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FAME-UHD experimental station
5 crystals Crystal Analyser Spectrometer
Volume I - User Instruction
Date Version Reason Writer Technical
approval
Safety approval
25/11/2016 A Creation O. Proux J.-L. Hazemann S. Ricot
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Table of contents
1 Introduction ....................................................................................................................... 5
1.1 Contents of the CE declaration ............................................................................................ 5
1.2 Details of the different volume ........................................................................................... 5
2 Safety ................................................................................................................................. 6
2.1 General instructions ............................................................................................................ 6
2.2 Obligations ........................................................................................................................... 6
2.3 Interdictions ........................................................................................................................ 7
2.4 Residual risks ....................................................................................................................... 7
3 Description of the equipment & scope of the certification.................................................... 8
3.1 Part 1 - Experimental table ................................................................................................ 10
3.1.1 Description ................................................................................................................ 10
3.1.2 Safety in place / implemented protective measures ................................................ 11
3.2 Part 2 - Crystal Analyzer Spectrometer ............................................................................. 12
3.2.1 Description ................................................................................................................ 12
3.2.2 Safety in place / implemented protective measures ................................................ 13
Part 3 - Helium bag ..................................................................................................................... 15
3.2.3 Description ................................................................................................................ 15
3.2.4 Safety in place / implemented protective measures ................................................ 15
3.3 Part 4 - Experimental slits, tubes, diodes & windows ....................................................... 16
3.3.1 Description ................................................................................................................ 16
3.3.2 The slits ...................................................................................................................... 16
3.3.3 The diodes ................................................................................................................. 17
3.3.4 The vacuum set-up & the windows ........................................................................... 18
3.4 Part 5 - Sample-holder ....................................................................................................... 19
3.4.1 Description ................................................................................................................ 19
3.4.2 Motions ..................................................................................................................... 20
3.4.3 Aim of the sample holder .......................................................................................... 20
3.4.4 Safety in place / implemented protective measures ................................................ 20
4 Assembly and Dismantling ................................................................................................ 21
4.1 Part 1 - Experimental table ................................................................................................ 21
4.2 Part 2 - Crystal Analyzer Spectrometer ............................................................................. 23
Experimental table - CAS interface ........................................................................................ 23
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5-crystals Crystal Analyzer Spectrometer mechanical assembly .......................................... 24
Crystal Analyzer Spectrometer cabling and control command ............................................ 25
4.3 Part 3 - Helium bag ............................................................................................................ 26
4.4 Part 4 - Experimental slits, tubes, diodes & windows ....................................................... 29
Mechanical assembly ............................................................................................................. 29
Mounting of the Be windows on the flange .......................................................................... 30
4.5 Part 5 - Sample-holder ....................................................................................................... 32
Mechanical assembly ............................................................................................................. 32
Cabling and control command ............................................................................................... 33
5 Use ................................................................................................................................... 34
5.1 User mode 1 - Operation mode......................................................................................... 34
5.1.1 Sample positioning .................................................................................................... 34
5.1.2 Making the hutch search ........................................................................................... 35
5.1.3 Sample alignment ...................................................................................................... 36
5.2 User mode 2 - Expert mode or experiment preparation mode ........................................ 37
5.2.1 Helium bag operations .............................................................................................. 37
5.2.2 Crystal change ........................................................................................................... 37
5.2.3 Crystal alignment with laser ...................................................................................... 38
5.2.4 Crystal alignment with the X-ray beam ..................................................................... 39
5.2.5 Detector change ........................................................................................................ 41
5.2.6 Slits vessel venting ..................................................................................................... 41
6 Annex ............................................................................................................................... 42
6.1 Annex 1: CE plate ............................................................................................................... 42
6.2 Annex 2: CE declaration ..................................................................................................... 43
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1 Introduction
1.1 Contents of the CE declaration
Designation of the equipment:
Type: 5 crystals Crystal Analyzer Spectrometer for High Energy Resolution X-ray
Fluorescence detection
The equipment manufacturer is:
CNRS - Institut Néel No. SIRET: 180 089 013 00387
25 Avenue des Martyrs
38042 Grenoble, France
Authorised representative:
Etienne Bustarret – Head of the French CRG Exploitation Structure for the CNRS - Neel
Institute Director
Institut NEEL CNRS/UGA UPR2940
25 rue des Martyrs
38042 GRENOBLE Cedex 9 - FRANCE
The equipment is in conformity with:
2006/42/EC Machinery
2006/95/EC Low voltage Equipment
1.2 Details of the different volume
The technical documentation for the CE Certification is:
Volume I: User instruction (User manual + Maintenance)
Volume II: Risk assessment
Volume III: Drawings, calculation notes, tests results, graph
Volume IV: Documents concerning other products incorporated into the equipment
This document has been compiled by:
Olivier PROUX
Observatoire des Sciences de l'Univers de Grenoble beamlines (UMS 832 CNRS - UGA)
beamlines CRG-FAME & CRG-FAME/UHD
71, avenue des Martyrs
38000 GRENOBLE- FRANCE
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2 Safety
2.1 General instructions
Please read the following safety precautions carefully before using the equipment to avoid
accidents and damage to the equipment. Keep these safety instructions readily available for
all users of the equipment.
WARNING:
This symbol is used to indicate general dangers. To prevent possible injury,
read all warnings before using this equipment.
2.2 Obligations
This symbol refers to other pages or documents.
Read the associated procedure in the annex or carefully read this procedure
Safety gloves must be worn
Safety shoes must be worn
Eye protection must be worn
Mask must be worn
Ear protection must be worn
Hard Hat must be worn
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2.3 Interdictions
It is forbidden to sit on the experimental table during sample positioning
do not use sharp objects close to the helium bag
2.4 Residual risks
Danger of falling
Danger: electricity
Warning moving parts. Risk of crushing
Laser beam
Overhead load
Pressurized helium bottle
Chemical risk : beryllium
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3 Description of the equipment & scope of the certification
This document describes the essential safety regulations that must be respected during
operation and maintenance of the experimental station installed on CRG/FAME-UHD BM16
beamline. This beamline is one of the Collaborative Research Group beamline called French
Absorption spectroscopy beamline in Material and Environmental sciences at Ultra-High
Dilution (CRG/FAME-UHD) and operated by CEA and CNRS.
The experimental station on BM16 is based on a Crystal Analyzer Spectrometer (CAS) devoted
to X-ray Absorption Spectroscopy (XAS) measurement in fluorescence mode. Fluorescence-
XAS measurements are routinely achieved using a Solid State Detector (SSD). A way to improve
significantly this detection in term of dilution and discrimination of speciation is to use instead
a CAS to perform High Energy Resolved Fluorescence Detection (HERFD) acquisitions.
The CAS is constituted of 5 bent crystals, aligned to select the photons emitted by the sample.
The selected photons are then focused on a detector, which allows to count them (Figure 1).
The sample, the crystals and the detector are located on an experimental table, which can be
precisely aligned with respect to the incident X-ray monochromatic beam.
Figure 1. View of the 5-crystals CAS on CRG-FAME-UHD (BM16) beamline
The5 crystals has been designed and assembled by the FAME-UHD team at the Neel Institute.
The experimental table is manufactured by Symétrie (Nîmes, France) ; the table itself is CE
certified (Cf. §5 of the Vol. IV of the present CE declaration form).
Several apparatus are linked to the experimental table and the CAS. 4 pairs of slits (JJ X-ray)
surround silicon diodes which allow to measure the intensity of the photon flux. These two
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apparatus are under a primary vacuum ; Be windows are under the X-ray beam path. The
sample is positioned on a sample holder, not yet designed. The detectors used to collect the
photons selected by the CAS will be either a silicon drift detector (SII NanoTechnology) or a
hybrid pixel detector (imXPAD).
The scope of the CE certification concerns the crystal analyzer spectrometer and all the
elements around installed permanently. All these constituents are list on Table 1.
Apparatus Type Manufacturer
Crystal Analyzer Spectrometer
prototype 5-crystals spectrometer FAME / FAME-UHD
Detector arm * XYZ linear motions FAME-UHD
Bent crystals Si or Ge wafer on glass curved
substrate (Rcurvature : 0.5 or 1m) ESRF & XRS-Tech1
Detectors silicon drift detector SII NanoTechnology2 - Vortex EX 60
hybrid pixel detector imXPAD3 - Model XPAD S70
Experimental table * Steel honeycomb table on
precision positioning hexapod Symétrie4 ( )
Experimental slits large apertures slits under
vacuum JJ X-ray5 - Model : AT-C30-HV
Sample holder 3 (XYZ) linear & 1 rotation
motions Newport/micro-control
Incident and transmitted
beams intensities
measurement
Si diodes Hamamatsu6 - Model S3590-09
vessel FAME-UHD
Be windows Materion Brush Inc.7
Pico-amperemeter CAEN ELS8 - Model AH401D ( )
Table 1. Scope of the CE certification : constituents of the spectrometer and other apparatus linked to it
1 http://xrstech.com/ 2 now Hitachi High-Tech Science Corporation, http://www.hitachi-hightech.com/global/products/ 3 http://www.imxpad.com/ 4 http://www.symetrie.fr/ 5 http://www.jjxray.dk/ 6 http://www.hamamatsu.com/us/en/index.html 7 http://materion.com/ 8 http://www.caenels.com/
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3.1 Part 1 - Experimental table
3.1.1 Description
Functionally, the experimental table is used to place the sample in the X-ray beam (alignment)
and to keep its position on the sample constant during a monochromator energy scan
(measurement), the monochromator being a variable-exit one (Figure 2).
Figure 2. View of the motorized experimental table supporting the sample, CAS and detector
The positioning of the table is ensured by a precision positioning hexapod with high stability
(based on the standard system "Joran"). Six high resolution actuators (in black on Figure 2)
linked to high precision spherical joints allows to perform the different required motions
(Table 2).
The optical breadboard table itself is built by OPTA9 and integrated on the hexapode by
Symétrie. The main core is made in steel honeycomb, the top and bottom plates in magnetic
9 www.opta-gmbh.de
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stainless steel (thickness of these plates : 3mm). The entire table is made of two identical
tables (HDT 250/25). Size of each table is 1000x2000x250mm3. The entire table size after
junction will be 2000x2000x250mm3. The junction will be done along the Ytable axis (Table 2).
Motion Range speed
Xtable ± 50 mm ~1.10 mm/s
Ytable ± 60 mm ~1.10 mm/s
Ztable ± 100 mm ~0.90 mm/s
α ± 4° ~0.04 °/s
β ± 4° ~0.04 °/s
γ ± 4° ~0.06 °/s
Table 2. Experimental table motion specificities : range and speed (source : Final Design Review -
Symétrie 17/04/2015)
SYMETRIE control enclosure integrates a motion controller and DC power supplies. The
motion controller is based on a DeltaTau Geo Brick LV (Low Voltage) which includes the axis
control and amplifiers.10 The system requires a standard power supply (voltage : 110-240 VAC
– 50/60 Hz - Fusible 10A - power requirement <500W).
3.1.2 Safety in place / implemented protective measures
risk protective
measures
An emergency stop button, directly linked to the controller, allows
to stop all the experimental table motions
The system is equipped with a grounding connection.
10 http://www.deltatau.com/
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3.2 Part 2 - Crystal Analyzer Spectrometer
3.2.1 Description
Functionally, the spectrometer is used to align bent crystals in Bragg conditions with respect
to the probed photons energy (fluorescence or scattered). The detector is aligned to collect
the diffracted photons (in the Z direction) and to be around the focus point of the fans (in the
X direction) as shown on Figure 3.
Figure 3. Crystal Analyzer Spectrometer design : energy selection principle
Figure 4. 5-crystals FAME-UHD spectrometer motions
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Motion Number Range Speed Motorization
5-crystals spectrometer (prototype)
Xcrystals 5 ± 110 mm < 1mm/s B
Zcrystals 5 ± 5 mm < 0.1mm/s B
Zall crystals 1 ± 200 mm ~1mm/s B
tilt 5 ± 2° < 0.1°/s A
θ 5 ± 2° < 0.1°/s A
Detector Xdetector 1 ± 10 mm ~2mm/s
Ydetector 1 ± 10 mm ~2mm/s
Zdetector 1 ± 400 mm ~2mm/s
Table 3. Crystal Analyzer Spectrometer motion specificities: range, speed and motorization. A : Turbo Disc ESCAP P110-0.64-2.5 step-motor. B : MAE HY200 1718-0.9 step-motor. Documentations
linked to the motors can be found in the Vol. III of the present CE declaration form
3.2.2 Safety in place / implemented protective measures
All the motions are irreversible. Moreover, general emergency button are positioned all
around the experiment table (Figure 5).
risk protective
measures
The hutch emergency stop button allows to stop all the
experimental spectrometer motions
The system is equipped with a grounding connection.
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Figure 5. Safety elements around the experimental table : general emergency stop, emergency door opening, PSS hutch button and oxygenometer
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Part 3 - Helium bag
3.2.3 Description
Functionally, the helium bag is used to limit the absorption of the fluorescence photons on
the path sample - crystal - detector. Air is replaced by helium gas. The bag itself is made in
polyethylene. The bag is shown on Figure 6.
Figure 6. Helium bag
3.2.4 Safety in place / implemented protective measures
The main risk linked to the enclosure is the suffocation, due to a lack of oxygen.
If all the helium gas is suddenly dispersed in the hutch (strong leak). The internal volume of the
enclosure is estimated to 0.8 m3 from the 3D design software used for its conception. The
volume of the experimental hutch is 88 m3. The ratio volume of He / volume of air is below
2% : such leak won't change drastically the percentage of O2 in the hutch
If the helium gas is slowly dispersed in the hutch (small leak). The experimental hutch is
equipped with a O2 level detector, as well as an air extractor: if the percentage of O2 in the
hutch is below 19%, the corresponding alarm will be active. The He bottle which allows to fill
the enclosure will be located outside the hutch, it will be then possible to close it.
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3.3 Part 4 - Experimental slits, tubes, diodes & windows
3.3.1 Description
The different elements are shown on Figure 7. The different aims of this set-up are :
to define, to "clean" the monochromatic beam focused on the sample from any
unwanted signals, with the slits,
to measure the intensities of the beam (incident and transmitted), with the diodes,
to limit the absorption of the beam, all the path being under primary vacuum, with
windows transparent to X-ray and allowing the pumping such as Be windows.
Figure 7. General view, principle (left) and detail of the entrance slits & diodes block (right).
3.3.2 The slits
The slits are made by JJ X-ray. The model is AT-C30-HV, i.e. with a maximum aperture of 30mm
and High Vacuum compatible (even if they are going to be used under primary vacuum). Main
characteristics are gathered in Table 4.
Outside properties Dimensions 249 mm x 249 mm x 68 mm
Weight 6.1 kg
Blades & aperture
Aperture size Maximum: 30 mm x 30 mm
Minimum: Full Overlap
Speed Maximum 1mm/s
Nature 2 mm thick tungsten carbide
Motors & control-command
Motor type 2-phase stepping motor
Current 1.2A per phase
Electronic IcePap
Table 4. Slits main characteristics
Cf Volume IV of the present CE declaration, §2, for more details
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3.3.3 The diodes
The system used to measure the photon flux before and after the samples is an home-made
set-up. Two photo-diodes (Hamamatsu S3590-08) parallel to the beam collect the photons
scattered by a kapton foil at 45° (Figure 8). The currents created by the photo-diodes are
summed and measured using a pico-amperemeter (such as a Novelec, a Keithley...).
Figure 8. Measurement of the photons flux using Si diodes.
Outside properties Dimensions ~ 70 mm x 70 mm x 70 mm
Weight < 0.5 kg
Photo-diodes Active size 10 mm x 10 mm
Depletion layer thickness : 300µm
Current & measurement Typical current 1-100 nA
Electrometer As close as possible from the diodes
Table 5. Diodes main characteristics
Cf Volume IV of the present CE declaration, §6, for more details on the diodes
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3.3.4 The vacuum set-up & the windows
All the X-ray path (including the slits and the diodes) is under a primary vacuum on the
experimental table (Figure 7, right). The pumping is done using flexible plastic tube (Ø8mm
interior). Beryllium windows are used for the X-ray entrance and exit.
Tube Dimensions Ø 50mm
Pumping Typical vacuum 1-10 mbar
Safety bursting disk
Be windows Dimensions of the aperture 10 mm x 5 mm (HxV)
Thickness 25µm
Table 6. Experimental vacuum system & diodes main characteristics
The Be thickness (25µm) has been calculated by the furnisher (Materion) following the
aperture requests. The Be windows can only be mount ounce on the flange (Figure 9). After
the 1st use under vacuum the window is plastically deformed following the aperture
dimensions.
Figure 9. Be Window and its support
Cf Volume IV of the present CE declaration, §7, for more details on the Be
material
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3.4 Part 5 - Sample-holder
3.4.1 Description
The Newport multi-axis sample-holder is composed of
• 4 linear "x" stages, with their corresponding actuator
• 1 linear "z" stage, with their corresponding actuator
• 1 rotation stage
Figure 10. Newport sample holder
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3.4.2 Motions
Motion Name Range Characteristic speed
linear "x" stage TRech 25 mm 0.4 mm/s
linear "x" stage TLech 25 mm 0.4 mm/s
rotation stage Rech 360° 4 °/s
linear "z" stage Zech 12.7 mm 0.2 mm/s
linear "x" stage Yech 25 mm 0.4 mm/s
linear "x" stage Xech 25 mm 0.4 mm/s
Table 7. Description of the Newport sample holder motions
3.4.3 Aim of the sample holder
The aim of the sample holder is to align a sample 1) on the beam and 2) on the appropriate
position with respect to the Crystal Analyser Spectrometer.
3.4.4 Safety in place / implemented protective measures
All the motions are irreversible. The motorization are CE certified.
Cf Volume IV of the present CE declaration, §8, for more details on the sample
holder
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4 Assembly and Dismantling
This symbol refers to other pages or documents.
The PDF files are gathered on the Volume III (Drawings, calculation notes,
tests results, graph) of the CE certification
4.1 Part 1 - Experimental table
Assembly of the experimental table will be done on-site by the manufacturer (Symétrie). The
table will be bring at ESRF in different parts (Figure 11) :
the fixed platform (hexapod's attachment), on the floor,
the 6 actuators,
the mobile platform.
Only qualified person from ESRF handling group in collaboration with supplier of the machine
with the external hall crane will perform handling. Supplier (attachment point, number,
position vs. centre of gravity) has defined handling procedures at designed phase. The
procedure for the assembly is described on Table 8, the synoptic for the cabling of the
actuators on Figure 12.
The first tests will be done by trained operators (the supplier) using personal protective
equipments.
Use of solvent (ethanol) to clean several part before assembly will be done with
limit quantities and only in well-ventilated space. Use of masks and gloves,
respect Material Safety Data Sheet
Figure 11. Main constituents of the experimental table
Figure 12. Synoptic of the experimental table cabling
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Obligations &
residual risks item
Implantation of the fixed platform
The fixed platform (hexapod's
attachment) will be installed in the
hutch with the crane, aligned on the
hutch (X,Y, horizontality)
Fixation of the fixed platform on the floor
Holes will be drilled in the floor in order
to position "inserts" for the fixation Cf. Vol. IV §9.3
Stability and fixation of the fixed platform
butyl / nitrile type gloves
A 2-component, solvent free, epoxy
resin will be injected in order to fill all
the free spaces between the floor and
the fixed platform.
Cf. Vol. IV §9.1
Positioning of the six actuators
All the actuators components will be
assembly at the manufacturer's site
and installed manually on the
hexapod's attachment (individual
weight : 25.7 kg).
Implantation of the mobile platform
The mobile platform will be brought by
the external crane and positioned on
the actuators. The total weight of this
part is lower than 850kg. Metallic
elements will be positioned between
the platform and the floor to avoid
crushing (right figure).
Cf. Vol. IV §9.2
Cabling and DC power supply
Cabling will be made at the
manufacturer's site. Use of different
kind of connectors will avoid any error
during connection. The controller will
be switch off during connection.
Figure 12
Cf. Vol. IV §9.4
Table 8. Step-by-step procedure for the assembly of the experimental table
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4.2 Part 2 - Crystal Analyzer Spectrometer
Experimental table - CAS interface
All the actuators of the hexapode table needs to be in compression. To eliminate any risk of
tipping, all the possibilities of installing the various apparatus (CAS, detector arm, slits...) on
the table have been studied by Symétrie. In all the case the actuators are in compression,
there is no risk of tipping.
Cf Final Design Report of the experimental table, p.10-11
Moreover, in the improbable case where an actuator is no more in compression (positioning
of overweight apparatus on the table for example), each actuator junction is equipped with
metallic parts with avoid any dislocation (Figure 13). The table cannot operate correctly but
there is no risk of tipping.
Figure 13. Anti-dislocation ring for the actuators. Each of the 6 actuators is equipped of 2 rings
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5-crystals Crystal Analyzer Spectrometer mechanical assembly
5-crystals CAS machinery has been designed in several constituents in order to facilitate its
handling and assembly (Figure 14). The complete spectrometer assembly will be done on-site,
using the internal crane installed in the experimental hutch (max. support weight: 500kg).
Use of solvent (ethanol) to clean several part before assembly will be done with
limit quantities and only in well-ventilated space. Use of masks and gloves,
respect Material Safety Data Sheet
Figure 14. Schematic view of the assembly of the different constituents of the entire spectrometer
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Obligations & residual risks
item
Basis of the spectrometer (1st element on Figure 14)
This part will be installed and aligned on the table as a
reference Weight : 10kg
Mounting angle (2nd element on Figure 14)
Weight : 50kg
Mounting angle support (3rd element on Figure 14)
Weight : 15kg
Crystal angular and horizontal linear motions (4th element on Figure 14)
Weight : 5x2kg
Table 9. Step-by-step procedure for the assembly of the spectrometer
Crystal Analyzer Spectrometer cabling and control command
The control command of the spectrometer is achieved :
using commercial Wago electronic controller system
with standard control command software
Cf Volume III of the present CE declaration for more details on the controller
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4.3 Part 3 - Helium bag
The helium bag is prepared following the instructions given in the Vol. 3 of the present CE
declaration form. It has to be connected to the He bottle using the different elements given
on the figure (Figure 15). The procedure to fill the helium bag is given on Table 10.
Figure 15. Helium bag gas connection.
Figure 16. Helium bag on place
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Obligations & residual risks
item
connect all the elements following the appropriate instructions (see Figure 15).
ensure that the pressure limiter and the
flowmeter are closed →
open the He gas bottle
open the pressure limiter in order to have a pressure at the exit of the limiter ~2 bars
open the flow meter in order to have a flow rate around 0.1 - 0.2 l/min →
when the helium bag is full, fit it between the sample, the crystals and the detector (Figure
16)
adjust if necessary the flow meter : the helium bag mustn't be under pressure →
Table 10. Step-by-step procedure for the assembly of the helium bag
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Obligations & residual risks
item
close the He gas bottle
close the pressure limiter in order to have a pressure at the exit of the limiter ~0 bars
disconnect the flexible tube at the flow meter level
Connect the He bag flexible tube to the experimental gas recovery tube (left) →
Open the experimental gas recovery valve (right) →
Table 11. Step-by-step procedure for the dismounting of the helium bag
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4.4 Part 4 - Experimental slits, tubes, diodes & windows
Mechanical assembly
Like for the CAS machinery, the slits & diodes set-up has been designed in several constituents
in order to facilitate its handling and assembly (Figure 17). The complete assembly will be done
on-site, using the internal crane installed in the experimental hutch (max. support weight : 500kg).
Figure 17. Schematic view of the assembly of the slits, diodes & windows (x2)
Obligations &
residual risks item
Basis (1st element on Figure 17)
This part will be installed and aligned
on the table as a reference 17kg
Slits and central diodes (2nd element on Figure 17)
The initial assembly (2 pairs of slits
surrounding the diode) will be done in
the workshop.
Weight : 12kg
2nd diode and tubes (3rd element on Figure 17)
<1kg
Windows (4th element on Figure 17)
See next § for more details <0.1kg
Table 12. Step-by-step procedure for the assembly of each slits & diodes set-up
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Mounting of the Be windows on the flange
The procedure to mount / unmount the Be windows is the following (Table 13).
Obligations &
residual risks item
Unmount the flanges from the support
The flanges are fixed with 8 CHC
bolts
Remove the safety tape "Follow the user manual to unmount the Be window"
The tape is here to avoid any
unmounting without being aware of
all the details of the procedure
Remove the upper flange and the Be window
butyl / nitrile type
gloves
On a flat working surface, remove the
bolts from the upper flange (1) then
the Be window using a flat Brucelle
plier (2).
This Be window has to be store in an
appropriate labelled container and
can not be used again
Clean the upper and lower flanges
butyl / nitrile type
gloves
Clean the surfaces in contact with the
Be window using a soft tissue, the
upper flange and the lower flange
with the Viton ring. Do not use any
solvant.
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Installation of the new Be window
butyl / nitrile type
gloves
On a flat working surface, install the
new Be window using a flat Brucelle
plier on the lower flange with the
Viton ring (1), position the upper
range (2) screw the bolts on the
upper flange (3). It is not necessary to
screw strongly the bolts.
Position the safety tape "Follow the user manual to unmount the Be window"
The tape has to be positioned on both
flanges
Mount the flanges on the support
Table 13. Step-by-step procedure for the assembly of the Be windows
Beryllium windows
→ put the protec�ons on both Be windows before any operation
Nitrile gloves must be worn, even if the Be window doesn't have to be touched
directly
Slits control command
The control command of the slits is achieved :
using Icepap electronic
with standard control command software
Cf Volume IV of the present CE declaration, §2, for more details on the slits
cabling
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4.5 Part 5 - Sample-holder
Mechanical assembly
Figure 18. Newport sample-holder vertical dimensions
Motion Name Stage weight Actuator weight
linear "x" stage TRech 0.3 kg 0.1 kg
linear "x" stage TLech 0.3 kg 0.1 kg
rotation stage Rech 0.3 kg Includ. in stage
linear "z" stage Zech 3.2 kg Includ. in stage
linear "x" stage Yech 0.3 kg 0.1 kg
linear "x" stage Xech 0.3 kg 0.1 kg
total 5.1 kg
Table 14. Newport sample-holder weight
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The sample-holder mechanical assembly has been done by Newport. Its limited weight allows
to install it already mounted on the experimental table.
Cabling and control command
The control command of the sample-holder is achieved :
using Icepap electronic
with standard control command software
risk protective
measures
The system is equipped with a grounding connection.
Switch-off the motor power supply before plugging / unplugging
the connectors. This operation must be done by training staff
Cf Volume IV of the present CE declaration for more details on the sample-holder
cabling
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5 Use
Two user modes are described.
User mode 1, during operation of the beamline by external users and by the staff.
User mode 2, during alignment and preparation of the experiment by the staff.
Any other use of the equipment is considered as non compliant.
5.1 User mode 1 - Operation mode
5.1.1 Sample positioning
The sample is installed on a dedicated sample holder (Figure 19; picture on the left). Access to
the sample holder is free from any apparatus (Figure 19; left). Sample height is moderate and
its position with respect to the edge of the table (50cm, Figure 19; right) allows to position the
sample without use of stepladder. The users must follow the path described on Figure 19 (Blue
arrow) to reach the sample positioning area.
Figure 19. Sample positionning
Beryllium windows are located close to the sample-holder
→ put the protec�ons on both Be windows before any operation
The space around the sample is limited : access around it is limited to one operator
during sample change / priority is given to operations from remote station
It is forbidden to sit on the experimental table during sample positioning
Potential risk : crushing, bumping, stumbling
→ keep path free, no cables pipes equipment or tools on floor
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The procedure here described is adapted to ambient conditions measurements using
the dedicated sample-holder. Using of another sample holder system such as a
cryostat, an high pressure - high temperature vessel or another in situ set-up must be
done after carefully reading of the associated documentation
5.1.2 Making the hutch search
The hutch search has to be done following the rules of the ESRF user safety training.
1) Start search on PSS
2) Enter the hutch and follow the green path (Figure 20), , verify that no one is in the
hutch, and press the search button.
3) Close door 1 end press final search
Figure 20. EH1 hutch search
Potential risk : crushing, bumping, stumbling
→ keep path free, no cables pipes equipment or tools on floor
The complete procedure is described in the ESRF user safety training followed by each
user before using the beamline
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5.1.3 Sample alignment
All these operations will be performed from the control-command hutch. The procedure is the
following (Figure 21):
Alignment of the sample on the incident beam (Figure 21 a):
This alignment can be done in transmission mode, to determine which part of the
sample will be analysed,
The alignment is done both in Y and Z directions.
Alignment of the sample with respect to the spectrometer (Figure 21 b):
This alignment will be done in fluorescence mode,
The alignment is done only in X direction.
Figure 21. Procedure for the sample alignment, on the incident beam (a) and with respect to
the CAS spectrometer (b)
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5.2 User mode 2 - Expert mode or experiment preparation mode
5.2.1 Helium bag operations
The helium bag allows to limit the absorption of X-ray by air in the path sample - crystal -
detector (Figure 6). The bag doesn't include the crystals, the sample and the detector. It is
possible to change the crystals, to change the detector... without removing the bag or at least
without removing the helium from the bag.
Potential risk : lack of oxygen
→ do not use sharp objects close to the helium bag
5.2.2 Crystal change
The crystals of the spectrometer need do be adapted to the selected photons energy. The
crystal change will be done by the beamline staff, between each user's experiment.
The crystal support (Figure 22, left) has been designed in order to mount / unmount it without
any tool (Figure 22, right). The minimum height of the crystals is 1.3m for the lower row, 1.5
for the upper one
Figure 22. Left : backside of the crystal support. Right : example of crystal change on BM30b (with a 5-crystals spectrometer)
Crystals can be changed only by trained staff. The procedure to change the crystal is the
following:
position of the crystals at the minimum height,
venting of the enclosure if necessary following the appropriate procedure,
opening of the side windows,
change the crystals using the most appropriate windows depending on their position.
Nitrile gloves must be worn, even if the crystal surface mustn't be touched directly
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5.2.3 Crystal alignment with laser
The angular alignment of each crystal will be done firstly using a laser beam (Figure 23). The
laser beam will go from the sample to the middle of each crystal, its reflection should be
located on the detector. This alignment will be done
during the first initial tests,
after a major maintenance of the spectrometer.
The procedure is the following
position of the beam on the sample is marked using photo-sensitive paper (such as
"pink paper", Kodak Linagraph Direct Print paper),
a white screen is put on the detector detection area,
a class 2 laser is aligned in order to represent the photons path emitted by the sample
and incident on the middle of the crystal,
the and tilt angles are optimized to have the laser spot on the detector.
Figure 23. Crystal alignment using laser
Laser beam - Class 2
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5.2.4 Crystal alignment with the X-ray beam
The angular alignment of each crystal will be done secondly using the X-ray beam. A reference
containing a huge amount of the probed element is located at the sample position (Figure 24).
The reference has to be:
a metallic reference, a filter... The amount of the element of interest mustn't be a
limited factor
as thin as possible, in order to define precisely the interaction "point" between the
incident beam and the sample.
The procedure is the following:
Optimization of the first crystal
choose the 1st crystal to optimize and change the Bragg angle of the others (crystal +
0.3°), in order to be sure that the others crystal won't contribute to the signals,
choose the incident energy in order to excite the selected electronic level, in order to
be "after-edge" :
Energy (RXmono) > Energy (Edgeelement)
optimize the position of the crystal, in x, z, and tilt, and of the detector, in x, y and z
check the optimization by doing an elastic-peak, i.e. by scanning the energy of the
incident photons around the energy of the selected fluorescence photons:
Energy (RXfluo) - 10eV → Energy (RXfluo) + 10eV
the main information given by the elastic peak at this level is the energy of optimization
(which is around the tabulated energy of fluorescence):
set positions spectrometer @ positions Energy (optimization)
set 1st crystal and tilt 1st crystal @ 0°
positions of the detector and position in z of the spectrometer are the same for all the
crystals and mustn't be changed now.
Optimization of the other crystals
change the Bragg angle of the optimized crystal ( 1st crystal + 0.3°), tuned the Bragg angle
of the 2nd crystal ( 2nd crystal - 0.3°)
choose the incident energy in order to excite the selected electronic level, in order to
be "after-edge" :
Energy (RXmono) > Energy (Edgeelement)
optimize the position of the crystal, in x, and tilt
adjust the incident energy at the energy of optimization for a fine tune in )
Energy (RXmono) = Energy (optimization)
optimization
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check the optimization by doing an elastic-peak, i.e. by scanning the energy of the
incident photons around the energy of the selected fluorescence photons:
Energy (RXfluo) - 10eV → Energy (RXfluo) + 10eV
set positions spectrometer @ positions Energy (optimization)
set 2nd crystal and tilt 2nd crystal @ 0°
repeat the procedure " Optimization of the other crystals" for all the crystals
Final check
all the crystals are tuned: all crystals = 0°
check the optimization by doing an elastic-peak, i.e. by scanning the energy of the
incident photons around the energy of the selected fluorescence photons:
Energy (RXfluo) - 10eV → Energy (RXfluo) + 10eV
in addition to the value of the energy of optimization, the elastic peak will give the
energy resolution of both the beamline and the spectrometer.
Figure 24. Crystal alignment using X-ray
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5.2.5 Detector change
The detectors linked to the spectrometer need do be adapted to experiment requirements.
For example:
a Silicon Drift Detector allows to discriminate in energy the diffracted photons from
the scattered ones, but the detection area is quite limited,
a Hybrid Pixels Detector allows to measure large diffracted fans, but it is not (or poorly)
energy resolved.
The detectors change will be done by the beamline staff, between each user's experiment.
The procedure is the following:
Change the height of the detector to its low position, from the control-room,
Switch off the electric power linked to the detector following the associate procedure,
Unplugged the detector,
Put the protection on the detection window,
Unmount the installed detector using the appropriate tools,
Mount the new detector using the appropriate tools,
Plugged the detector,
Switch on the electric power linked to the detector following the associate procedure.
Potential risk : electric
→ Turn off the devices before establishing any connection
→ This operation must be done by training staff
Potential risk : Beryllium by breaking Be windows for the SDD detector
→ Put the protection before any manipulation
More details on the detectors can be found on the Volume IV of the present CE declaration form.
5.2.6 Slits vessel venting
The venting of the vessels is simply done on the primary pump
Switch off the pump using the electrical switch
Open the venting valve on the pump
Potential risk : explosion
→ do not plug any pressurized system on the venting valve
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6 Annex
6.1 Annex 1: CE plate
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6.2 Annex 2: CE declaration
Recommended