Thermo Scientific ARL EQUINOX 5000 Instruction Notice
Thermo Scientific ARL EQUINOX 5000 Instruction Notice

Thermo Scientific ARL EQUINOX 5000 Instruction Notice

X-ray diffractometer
Table of Contents

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1
H
Hydrogen
3
Li
Lithium
11
12
Na Mg
Sodium
Magnesium
19
20
K
Ca Sc
Potassium
Calcium
37
38
39
Rb Sr
Y
Rubidium
Strontium
Yttrium
55
56
57
Cs Ba La
Cesium
Barium
Lanthanum
87
88
89
**
Fr Ra Ac
Francium
Radium
Actinium
Rutherfordium
58
*
Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
Cerium
90
**
Th Pa
Thorium
Protactinium
Thermo Scientific
ARL EQUINOX 5000
ARL EQUINOX 5500
X-Ray Diffractometer
Instruction Notice
AA83865 - A • October 2019
4
Be
Beryllium
21
22
23
24
25
Ti
V
Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
Scandium
Titanium
Vanadium
Chromium
Manganese
40
41
42
43
44
Zr Nb Mo Tc Ru Rh Pd Ag Cd In
Zirconium
Niobium
Molybdenum
Technetium
Ruthenium
72
73
74
75
76
*
Hf
Ta
W Re Os
Hafnium
Tantalum
Wolfram
Rhenium
Osmium
104
105
106
107
108
Rf Db Sg Bh Hs Mt Ds Rg Cn Nh Fl Mc Lv Ts Og
Dubnium
Seaborgium
Bohrium
Hassium
Meitnerium
59
60
61
62
63
Praseodymium
Neodymium
Promethium
Samarium
Europium
91
92
93
94
95
U
Np Pu Am Cm Bk Cf Es Fm Md No Lr
Uranium
Neptunium
Plutonium
Americium
26
27
28
29
30
Iron
Cobalt
Nickel
Copper
Zinc
45
46
47
48
49
Rhodium
Palladium
Silver
Cadmium
Indium
77
78
79
80
81
Ir
Pt Au Hg Tl
Iridium
Platinum
Gold
Mercury
Thallium
109
110
111
112
113
Darmstadtium
Roentgenium
Copernicium
Nihonium
Flerovium
64
65
66
67
68
Gadolinium
Terbium
Dysprosium
Holmium
Erbium
96
97
98
99
100
Curium
Berkelium
Californium
Einsteinium
Fermium
Mendelevium
5
6
7
8
B
C
N
O
Boron
Carbon
Nitrogen
Oxygen
13
14
15
16
17
Al
Si
P
S
Cl
Aluminum
Silicon
Phosphorus
Sulfur
Chlorine
31
32
33
34
35
Gallium
Germanium
Arsenic
Selenium
Bromine
50
51
52
53
54
Sn Sb Te
I
Xe
Tin
Antimony
Tellurium
Iodine
Xenon
82
83
84
85
86
Pb Bi Po At Rn
Lead
Bismuth
Polonium
Astatine
Radon
114
115
116
117
118
Moscovium
Livermorium
Tennessine
Oganesson
69
70
71
Thulium
Ytterbium
Lutetium
101
102
103
Nobelium
Lawrencium
2
He
Helium
9
10
F
Ne
Fluorine
Neon
18
Ar
Argon
36
Krypton

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Summary of Contents for Thermo Scientific ARL EQUINOX 5000

  • Page 1 Np Pu Am Cm Bk Cf Es Fm Md No Lr Thorium Protactinium Uranium Neptunium Plutonium Americium Curium Berkelium Californium Einsteinium Fermium Mendelevium Nobelium Lawrencium Thermo Scientific ARL EQUINOX 5000 ARL EQUINOX 5500 X-Ray Diffractometer Instruction Notice AA83865 - A • October 2019...
  • Page 2: Revision Table

    The information in this document is subject to change without notice. We assume no responsibility for any errors that may appear in this document. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 2...
  • Page 3: Table Of Contents

    Gas Safety ......................General Information ..................Front View ......................Rear View ......................X-Ray Goniometer Description ................4.3.1 ARL EQUINOX 5000 Goniometer Description ........4.3.2 ARL EQUINOX 5500 Goniometer Description ........X-Ray Optic Configurations ................4.4.1 Monochromator Configuration ..............4.4.2 Mirror Configuration ................
  • Page 4 Connection Specifications .................. 6.4.1 Computer Communication ..............6.4.2 Electrical Power Supply Connection ............6.4.3 Gas Connection ..................6.4.4 ARL EQUINOX 5000/5500: Installation of an External Gas Cylinder ..6.4.5 Additional Documentation ............... Operation ......................Start Up ......................Shut Down ......................
  • Page 5: Introduction

    For any additional information, contact Thermo Fisher Scientific. Supplied Items Before the shipment, ARL EQUINOX 5000/5500 X-Ray diffractometer is 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.
  • Page 6: Safety

    3.1 General Safety Guidelines • Before using your ARL EQUINOX 5000/5500 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.
  • Page 7: Hazard Statements And Symbols

    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. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 7...
  • Page 8: Emergency Stop

    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 5000/5500 allows disconnecting the power supply from the mains. The position “ 0” “Off “means that the system is disconnected from the mains.
  • Page 9: High Voltage Generator

    Safety interlocks located on the enclosure's door enable to lock the door during the emission of X-Rays in the analysis area. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 9...
  • Page 10: Security Beacons

    Chapter | Safety 3.8 Security Beacons The ARL EQUINOX 5000/5500 X-Ray diffractometer is equipped with two security beacons located on the upper 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.
  • Page 11: Gas Safety

    Chapter | Safety 3.9 Gas Safety The ARL EQUINOX 5000/5500 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 0.6 to 0.7 ccm of the detector gas is released from...
  • Page 12: General Information

    OFF and ON again in order to restart the safety loop. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 12...
  • Page 13: Rear View

    3- ARL EQUINOX connections panel 4- Electrical connections panel 5- Cooling fans 6- Access to furnace controller front panel 7- Cables feed through 8- Cooling grids Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 13...
  • Page 14 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. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 14...
  • Page 15 SERVICE! The service engineer can connect the X-Ray video for beam alignment. The use of this connector is explained in the Service Guide. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 15...
  • Page 16: X-Ray Goniometer Description

    Chapter | General Information 4.3 X-Ray Goniometer Description 4.3.1 ARL EQUINOX 5000 Goniometer Description 1 - CPS 120 X-Ray detector 2 - 2 arm 3 -  Rotation 4 - X-Ray source 5 - Alignment camera 6 - Sample holder stand...
  • Page 17: Arl Equinox 5500 Goniometer Description

    8 - Goniometer stand 9 - Beam stop and anti-diffusion blade 4.4 X-Ray Optic Configurations The ARL EQUINOX 5000/5500 can be equipped with three different optic configurations (see next drawings). For these three configurations, the operator is allowed to configure following parameters: •...
  • Page 18: Monochromator Configuration

    The Germanium monochromator allows the separation between Kα1 and Kα2 for high resolution studies. The drawback is the lack of signal meaning longer acquisitions. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 18...
  • Page 19 CPS detector and the X -Ray source and its components: slits (4), monochromator housing (3), shutter (2) and the tubeshield. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 19...
  • Page 20: Mirror Configuration

    The alignment is a bit more complicated than the alignment of a flat monochromator and an X-Ray mirror is always dedicated to only one X-Ray radiation (Cu, Co, etc.). Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 20...
  • Page 21: Mirror-Monochromator Configuration

    3a - Mirror housing 3b - Monochromator housing 4 - Crossed slits 5 - Sample holder (SSRT type) 6 - Safety sensor for service tasks Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 21...
  • Page 22: Beam Stop And Anti-Diffusion Blade

    3 - Beam stop height adjustment screw 4 - Anti-diffusion Blade height adjustment screw 5 - Anti-diffusion Blade tilt adjustment screws 6 - Beam stop tilt adjustment screws Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 22...
  • Page 23: Front Panel

    Please, see the section Operation on page for further information. 4.7 Connections Inside the ARL EQUINOX 5000/5500 The power supply plug for the spinning sample holder, the selector switch with the key for maintenance and the vacuum connections to mirror are located below the sample area.
  • Page 24: Sample Holders Connections

    3- A 4 pin circular connector for the thin film sample holder. 4 - A RJ45 connector for the 30 positions sample changer (ASC30). Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 24...
  • Page 25: Service Connections

    Thermo Fisher Scientific FSE or other qualified personnel only. This key allows activating the maintenance mode by adapting the safety loop for receiving the service tooling. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 25...
  • Page 26: Vacuum For Mirror

    Chapter | General Information 4.7.3 Vacuum for Mirror 9- ON-OFF for vacuum pump 10- Vacuum connections to mirror Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 26...
  • Page 27: Furnaces Connections

    1/ 2- Gas connection for BTS furnace 3 /4- Cooling water for BTS furnace 1 /2- Cooling water for HTK 3 /4- not used for HTK furnace Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 27...
  • Page 28: Connection Specifications

    ARL EQUINOX 5000/5500 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 5000/5500 X-Ray diffractometers do not have any protection against the ingress of liquids.
  • Page 29: Cooling Fluid

    Chapter | Connection Specifications 5.2 Cooling Fluid The cooling circuit of the ARL EQUINOX 5000/5500 has to be connected to an external cooling device. The cooling specifications are given in the table below. Parameter Critical values for generator safety stop Flow rate 3.5 L/min...
  • Page 30: Gas Specification

    Chapter | Connection Specifications 5.3 Gas Specification The ARL EQUINOX 5000/5500 uses curved position sensitive X-Ray detectors (CPS) which belong to the family of gaseous ionization detectors. A gas cylinder has to be co nstantly connected to the instrument in order to enable stable and optimal working conditions for a long term use.
  • Page 31: Specifications Of The Detector Gas

    < 10 5.4 Environment The instrument is rated as a Pollution Degree 2 (PD2) equipment. For disposal, follow the legal requirements of your country. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 31...
  • Page 32: Installation

    When installing the ARL EQUINOX 5000/5500, use lifting inst ruments as the ARL EQUINOX 5000/5500 weights about 400 kg. The ARL EQUINOX 5000/5500 X-Ray diffractometer is designed for indoor use only at an altitude level below 2,000 m above sea level. The ARL EQUINOX 5000/5500 X-Ray diffractometer must be placed in a clean environment with constant ambient temperature.
  • Page 33: Gas Line Installation

    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). Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 33...
  • Page 34: Connection Specifications

    6.4 Connection Specifications 6.4.1 Computer Communication The ARL EQUINOX 5000/5500 is shipped with a computer that already has all software required for operating the instrument. You just have to connect the RJ45 cable to the ARL EQUINOX connections of the ARL EQUINOX 5000/5500 X-Ray diffractometer and to the Ethernet port of the computer.
  • Page 35: Gas Connection

    Section Installation of an external gas cylinder. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 35...
  • Page 36: Arl Equinox 5000/5500: Installation Of An External Gas Cylinder

    Chapter | Installation 6.4.4 ARL EQUINOX 5000/5500: Installation of an External Gas Cylinder The gas regulator has to be mounted on the gas cylinder (be careful, the thread is anti-clockwise). If the gas regulator is not shipped with the instrument, it is the responsibility of the user to obtain and install the regulator locally as well as a safety valve (preloaded to max 6.5 bar) on the input gas circuit to avoid any overpressure inside of the instrument.
  • Page 37: Additional Documentation

    Additional documentation concerning the X-Ray diffraction theory, asymmetrical geometry, alignment, calibration and the adjustment of the ARL EQUINOX 5000/5500 X -Ray diffractometer's accessories are supplied in PDF file format in the folder “C:\INEL\Documentation”...
  • Page 38: Operation

    After several tens of seconds the system will be ready for operation. Note The ARL EQUINOX 5000/5500 X-Ray diffractometer driving operations are made by Symphonix software. Please, read the Symphonix user guide for further inform ation on how to use the instrument. The Symphonix user's guide is available in PDF file format in the folder c:/inel/Documentation/SymphoniX user guide.pdf...
  • Page 39: Shut Down

    Then, when the door is opened, the button is illuminated whatever if it is pushed or released. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 39...
  • Page 40: Sample Holder

    Chapter | Operation 7.5 Sample Holder All ARL EQUINOX 5000/5500 instruments are shipped with a basic non -spinning sample holder suited for powder measurement in reflection mode. This sample holder is necessary for adjustment and alignment and can be used for measurement as well.
  • Page 41 Chapter | Operation CAUTION! For the ARL EQUINOX 5000/5500 the incidence angle must be fixed with the omega motor setting! Note In the above configuration, the incidence angle is equal to 6°. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500...
  • Page 42: Sample Preparation Procedure

    The powder mount is clamped in the sample holder by tightening lightly the screw of the non-spinning sample holder. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 42...
  • Page 43: Maintenance And Cleaning

    Chapter | Maintenance and Cleaning Maintenance and Cleaning The ARL EQUINOX 5000/5500 X-Ray diffractometer is designed to require only minimal maintenance operations. However, several preventive maintenance tasks should be performed regularly to keep an optimal working state of your instrument. Please refer to...
  • Page 44: Replacing The Gas Cylinder

    The gas leak valve (7) is adjusted in the factory and should not be modified. It allows controlling the right consumption of gas, allowing an optimum regeneration of the gas inside detector. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 44...
  • Page 45 (consisting in a female quick fitting receptacle) for a fe w seconds. Increase again the pressure by opening slowly the gas regulator. Remount the front bottom left cover of the ARL EQUINOX 5000/5500. Start up the ARL EQUINOX 5000/5500 (see Operation on page 38).
  • Page 46: Check Emergency Stop Button

    External parts and the enclosure can be cleaned with a soft and dry duster. Domestic alcohol is forbidden as it can damage paint and markings. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 46...
  • Page 47: Troubleshooting

    Push the OFF button of the instrument, wait for few minutes and turn the instrument ON and launch software again. • If the problem remains, contact Thermo Fisher Scientific. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 47...
  • Page 48: Appendix 1: Certificate Of Conformity

    EMC requirements - Part 1: General requirements, • 2011/65/EC: restriction of the use of certain hazardous substances in electrical and electronic equipment, RoHS2. Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 48...
  • Page 49: Appendix 2: Optical Paths Of X-Rays In Arl Equinox 5000/5500

    EQUINOX 5000/5500 11.1 Mirror Configuration The figure shows an ARL EQUINOX 5000 with a CPS120 detector. For the ARL EQUINOX 5500 that is equipped with a CPS590 (bigger radius), the X-ray path is identical except that the X-rays travel more distance up to the detector.
  • Page 50: Monochromator Configuration

    11.2 Monochromator Configuration The figure shows an ARL EQUINOX 5000 with a CPS120 detector. For the ARL EQUINOX 5500 that is equipped with a CPS590 (bigger radius), the X-ray path is identical except that the X-rays travel more distance up to the detector.
  • Page 51: Mirror And Monochromator Configuration

    11.3 Mirror and Monochromator Configuration The figure shows an ARL EQUINOX 5000 with a CPS120 detector. For the ARL EQUINOX 5500 that is equipped with a CPS590 (bigger radius), the X-ray path is identical except that the X-rays travel more distance up to the detector.
  • Page 52 Chapter | Appendix 2: Optical paths of X-Rays in ARL EQUINOX 5000/5500 The anti-scattering knife decreases the diffusion from the slits. The sample is able to diffract the beam according to its atomic structure. The beam stop blocks the direct beam. A proper adjustment of this plate allows to improve the low angle detection.
  • Page 53: Appendix 3: Periodic Preventive Maintenance

    Contact Thermo Fisher Scientific or an authorized person. circuit tightness Annually Check the Contact Thermo Fisher Scientific or an authorized person. safety interlocks Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 53...
  • Page 54: Appendix 4: Sample Holders For Arl Equinox 5000/5500

    13 Appendix 4: Sample Holders for ARL EQUINOX 5000/5500 ARL EQUINOX 5000/5500 Thermo Fisher Scientific X-Ray diffractometer allows several types of configurations. Thanks to the number of proposed sample holders, user can perform conventional XRD powder analysis for quality control or quantitative analysis (reflection or transmission).
  • Page 55 Chapter | Appendix 4: Sample Holders for ARL EQUINOX 5000/5500 Motorized thin layer Anton Paar high sample holder. temperature furnace From 20°C to 1500˚C. Bulk sample also Reflection mode Reflection mode CAUTION! Hot surface on high temperature furnace! Do not touch this surface without adequate protective measures. Refer to Anton Paar instruction manual for more information.
  • Page 56: Index

    Hazard Statements and Symbols • 6 Periodic Preventive Maintenance • 47, 56 High Voltage Generator • 8 Appendix 4 Sample Holders for ARL EQUINOX 5000/5500 • Installation • 34 17, 58 ARL EQUINOX 5000 Goniometer Description • 16 Introduction • 5 ARL EQUINOX 5000/5500 Installation of an External Gas Cylinder •...
  • Page 57 Troubleshooting • 51 Vacuum for Mirror • 27 X-Ray Goniometer Description • 16 X-Ray Optic Configurations • 17 X-ray Tube Maintenance • 47 Confidential, limited rights Instruction Notice, ARL EQUINOX 5000-5500 PN AA83865 | Revision A | 25-Oct-2019 Page 57...
  • Page 58 Thermo Fisher Scientific (Ecublens) SARL, Switzerland is ISO certified. In Switzerland: Thermo Fisher Scientific +41 (0)21 694 71 11 En Vallaire Ouest C, Case Postale info.spectrometry@thermofisher.com CH-1024 Ecublens, Switzerland thermofisher.com/elemental Find out more at For Research Use Only. Not for use in diagnostic procedures. © 2018 Thermo Fisher Scientific Inc. All rights reserved.

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