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X-ray Absorption Spectroscopy at SESAME

“BASEMA Status”

Messaoud Harfouche

Synchrotron-light for Experimental Science and Applications in the Middle

East 

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Answers to Previous Questions and suggestions

• What is the vision for BASEMA BL– Focus on the XAFS techniques (XANES, EXAFS, XRF, XRD)– Need to meet user demands– Beamline scientist can propose different techniques that can be

combined with XAS• RAMAN is the widely used technique and maybe the cheapest • XES, HERFD, RIXS are the most advanced techniques but very expensive and

needs special design (can’t buy as a complete system)– Need multitude of bent crystals (larger is the number better are the results)– Need different type of crystals to cover all the energy regions

– Priority should be given to build a strong XAS user community• Need to connect with universities in the region (not that easy)

– SESAME should offer joint positions with universities (home universities ) to beamline scientists

– Sign MoUs with universities and research institutions– ……..

• Need to encourage scientists to develop their own research and allow collaborations among the members and other countries.

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• Modify the DCM to use MCM & Easy exchange by users– The DCM doesn’t allow motorized crystal exchange lots of time to

change the crystals need mechanical & vacuum technicians– Gain in flux but loss in resolution can’t be used for most of EXAFS

measurements– Flux on the sample is good enough even at higher energies - ~30

keV- if good detectors are used.– Cost of such a modification is very high (according to Ricardo Seniorato

Bruker ‘former Accel’)

Answers to Previous Questions and suggestions

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• A future upgrade of beamline to use KB focusing system to achieve 3x3 mm2

– Ray tracing calculations already performed– Beam size from the source is too large difficult to focus– Smallest beam size that can be achieved is 8 x 10 mm2 with a flux of 5

x 109 ph/sec at 8 keV– The option of short beamline is excluded

• need a small intermediate source point with small demagnification

– Smaller is the beam size - lower is the flux on the sample– Project for a micro-focusing beamline on insertion device (Undulator)

can be proposed for phase II beamlines (to be proposed by potential users)

Answers to Previous Questions and suggestions

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• What makes a good beamline? Stability and Low noise are key factors!– Beamline scientist totally agree on this proposition – It is a practical matter rather than calculations and design issue

• Need to minimize the number of motorization and disconnect the non used ones.

• Find a system that allows to disconnect a motor remotely and make it passive as soon as it is not used.

• Find the adequate solution for internal and external cooling system. • Use insolating material between the ground and girders for the optics

components• Other tricks can be collected from experts – starting from SAC/BAC

Answers to Previous Questions and suggestions

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• Being competitive by having reliable and impressive software – data acquisition and control software

• A sketch (Mock-up) of the data acquisition software is already done • See the demonstration version • Will be discussed with control group• Need a very good physicist who is a good programmer or a very good

programmer and good in physics.

– Data reduction and analysis • Many software are developed

– Ifeffit , WInXAS, XAFS, EXAFS pour le mac, PyMCA, fit2D, Match, etc.– Some have active mailing list and provide help for the users.

• Users are free to use there own software

Answers to Previous Questions and suggestions

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Other Comments

• Opening of the boxes from ESRF– On going (with many delays)

• Monochromator has been opened and inspected in presence of an expert (A. Simionovici)– Visual inspection (internal, external)– Testing of stepper motors, cooling and vacuum system– Could not test all the motors and signals (No control hardware)

• Other beamline components are in testing phase – XBPM, Slits, Wire monitor

• The opening of the VCM mirror is delayed until receiving the second mirror VFM– Metrology tests are already done at ESRF (thanks to Amparo Vivo)– Need an expert who worked with ZEISS mirror mechanisms (Eric Detonna, ESRF)

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Other Comments

• Budget estimation of the control system– Discussed with 3 beamline scientists from SOLEIL

• SAMBA, DiFabs, ODE

– The average construction budget for a beamline at SOLEIL was given by the control group (Pascale Betinelli + Yves-Marie Abevin)

– Will be shown in details at the end of this presentation

• Annual upgrade budget– Not needed at this stage of the construction

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Raman technique will be a good technique to be combined

with XAFS, XRF and XRD

Need for a cryojet or cryostat for biological and some

environmental samples. Needs for users will be submitted as proposal through EUC or directly to BL

scientist

Should focus more on building the users community which

leads to scientific collaborations between users

A large beam is needed for bulk measurements and 10x10 mm2

is a good beam size for many applications.

Users recommendations and wishes

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BASEMA

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Current Status of BASEMA

CDR has been written and ready to be reviewed TDR has been started

3D drawing of all the components is ongoing (Akrum) Inspecting, testing and documenting the optics

components Research vision for the beamline (preparing students,

collaborations)

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BASEMA

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BASEMA Port D08

Booster

Storage ring

Beamline

by Adel Amro

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Machine:

1011

1012

1013

1014

1 10 100

SESAME (400 mA)

SLS (400 mA)

SOLEIL (400 mA)

ESRF (100mA)

Flu

x [P

hot

ons/

sec/

0.1%

bw

]

Photon Energy [keV]

Can’t go to higher Energies due to the machine performances

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Beamline Characteristics

1011

1012

1013

1014

1 10 100

SESAME (400 mA)

SLS (400 mA)

SOLEIL (400 mA)

ESRF (100mA)

Flu

x [P

hot

ons/

sec/

0.1%

bw

]

Photon Energy [keV]

Parameter Unit ValueSource (BM) T 1.45

Hor. acceptance mrad 3

Vert. acceptance mrad 0.6

Energy range keV 4 – 30

Energy resolution - ~ 10-4

Photon flux (S1) Ph/sec 2x1012 (8keV)

Beam size (S1) mm2 ~0.1 x 0.1

Beam size (S2) mm2 8x10

Photon flux (S1) Ph/sec 5x109 (8keV)

Lower limit due to absorption of air in the EH Higher limit due to machine limitation

Energy range

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Spectral energy range (~4 –30 keV)

It will be hard to probe some elements at very lower concentrations

: K- edge: L- edge

: Difficult

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Control racksOptics Hutch

Control room Experimenta

l Hutch

Optics Hutch

Control room Experimenta

l HutchControl racks

Lab.

Beamline Hutches

NEW

OLD

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Control racksOptics Hutch

Control room Experimental

Hutch

Hutches & Optics Layout

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Beamline Optics

VCM VFM

Still at ESRF: to be delivered with BM16 comp.

Arrived at SESAME:will be opened once VCM arrived

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Beamline Optics

13 points evenly spaced by 50.8mm are measured on each strip

Surface Roughness

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Averaged rms valuesVCM

VFM

Beamline Optics

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Beamline Optics

Micro-roughness RMS distribution on VCM stripes

Pt Si

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Micro-roughness RMS distribution on VFM stripes

Pt Si

Beamline Optics

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LTP measurement VCM (Slope error)

Pt

Si

Beamline Optics

bender performances were not checked

Slope errors correspond to residuals to the best cylinder Three parallel traces spaced by 15 mm are measured on each stripe

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LTP measurement VFM (Slope error)

Pt

Si

Beamline Optics

bender performances were not checked

Slope errors correspond to residuals to the best cylinder Three parallel traces spaced by 15 mm are measured on each stripe

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Element Transmitted Power (W)

AbsorbedPower(W)

Abs. PowerDens.(W/mm²)

Prim slits 108.8 - -

Be 250 µm 78.1 30.7 0.17

M1 mirror 33.6 26.0 0.0009

1rst crystal (23°) 0.003 33.6 0.11

Element Transmitted Power (W)

AbsorbedPower(W)

Abs. PowerDens.(W/mm²)

Prim slits 108.8 - -

Be 250 µm 78.1 30.7 0.17

M1 mirror 51.9 7.6 0.00026

1rst crystal (23°) 0.003 51.9 0.18

Heat load absorption and power density on VCM

Si

Pt

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Without cooling With cooling

Beamline Optics

Thermoelastic calculations (FE)

Power density calculated on the surface of the Si coated

stripe of the VCM

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Beamline Optics

DCM

ROBL DCM at ESRF Arrived to SESAME Opened in presence of an expert (A. Simionovici)

Discussions and decisions: Use the current set up of cooling system for whole period of commissioning

Mount the bender for the second crystal once we have beam through optics to experimental hutch

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Stepper motors

Beamline Optics

Tests on the DCM

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Beamline Optics

Tests on the DCM

Cooling System

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Beamline Optics

Tests on the DCM

Cooling System

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Beamline Optics

Tests on the DCM

Vacuum System

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Beamline OpticsProblems encountered

Vertical motors can’t be mounted (need to be fixed on the floor)

Some Controllers still at ESRF for pico- and servo-motors

No controller at SESAME

Drops were observed on the first crystal

Contacted optics groups at ESRF, APS

Need to find a way to clean them

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Beamline Optics

Other Components All the components from ESRF were unpacked Except the VCM Test is ongoing for the motors and motor controllers Cooling and vacuum will follow soon

Tested components will be covered and stored in the Lab. Primary alignment of the components will be done at the end

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E (keV) Mirror angle(mrad)

N (ph/s)

E (eV)

Size( HV mm)

Div.(HV mrad)

3rd order

5 (a) 3.2 mrad 2.41012 0.63 0.550.25 2.910.28 3.1107 (1.3X10-5)

5 2.8 mrad 2.21012 0.64 0.550.24 2.920.25 1.3108 (6.0X10-5)8 2.8 mrad 2.81012 1.07 0.560.25 2.910.25 2.5105(8.9X10-8)12 2.2 mrad 1.81012 1.83 0.550.24 2.910.20 6.0103(3.3X10-9)

E (keV) Mirror angle(mrad)

N (ph/s)

DE (eV)

Size(HV mm)

Div.(HV mrad)

3rd order

14 2.8 2.41011 0.92 0.540.24 2.910.25 2.7104 (1.1X10-7)

18 2.8 1.41011 1.49 0.540.23 2.850.24 -

24 2.8 4.51010 2.66 0.540.25 2.700.24 -

30 2.2 1.71010 4.22 0.560.25 2.500.19 -

Optical properties at the sample positionSi(111) crystal

Si(311) crystal

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Optical properties at the sample position

Number of photons on the sample (S1)

without focusing system (KB)

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Sec. slits N (ph/s) DE (eV) Size (µm HV) Div (mrad HV)

Fully open1.41012 1.06 54 x 23 2.231.18

10050 µm 4.9109 1.04 7.5x9.7 2.101.12

Optical Element

Distance (m)

Demagn.

S1 – VFM (P) 2.92

VFM – S2 (q) 0.58 1/10

S1– HFM (p) 3.18 1/6

HFM – S2 (q) 0.32

KB parameters from secondary source

KB Focusing system

Ray tracing simulation results

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KB Focusing systemSecondary source (S1 sample) Focused beam (S2 sample)

8x10 mm2

~5x109 Ph/sec

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  Materials Costs (M$)Interface (hutches and infrastructure) 0.50Front End 0.15Beamline Optics 0.49 o XBPM 0.10o Crystals for DCM 0.04o Modifications on the existing optics 0.10 (if needed)o Focusing system (KB+microscope) 0.25 (To be discussed)

Vacuum System 0.03

Computing and Control System 0.40Hardware (PCs, VME, drivers,…) 0.3Software and DAQ 0.1Furniture End Station 0.51Tables (2) 0.12Detectorso ICs, diodes and gas mixing system 0.04o SDD (1) 0.05o Multi-element Ge detector 0.30 (promises for 7e Ge detector S.H.)

Total costs with focusing system 2.08Total costs without focusing system (-0.25) 1.83

Estimated Costs

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Task Start End

Conceptual Design Report (CDR) 2011 November, 2012

Technical Design Report Design Report Final Design Report

December, 2012July, 2013

Jun, 2013November, 2014

Lead procurement December, 2014 May, 2015

Components modifications and procurement January, 2015 September, 2015

Installation May, 2015 October, 2015

Control Integrating and testing Jun, 2015 December, 2015

Commissioning (depending on machine) January 2016 July, 2016

Proposals for expert users April, 2016 -

Accepting Expert Users July, 2016 October, 2016

Proposals for beamtime (all users) September 15, 2016 -

Users at bemlline January, 2017 -

Estimated Time Schedule

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Other ActivitiesIAEA Coordinated Research Project (2 proposals)

  Adsorption and mobility of heavy metals in soils in the vicinity of      Jordanian- and Yarmouk- rivers  (SESAME project)

  Antimony as an element with environmental concern and its pollution in Mongolia collaboration  project between SESAME, Jordan  and The Institute of Chemistry and Chemical Technology, Mongolia

Accepted proposal for joint SESAME/ICTP School  Advanced School on Synchrotron Techniques in Environmental Scientific projects

SESAME-ICTP 

Co-supervising a Master Student from Al-Quds University Upgrade of BASEMA “the XAFS/XRF Beamline at SESAME” and application to a scientific 

case 

Co-supervising a Master Student from Jordanian Uniersity Heavy metals in the vicinity of Jordanian and Yermok rivers soils

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Acknowledgement Andreas Scheinost (ROBL, ESRF) Amparo Vivo (metrology Lab., ESRF) Alexander Simionovici (Univ. Josef Fourier and ESRF)Thiery Moreno (SOLEIL, France)

A. Amro, T. Abu Hanieh,Y. Moumani, F. Al-Omari, A. Attyeh,

SESAME StaffM. Shehab M. Al-Najdawi, S. Budair, O. Noor, M. Al-khalilietc.