety beacons the voltage of the X-Ray generator will be
limited and/or the shutter will remain closed.

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3.9 Gas
The ARL EQUINOX 100 uses a mixture consisting of 85% of argon and 15% of ethane . A gas
cylinder of 1 liter under 150 Bar can be installed in the system. During the operation of the
instrument, a micro-leakage of about 30 to 40 mm3of the detector gas may be released every
20/30 seconds from the GAS OUT valve located at the rear of the instrument. This is a
standard behavior.
WARNING!
Exposure to high concentrations of the detector gas may cause asphyxiation.
Symptoms of the asphyxiation may include loss of mobility and/or loss of
consciousness. The victim of the exposure of high concentrations of the detector gas
may not be aware of the asphyxiation. In such a case, remove the victim from the
contaminated area wearing self-contained breathing apparatus. Keep the victim warm
and rested and seek medical assistance. Apply artificial respiration if the victim
stopped breathing.
Ingestion is not considered as a potential route of exposure.
There are not any known toxicological effects related to this product.

Chapter | General Information
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ARL EQUINOX 100
Page 11
4 General Information
4.1 ARL EQUINOX 100 Front View
Height: 550 mm
Width: 750 mm
Depth: 560 mm
Weight ~80 kg
1 - Door locking system (safety
interlock)
2 - Front panel
3 - Security beacons
The door can be opened by pulling. The door is blocked while the instrument is in operation,
the door lock is released when the shutter is closed.

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4.2 ARL EQUINOX 100 Rear View
1 - Heat exhaust fan
2 - Water cooling fan
1 - Vacuum connection for
the mirror
2 - Gas outlet from the
detector
3 - Gas outlet from the safety
valve
4 - Gas inlet (for external gas
cylinder) max 6.5 Bar
5 - Outlet gas valve
6 -Main breaker
7 - Power cord connector with
a fuse
8 - RJ45 plug
9 - BNC video
SERVICE!
The connection of the instrument should be done by qualified personnel. The safety
valve hose should never be extended using any tubing device consisting of
components able to block the tubing.

Chapter | General Information
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Page 13
•Power: The electrical connection should be done by qualified personnel only.
•Vacuum: It is recommended to use a peristaltic pump in order to achieve vacuum in the
optic chamber. This will minimize the background noise and preserve the quality of the
layering of the mirror.
•Gas in: Gas in allows to connect the instrument to an external gas cylinder.
•Gas out: Gas out is the exhaust of the detector flush. By using the "flow valve" it is
possible to close the flushing and lower the gas consumption.
•RJ45: The RJ45 connector serves to connect the instrument to a computer using the
TCP/IP protocol.
SERVICE!
The service engineer can connect the X-Ray video for beam alignment. The use of
this connector is explained in the Service Guide.
4.3 ARL EQUINOX 100 Inside View
Sensitive components are protected by appropriate sensors to avoid radiation exposure:
optical line assembly, alignment tooling, door and panels. The picture describes the main
goniometric components of the instrument.
1 - CPS180, curved position sensitive detector
2 - Low power X-Ray source
3 - Shutter
4 - Elliptical mirror
5 - Crossed slits
6 - Anti-scattering knife
7 - Sample holder (SSRT type)
8 - Beam stop
9 - Safety sensor for service tasks
10 - Source alignment system

Chapter | General Information
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ARL EQUINOX 100
Page 14
The operator is allowed to configure following parameters:
•beam size, by adjusting the crossed slits (5),
•anti-scattering knife, to optimize beam/signal ratio (6),
•beam-stop height, to optimize low angle detection range (8),
•sample holder inclination, to set the appropriate incidence angle,
•sample holder type in order to choose the appropriate analysis (transmission, reflection,
thin film, ...). There are several sample holders available (see the Appendix 5: Sample
Holders for ARL EQUINOX 100 on page 41 for further information).
SERVICE!
In service mode, appropriate tools are used by the qualified personnel. Sensor (9)
allows to detect the service tooling.
Only the field service engineer is allowed to adjust the mirror housing (4) and
perform the beam centering procedure, dismount the CPS detector (1) and the X-Ray
source and its components: slits (5), mirror housing (4), shutter (3) and the
tubeshield (2).
4.4 Front Panel Information
There is a panel with an emergency stop button, a Power ON button and a Power OFF button
located on the front of the instrument. Please, see the section Operation on page 25 for
further information.
4.5 Power Supply for Sample Holders
The power supply plug for the spinning sample holder is located below the sample area.
1. Set of plugs to connect the sample holder.
1.1 A jack connector for the 12V power supply for spinning
the sample holder.
1.2 A 4 pin circular connector for the thin film sample holder
1.3 A Sub D9 connector for the 6 positions sample changer
2 The switch to turn ON the sample holder power supply.

Chapter | General Information
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Page 15
4.6 Selector Switch with Key
SERVICE!
3- Connector for safety sensors for service purpose only.
4- Video BNC connector for beam alignment.
5- Bypass key for service purposes.
The 3 positions selector switch with the key for maintenance
and alignment mode must be used by Thermo Fisher
Scientific FSE or other qualified personnel only. This key
allows to activate the maintenance mode by adapting the
safety loop for receiving the service tooling.

Chapter | Connection Specifications
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5 Connection Specifications
5.1 Electrical Connection
ARL EQUINOX X-Ray diffractometers have an Ingress Protection rating of IP20. This means
that they are protected against the ingress of solid particles with a diameter over 12 mm (e.g.:
a finger). ARL EQUINOX X-Ray diffractometers do not have any protection against the
ingress of liquids.
All connections to the instrument have to comply with class SELV (Safety Extra Low Voltage)
according to norm EN 61010-1:2010.
Equipment
Voltage (V)
Frequency (Hz)
Phase
Power (W)
Max consumption
(A)
ARL EQUINOX
110/230 10%
50/60
1
300
Computer
100/240
50/60
1
250
Screen
100/240
50/60
1
1
The ARL EQUINOX 100 complies with overvoltage category II (OVCII).
The ARL EQUINOX 100 complies with insulation class 1.
5.2 Cooling Fluid
The cooling circuit is integrated directly to the instrument. The composition of the cooling fluid
is based on a mixture of distilled water and 6% of ethylene glycol.
Note The cooling fluid level check should be performed regularly.
5.3 Gases
ARL EQUINOX curved position sensitive detector (PSD) belongs to the family of gaseous
ionization detectors. A gas cylinder has to be constantly connected to the instrument in order
to enable stable and optimal working conditions for a long term use.
DANGER!
FLAMMABLE GAS
The gas mixture contains ethane which is a flammable gas. Never place the
instrument near an open flame or in an excessively hot environment. The instrument
must not be installed in an ATEX explosive hazard area

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ARL EQUINOX X-Ray diffractometer can be equipped with a gas cylinder integrated directly
to the instrument. In this case, the cylinder should not exceed given dimensions based on the
specific instrument. Our gas regulator is equipped with a safety valve adjusted to 6.5 Bar. In
case of overpressure, a tubing allows to release the gas outside of the instrument.
Note Always use a gas regulator with the instrument.
Maximum dimension of the gas cylinder:
Diffractometer
model
Height –Valve
included- (mm)
Diameter (mm)
Recommended Gas Regulator
ARL EQUINOX 100
380
85
Messer (type FM53 with indicators
positioned next to each other)
If the gas cylinder cannot be installed as a part of the instrument, please follow the
instructions in Section Installation of an External Gas Cylinder on page 23.
5.3.1 Specifications of the Detector Gas
Specification Parameter
Value, Comments
Gas
Argon / Ethane (C2H6)
Argon: Q.S. N56
Ethane : 15%+/-0,3% Ethane N35
Detector high voltage
9.8 kV
Gas Pressure
6 Bar
Gas Flow
450 mm/min +/- 100 mm/min (i.e. 2 bubbles/min)

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5.3.2 Gas Impurities Specifications
The impurity levels are given in volumetric [ppm].
Argon > 99.9996 %
Ethane (C2H6) > 99.9 %
O2< 0.5
O2< 10
H2O < 2
H2O< 5
N2< 0.5
N2< 40
H2< 0.01
H2< 5
CnHm< 0.2
CnHm< 20
CO+CO2< 0.1
CO2< 10
C2H4< 400
CH4< 10
5.3.3 Environment
The instrument is rated as a Pollution Degree 2 (PD2) equipment. For disposal, follow the
legal requirements of your country.

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6 Installation
6.1 Location
WARNING!
LIFTING HAZARD!
When installing the EQUINOX 100, in the next step, either use lifting instruments or
four person lift as the EQUINOX 100 weights 80 kg.
The ARL EQUINOX X-Ray diffractometer is designed for indoor use only at an altitude level
below 2,000 m above sea level. The ARL EQUINOX X-Ray diffractometer must be placed in a
clean environment with constant ambient temperature. We advise an air conditioned room
where the room temperature is kept between 15 °C and 30 °C. The room must be ventilated
sufficiently. The relative humidity has to be in range from 20% to 80% without condensation.
•Never place the instrument near an open flame or in an excessively hot environment. The
instrument must not be installed in an ATEX explosive hazard area.
•Never place the instrument in locations where excessive moisture or corrosive materials
are present.
The ARL EQUINOX X-Ray diffractometer should be positioned in such a way so there is a
minimum clearance of 50 cm on each side of the instrument in order to keep access to the
main breaker easily.
Excessively dusty areas should be avoided and a periodic cleaning schedule should be
instituted.
The instrument should be placed on an appropriate surface. Accidental motion should be
avoided.
6.2 Assembly Instructions of Diffractometer's Parts
Installation, adjustment procedures and calibration should be performed by Thermo Fisher
Scientific service engineers only or by personnel certified by Thermo Fisher Scientific.
Otherwise, Thermo Fisher Scientific does not take any responsibilities for any malfunction or
damage caused by unauthorized installation of the instrument.
WARNING!
During any assembly operation, the ARL EQUINOX X-Ray diffractometer must be shut
down and disconnected from the power source!

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6.3 Gas Line Installation
The following assembly operations should be performed only by Thermo Fisher Scientific
service or one of its representative or properly trained users by Thermo Fisher Scientific.
If the gas cylinder cannot be installed that way inside the instrument, please follow the
instructions in the Installation of an External Gas Cylinder on page 23 where you will find the
procedure to install the cylinder outside of the instrument.
First, you will have to install the gas regulator on the gas cylinder. Simply screw the threaded
fitting of the gas regulator on the gas cylinder (pay attention to the way of tightening it, the
threads are reversed compare to a classical thread). Tighten it well in order to avoid any leaks
but not too hard to avoid damage of the threads. Apply appropriate procedure for detecting
gas leakage.
A short hose of 6 mm diameter with a male quick fitting already
mounted is shipped with the instrument.
Connect the hose to the gas regulator. The connector is a standard
Swagelok gas connector.
Insert the hose to the gas regulator outlet (without dismounting the nut)
and tighten the nut by hand. Then, by using a wrench, tighten it by 1 full
turn and ¼ of turn.
Ensure the gas regulator is well closed (turn completely anti clockwise).