Status of the crystallography beamlines at...
Transcript of Status of the crystallography beamlines at...
A. Lausi
Status of the crystallography beamlinesat Elettra
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin •2
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
Photon sources at Elettra
1015
1017
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1021
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1025
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Pea
k B
rilli
ance (
Pho
tons/s
/mm
2/m
rad
2/0
.1%
bw
)
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Photon Energy (eV)
0.11101001000
Wavelength(nm)
U5.6
13
5U12.5
FEU
W14.0
SCW
Short W15.0
Short U5.61
3 5
Bending Magnet
EUFELE
100 nm
40 nm10 nm
Elettra
E=2 GeV
I=400 mA
FERMI
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
1995-2006:XRD beamline
macromoleculesbut also material science, high pressure, fibers, inorganic crystals...
Diffraction at ELETTRA
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Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
HRD(1) diffraction beamline (1995 version)
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source
slits
monochromator
refocussing mirror
sample stage
filter
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
XRD1: present and future
General purpose X-ray beamline with a extended spectrum(4-21 keV)
from a wiggler source, shared with the SAXS BL. The BL hosts PX and
material science experiments, in collaboration with CNR.
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
• Top-up mode introduced serious thermal load problem affecting the BL
monochromator. Three water direct-cooled crystals already substituted
in the last three years. This was reflected in a reduced (total) flux and
enlarged spot size, causing problems both with users and industry (long
exposure time, and beam divergence in particular).
XRD1: present and future
A closed loop cryogenic system (liquid nitrogen) from Bruker has been purchased and is expected to be tested by the early 2015.
XRD1 is expected to be up and running at full capacity at the beginning of 2015.
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
Structural biology lab
Molecular biology
Large scale proteinexpression
Protein purification
Protein characterisation
Biophysical analysis
Biochemical analysis
Crystallisation
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Recombinant proteins are fundamental “reagents” for basic and applied bioresearch. Obtaining pure and folded proteins is usually a bottleneck in biological studies.
The PROTEO protein factory
Construct Design Multiple Cloning Test Expression Purification SCALE UP
X-Domain Y-Domain
PCR
Thanks to an INTERREG grant we have established a biotechnological platform that provides a specialized support to express and purify recombinant proteins for functional and structural studies. We implemented a multistep process to go from gene to protein with high efficiency using multiparallel protocols in bacteria, insect and mammalian cell expression systems
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Tecan liquid handler robotic platform for High Troughput cloning & small scale purification
2 Sartorius Certomat BS-1 orbital shakers to grow bacterial cells
5 Sartorius fermentors for controlled expression in prokaryotic and eukaryotic cells, including 2 Biostat B (2L), 2 Biostat C (10L) and oneCultibag 20/50 RM (50 L).
4 Akta FPLC with column fleet for chromatographic protein purification
Suite of centrifuges (Beckmann Allegra 22R, Allegra 64R, AvantiJ-26XP) with rotor fleet
Spectrophotometers & gel imaging system (ImageQuant)
Expression & purification facilities
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
Molecular biology lab
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Bacterial protein expression
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Liquid handler Tecan EVO Freedom 150 for re-formatting commercialcrystallization screens and setting up crystallisation plates
TTP Labtech Mosquito nanoliter crystallization robot to set up 50-100nLcrystallization drops
Explora Nova Xtal Focus system for automatic crystal imaging and remote monitoring of crystallization experiments
The facility has been designed to be open for external users. Users will be able to bring/send purified protein samples, set up a variety of commercial crystallization screens, and monitor the results of the experiments in remote, through a web-based system.
The crystallization suite
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
Crystallization lab
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
2009 - Present:MCXnew XRD1
currently in construction:XRD2 cluster
BM 7.1
Beamline designed for non single crystal diffraction experiments
Open to users since 2009
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
Before MCX: “Powder Diffraction Facilities at ELETTRA”
• Powder in capillary on XRD1 area detector
(Si powder @ ~18 keV)
• Fit2D to integrate rings
• Resolution limited by spatial response of detector and by sample dimensions
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Diffraction analyses
Phase identifications
Texture analysis
Phase transitions
Crystal structure determination
Crystal structure refinements
Quantitative phase analysis (and crystallinity determination)
Microstructural analyses (crystallite sizes - microstrain)
Residual stress analysis
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Design Guidelines
• High-flux tuneable source with a wide spectral range,
(6-12 keV)
• Possibility to extend the
• Flexible optics– line focus (10 x 1 mm2)
– point focus (1 x 1 mm2 and below)
• Accommodate large volume samples
• Use of different detectors
• Sample temperature control
• User-friendly software
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Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
1010
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Photo
ns/
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%bw
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Photon Energy (eV)
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Photo
ns/s
67891
2345678910
l (Å)
ELETTRA operated at 2.4 GeV, 200 mAbending magnet spectral fluxFlux at the sample (Air environment)Flux at the sample (He environment)
MCX optical design : source
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Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
1010
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ns/
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2 3 4 5 6 7 8 9
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Photon Energy (eV)
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1012
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Photo
ns/s
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2345678910
l (Å)
ELETTRA operated at 2.4 GeV, 200 mAbending magnet spectral fluxFlux at the sample (Air environment)Flux at the sample (He environment)
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MCX optical design : source
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
• High-transmission Filter-window assembly
• Collimating Pre-mirror
• Wide range monochromator with II crystal bender for dynamical sagittal focusing
• Bendable focusing mirror
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MCX optical design : outline
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Sagittal Focussing
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Grazing incidence reflection optics:• geometrical loss • small acceptances• difficult to manufacture• expensive
bent II crystal
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long 2nd crystal movement capability allow for the wide energy range
The Elettra Hard X-ray Monochromator
E. Busetto, I. Cudin, G. Fava
R. Borghes, G. Cautero
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The Elettra Hard X-ray Monochromator
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Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin Anrea Lausi The CX project… 25
Front-end Hutch
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First mirror
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0.5 µrad slope errormeasured on the ElettraLong Trace Profilometer
First mirror
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0.65 µrad slope error
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From the Optical to the Experimental Hutch
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Experimental Station
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Experimental Station
4 circle diffractometer(0.0001° precision in 2θ)
XYZ translation stage
Recieving slits
Analyzer crystal / scintillatordetection system
Hot air blower (up to 1273K)
Cryo stream (down to 100K)
Laser sensor for accurate sample positioning
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General User Interface
Control system based on pyton
General command interface for:• driving motors
• theta-2theta scan
• multiple theta-2theta scans
• single or two motor scan
• multiple scans
• monochromator functions
• calibration functions
• warnings management...
• ...
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Experimental Station
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Experimental Station
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Instrumental profile (capillary)
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Instrumental profile (flat plate)
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Instrumental profile (capillary)
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In Situ Reaction Furnace
Designed as a stand alone
equipment to be used on mcx
beamline.
Maximum temperatures reached in
current setup 1000 C.
Ideal for powder samples
Diffraction data recorded on a
translating Imaging plate.
Remote controlled
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin •39
Furnace Design
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Furnace Design
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Detection system
Images recorded on
translating imaging plate
Translation controlled by
Labview program
Measurements in
contiunuous and discrete
mode
Data integration using fit2d
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin •42
Capillary holder
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Experimental Station
•Phase identification
•Residual stress •Micro-structural analysis
•Structure determination
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The SCW beamlines cluster
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•Crytical photon energy 13.4 keV
•Total radiated power 6.85 kW
•Maximum field: 3.5 T
•Poles 49
•Pole gap 16.5 mm
•Period length 64 mm
The multipole superconducting wiggler, constructed by BudkerInstitute of Novosibirsk, was designed to produce a high flux andbrilliance source in the 10-25 keV range. Currently refurbished atNovosibirsk with new cryostat allowing to limit the liquid helium(LHe) consumption to a maximum of 2 refills per year
Multipole Superconducting Wiggler
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The new SCW compared to the permanent magnetwiggler of the existing Diffraction beamline (xrd1)
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Photon energy (eV)
E=2.4GeV; I=100mA SCW
W 14.0
A factor 14 higherbrilliance at 25 keV !!
Multipole Superconducting Wiggler
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25 keV High Pressure branch-line
Super conducting wiggler
Si111
17.2 m
Toroidal
Mirror
33 m Experiment 44.8 m
Mask
Filters
Acceptance 500*120 μrad2
Flux in 80*80 μm2 aperture at sample:
1011 ph/s @ 2.4 GeV, 100mA
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XRD2 – general layout
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
XRD2 and Xpress have been designed in collaboration with the Indian
Institute of Science (Bangalore)
The source can host a third fixed energy beamline (Pharma?).
Most optical components already characterized and installed. Orders
have been placed for >95% of the necessary items and we expect to
have all the items vacuum-related, controls and plants in house and
installed for September 2014 (commissioning till February 2015).
Will present all the features of a high throughput MAD BL (including
sample changer, SPINE compatible), with remote data collection
capability.
Xpress is expected to be up and running in Spring 2015.XRD2 is expected to be up and running in Summer 2015.
XRD2: status and perspective
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
SCW Front-end mask
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Beam splitter
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Flux at the sample: 3.3 E13 ph/s/0.1%BW (2GeV, 100mA)
Sizes of the focal spot: 330μm X 90μm, 2.3mrad X 0.3mrad [FWHM]
Estimated fluxes at the sample (taking account of filters, efficiency of the
monochromator, reflectivity of the mirrors and different sample sizes):
Flux @2GeV, 310 mA
Flux @2.4GeV, 140 mA
Square size
1 x 1013 7 x 1012 200µm X 200µm
9 x 1011 6 x 1011 50µm X 50µm
2.5 x 1010 2 x 1010 10µm X 10µm
XRD2: flux at focus
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Flux @2GeV, 310 mA0
Flux @2.4GeV, 140 mA
Square size
1 x 1013 7 x 1012 200µm X 200µm
9 x 1011 6 x 1011 50µm X 50µm
2.5 x 1010 2 x 1010 10µm X 10µm
BL spot size flux (ph/s)
BM14 300 x 750 4,50E+011
ESRF - Id14-1 50x200 1,00E+011
ESRF – Id14-2 100x100 1,00E+011
ESRF – Id14-4 90x250 5,00E+012
ESRF – ID23-2 10x10 4,00E+011
ESRF – ID29 30x50 1,00E+013
ALBA - XALOC 6x50 2,00E+012
BESSY - 14.1 50x50 1,60E+011
SLSPSI - X06DA 90x70 4,00E+011
SLSPSI - X10SA 50x10 2,00E+012
DIAMOND - I24 80x80 1,00E+012
Set against the existing MX beamlines in
Europe, XRD2 compare favourably with
most non-microfocus beamlines, such as
ESRF BM14/ID14-1/ID14-2, Bessy 14.1,
SLS X06DA, Diamond I24.
XRD2: status and perspective
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
XRD2 status
Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin
XRD2 status
THANK YOU FOR YOUR ATTENTION