fame-uhd experimental station 5 crystals crystal analyser ......fame-uhd experimental station - user...

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

FAME-UHD experimental station - User instruction - CE certification vol. I

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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


Part 3 - Helium bag ..................................................................................................................... 15

3.2.3 Description ................................................................................................................ 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


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


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



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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


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.


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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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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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


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


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


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


risk protective

measures


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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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°




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