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General Information

Confidential, limited rights

PN AA83865 | Revision A | 25-Oct-2019

Instruction Notice, ARL EQUINOX 5000-5500

Page

20

4.4.2 Mirror Configuration

1 - Sample holder supplies

2 - Shutter

3 - Mirror housing

4 - Crossed slits

5 - Sample holder (SSRT type)

6 - Safety sensor for service
tasks

This configuration is more advanced than the previous one. The optics consists in a multilayer X-
Ray mirror. Two famil

ies

of mirror

s

are available: Parabolic mirror or Ellipti cal mirror. The first

provide

s

a parallel beam (almost as parallel as the germanium monochromator), the second a

focused beam (focused on the detector).

The Kα1 and Kα2 separation is unavailable with X-Ray mirror but they produce a very high
flux of X-Ray (around 15 to 20 times more than Germanium monochromator).

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.).

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Содержание ARL EQUINOX 5000

Страница 1: ...ulfur Chlorine Argon Potassium Calcium Scandium Titanium Vanadium Chromium Manganese Iron Cobalt Nickel Copper Zinc Gallium Germanium Arsenic Selenium Bromine Krypton Rubidium Strontium Yttrium Zirconium Niobium Molybdenum Technetium Ruthenium Rhodium Palladium Silver Cadmium Indium Tin Antimony Tellurium Iodine Xenon Cesium Barium Lanthanum Cerium Praseodymium Neodymium Promethium Samarium Europi...

Страница 2: ...INOX 5000 5500 Page 2 1 Revision Table Revision Date ECO number Description of Changes A 23 OCT 2019 SDR21066 Initial release Note This document is the 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 ...

Страница 3: ...r Description 17 4 4 X Ray Optic Configurations 17 4 4 1 Monochromator Configuration 18 4 4 2 Mirror Configuration 20 4 4 3 Mirror Monochromator Configuration 21 4 5 Beam Stop and Anti diffusion Blade 22 4 6 Front Panel 23 4 7 Connections Inside the ARL EQUINOX 5000 5500 23 4 7 1 Sample Holders Connections 24 4 7 2 Service Connections 25 4 7 3 Vacuum for Mirror 26 4 7 4 Furnaces Connections 27 5 C...

Страница 4: ...0 7 6 Sample Preparation Procedure 42 8 Maintenance and Cleaning 43 8 1 X ray Tube Maintenance 43 8 2 Replacing the Gas Cylinder 44 8 3 Check Emergency Stop Button 46 8 4 Replace Main Power Supply Plug 46 8 5 Cleaning 46 9 Troubleshooting 47 10 Appendix 1 Certificate of Conformity 48 11 Appendix 2 Optical paths of X Rays in ARL EQUINOX 5000 5500 49 11 1 Mirror Configuration 49 11 2 Monochromator C...

Страница 5: ...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 co...

Страница 6: ...r 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 grids 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...

Страница 7: ... 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 Ray hazard may be present Take necessary precautions SERVICE A Service message indicates that the described procedure shou...

Страница 8: ...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 ...

Страница 9: ...ation which has effects on living tissue and on the organism While the X Ray generator is in operation and the shutter is opened 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 radi...

Страница 10: ... 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 LED ON represents an opened shutter In case of a malfunction of the safety beacons the v...

Страница 11: ...ment 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 breathi...

Страница 12: ... 828 mm Weight 400 kg 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 CAUTION Do not avoid the correct functioning of the door interlock When the shutter closes wait 5 seconds so that the door unlocks Trying to open the door too early when the door is still locked may block the door In this case the doo...

Страница 13: ...19 Instruction Notice ARL EQUINOX 5000 5500 Page 13 4 2 Rear View 1 Furnace connections 2 Water cooling and Gas connections panel 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 ...

Страница 14: ...nel 1 Main breaker 2 Circuit breakers 3 Main power cable 4 Ground connection ARL EQUINOX Connections Panel 5 RJ45 to PC 6 BNC video 7 USB 8 Vacuum for mirror housing 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 ...

Страница 15: ... 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 If the host space of the instrument is too small it is necessary to connect t...

Страница 16: ...ruction Notice ARL EQUINOX 5000 5500 Page 16 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 7 Z Motion motor 8 Goniometer stand 9 Beam stop and anti diffusion blade ...

Страница 17: ...tions see next drawings For these three configurations the operator is allowed to configure following parameters beam size by adjusting the crossed slits 4 usually 0 2 to 0 5mm anti scattering knife see Beam Stop and Anti diffusion Blade on page 22 to optimize beam signal ratio beam stop height see Beam Stop and Anti diffusion Blade on page 22 to optimize low angle detection range sample holder in...

Страница 18: ...s The picture describes the main goniometric components of the instrument 1 Sample holder supplies 2 Shutter 3 Monochromator housing 4 Crossed slits 5 Sample holder SSRT type 6 Safety sensor for service tasks This configuration is the most basic one The instrument can be equipped with a flat germanium monochromator or a flat Graphite HOPG monochromator The Germanium monochromator allows the separa...

Страница 19: ...ing in broader diffraction peaks These two kinds of flat monochromator share the same interests they are very simple to adjust are extremely strong and work for all X Ray radiations Resulting in no maintenance and only few realignments SERVICE In service mode appropriate tools are used by the qualified personnel Sensor 6 allows to detect the service tooling Only the field service engineer is allow...

Страница 20: ...nsists in a multilayer X Ray mirror Two families of mirrors are available Parabolic mirror or Elliptical mirror The first provides a parallel beam almost as parallel as the germanium monochromator the second a focused beam focused on the detector The Kα1 and Kα2 separation is unavailable with X Ray mirror but they produce a very high flux of X Ray around 15 to 20 times more than Germanium monochro...

Страница 21: ...ce tooling Only the field service engineer is allowed to adjust the mirror 3 or monochromator 4 and perform the beam centering procedure dismount the CPS detector 1 and the X Ray source and its components slits 4 mirror housing 3 shutter 2 and the tubeshield 4 4 3 Mirror Monochromator Configuration 1 Sample holder supplies 2 Shutter 3a Mirror housing 3b Monochromator housing 4 Crossed slits 5 Samp...

Страница 22: ...a Germanium monochromator alone One drawback of this optic is its adjustment complexity since it is difficult to monitor the beam coming out of the mirror housing before it reaches Germanium crystal SERVICE In service mode appropriate tools are used by the qualified personnel Sensor 6 allows to detect the service tooling Only the field service engineer is allowed to adjust the mirror 3a and monoch...

Страница 23: ...l avoid the direct X Ray beam to reach the detector in the case of transmission measurements or grazing incidence measurements 4 6 Front Panel 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 The Light button is used to turn ON the light inside the enclosure when the door is closed Please see the section Operation on pag...

Страница 24: ...ng of the sample holder This button is also used to power the alignment camera during service operation 2 A jack connector for the 12V power supply for spinning the sample holder SSRT or SSRZ and capillary sample holder This connector is also used to power the alignment camera during service operation 3 A 4 pin circular connector for the thin film sample holder 4 A RJ45 connector for the 30 positi...

Страница 25: ...ple holder 6 Connector for safety sensors for service purpose only 7 Video BNC connector for beam alignment 8 Positions selector switch with the key SERVICE The 3 positions selector switch 8 with the key for maintenance and alignment mode must be used by Thermo Fisher Scientific FSE or other qualified personnel only This key allows activating the maintenance mode by adapting the safety loop for re...

Страница 26: ...eneral Information Confidential limited rights PN AA83865 Revision A 25 Oct 2019 Instruction Notice ARL EQUINOX 5000 5500 Page 26 4 7 3 Vacuum for Mirror 9 ON OFF for vacuum pump 10 Vacuum connections to mirror ...

Страница 27: ...ited rights PN AA83865 Revision A 25 Oct 2019 Instruction Notice ARL EQUINOX 5000 5500 Page 27 4 7 4 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 ...

Страница 28: ...st 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 230 10 50 60 1 32 Water chiller 110 230 50 60 1 15 Computer 100 240 50 60 1 250 Screen 100 240 50 60 1 1 The ARL EQUINOX 5000 5500 complies with overvoltage category II OVCI...

Страница 29: ...ifications are given in the table below Parameter Min Max Critical values for generator safety stop Flow rate 3 5 L min 6 L min 3 L min Pressure 3 bar 8 bar Temperature 18 C 25 C 10 C 35 C Conductivity 10 μS cm 250 μS cm Harness German degrees 1 D 4 D Acidity pH 7 5 9 5 Input Output Quick fittings for polyurethanes hoses Øinner 7 mm Øouter 10 mm Taken from X Ray tube manufacturer specification The...

Страница 30: ...rea ARL EQUINOX 5000 5500 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 regulato...

Страница 31: ...S N56 Ethane 15 0 3 Ethane N35 Detector high voltage 9 8 kV Gas Pressure 6 bar Gas Flow 0 6 to 0 7 ccm 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 4 Environment The instrument is rated as a Pollution Degree 2 PD2 equipment Fo...

Страница 32: ... 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 5000 5500 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 ...

Страница 33: ...as 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 f...

Страница 34: ...as regulator and on the input gas circuitry a safety valve preloaded at max 6 5 bar to avoid any over pressure inside of the instrument 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 EQ...

Страница 35: ... be connected to earth by a wire of 6mm cross section 6 4 3 Gas Connection SERVICE Open the valve 2 of the gas cylinder 1 and open slightly the gas regulator 3 in order to have a low gas flow Then connect the male quick fitting to the Inside Gas Bottle connector 4 This will avoid air pollution in the detector Adjust very slowly the outlet gas pressure on the regulator to the recommended value 6 ba...

Страница 36: ...h 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 1 Open the gas cylinder and slightly open the gas regulator in order to have a small gas flow 2 Connect the long hose male fitting in the input receptacle GAS IN located on the back panel 3 Adjust the outlet gas pressure on the regulator to ...

Страница 37: ...sonnel certified by Thermo Fisher Scientific Otherwise Thermo Fisher Scientific does not take any responsibility for any malfunction or damage caused by unauthorized installation of the instrument 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 supplie...

Страница 38: ...stop button is released 4 When the white button marked Power ON located on the front panel is illuminated push on it 5 After powering the instrument ON the red light of the Power OFF button turns ON 6 If the instrument is connected to an external cooling circuit make sure the source of the cooling water is opened with appropriate characteristics 7 After several tens of seconds the system will be r...

Страница 39: ...ton labeled Power OFF located on the front panel After you pushed it this red button will turn OFF and the white button Power ON will illuminate 4 Turn the main breaker located on the rear of the unit to the 0 OFF position 5 Close the cooling fluid supply about ten minutes after the generator reached 0 kV and 0 mA in order to properly cool down the X Ray tube 7 3 Emergency Stop In case of any prob...

Страница 40: ... to maintain the powder sample mount Insert the sample holder in the sample holder mounting hole of the instrument 5 do not use any unnecessary force The sample holder and the mounting hole ø 30 mm are designed to avoid any mechanical clearance resulting in irreproducible results The pin 3 of the sample holder has to be inserted in the reference hole 6 The incidence angle indicator consists of two...

Страница 41: ...N AA83865 Revision A 25 Oct 2019 Instruction Notice ARL EQUINOX 5000 5500 Page 41 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 ...

Страница 42: ... microscopes If the powder to be measured is too coarse it s necessary to grind it a bit using a small mortar Fill the cavity with the powder Use a glass slide to make the surface flat and homogeneous The surface of the powder must not exceed the level of the surface of the powder mount in order to avoid line displacement error due to height error The powder mount is clamped in the sample holder b...

Страница 43: ...o the tube documentation to learn more about tube maintenance operations The most common maintenance operations on X ray tube are water flow issues and sudden X ray source failure With time X ray tube intensity will decrease this is a normal wear To keep maximum performance it is advised to change X ray tube periodically from 3 to 5 years In case of a water flow issue the X ray tube is the only pa...

Страница 44: ...eft indicator in case of using the FM53 gas regulator Gas circuit The gas cylinder 1 is connected to the instrument gas inlet 2 fast connector The T 4 distributes the gas in the detector 3 and the external gas inlet 5 The detector out 6 is connected to the micro leak valve 7 This one is connected to the isolating valve 8 and go to external exhaust 9 The last circuit is the overpressure line from t...

Страница 45: ... gas cylinder and open slightly the gas regulator in order to have a low gas flow Connect the inlet fitting to the input receptacle Inside Gas Bottle 2 and adjust the outlet gas pressure on the regulator to the recommended value 6 bar 11 If the gas pressure is set too high use the output connector of the CPS detector To decrease the pressure close the gas regulator and insert a male quick fitting ...

Страница 46: ...in Windows Push the emergency stop button The instrument must switch OFF no noise from the instrument can be heard the red POWER OFF button switches OFF and the white POWER ON button switches ON Pressing the POWER ON button should not allow powering ON the ARL EQUINOX 5000 5500 The emergency stop button has to be unlocked with the key 8 4 Replace Main Power Supply Plug If the shipped power supply ...

Страница 47: ...n I ON position Check the position of the circuit breakers on the back of the instrument they must be in ON position If the problem remains contact Thermo Fisher Scientific An error message appears when the control software is launched Close the error message by clicking on OK Terminate the communication between the instrument and the computer by right clicking on the radiation icon in the task ba...

Страница 48: ...ruments that emit X Ray radiations Thermo Fisher Scientific declares under its own responsibility that the ARL EQUINOX 5000 5500 X Ray diffractometers series and respective accessories comply with the CE mark according to the following standards and directives EN 61010 1 2010 Safety requirements for electrical equipment for measurement control and laboratory use Part 1 General requirements EN 6132...

Страница 49: ... that the X rays travel more distance up to the detector The figure above describes the X Ray beam propagation inside of the enclosure when the shutter is opened and with a mirror configuration During this operation the enclosure is closed and door is locked 1 X Ray source emission Scattering is emitted in all directions The tubeshield is limiting the X Rays 2 X Ray mirror allows capturing a given...

Страница 50: ...ntical except that the X rays travel more distance up to the detector The figure above describes the X Ray beam propagation inside of the enclosure when the shutter is opened and with a monochromator configuration During this operation the enclosure is closed and door is locked 1 X Ray source emission Scattering is emitted in all directions The tubeshield is limiting the X Rays 2 The monochromator...

Страница 51: ...travel more distance up to the detector The figure above describes the X Ray beam propagation inside of the enclosure when the shutter is opened and with a mirror monochromator configuration During this operation the enclosure is closed and door is locked 1 X Ray source emission Scattering is emitted in all directions The tubeshield is limiting the X Rays 2 X Ray mirror allows capturing a given so...

Страница 52: ... 25 Oct 2019 Instruction Notice ARL EQUINOX 5000 5500 Page 52 5 The anti scattering knife decreases the diffusion from the slits 6 The sample is able to diffract the beam according to its atomic structure 7 The beam stop blocks the direct beam A proper adjustment of this plate allows to improve the low angle detection ...

Страница 53: ...o Fisher Scientific or an authorized person When necessary Clean filter of X Ray tube Contact Thermo Fisher Scientific or an authorized person Annually Check the emergency stop button Pushing the emergency stop button must switch off the instrument This procedure can be done by the customer refer to Section Check Emergency Stop Button on page 46 Annually Check the beam alignment Contact Thermo Fis...

Страница 54: ...ion or transmission The user can also identify phase transition by using Anton Paar furnaces characterize thin film structures or acquire automatically up to 30 samples with our sample changer Fixed non spinning sample holder Reflection transmission mode Spinning sample holder for powder sample Reflection transmission mode Spinning sample holder for powder bulk sample Reflection mode Spinning samp...

Страница 55: ... ARL EQUINOX 5000 5500 Page 55 Motorized thin layer sample holder Bulk sample also Reflection mode Anton Paar high temperature furnace From 20 C to 1500 C 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 ...

Страница 56: ...e the ARL EQUINOX 5000 5500 24 Cooling Fluid 31 E Electrical Connection 29 Electrical Power Supply Connection 37 Electricity 8 Emergency Stop 7 42 Enclosure Light 42 Environment 33 F Front Panel 24 Front View 12 Furnaces Connections 28 G Gas Connection 37 Gas Impurities Specifications 32 Gas Line Installation 35 Gas Safety 10 Gas Specification 31 General Information 12 General Safety Guidelines 6 ...

Страница 57: ...on Notice ARL EQUINOX 5000 5500 Page 57 Service Connections 26 Shut Down 42 Specifications of the Detector Gas 32 Start Up 41 Symbols on the Instrument 7 T Troubleshooting 51 V Vacuum for Mirror 27 X X Ray Goniometer Description 16 X Ray Optic Configurations 17 X ray Tube Maintenance 47 ...

Страница 58: ...ghts reserved All trademarks are the property of Thermo Fisher Scientific and its subsidiaries unless otherwise specified In Switzerland Thermo Fisher Scientific En Vallaire Ouest C Case Postale CH 1024 Ecublens Switzerland 41 0 21 694 71 11 info spectrometry thermofisher com Thermo Fisher Scientific Ecublens SARL Switzerland is ISO certified ...

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