Status of the crystallography beamlines at Elettrailsf.ipm.ac.ir/News/2015-04-20-7thUsersMeetingFull/7thUs... · 2015-05-25 · 7° ILSF Users’ Meeting –Qazvin Andrea Lausi –

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

1019

1021

1023

1025

1027

1029

1031

1033

Pea

k B

rilli

ance (

Pho

tons/s

/mm

2/m

rad

2/0

.1%

bw

)

100

101

102

103

104

105

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


1995-2006:XRD beamline

macromoleculesbut also material science, high pressure, fibers, inorganic crystals...

Diffraction at ELETTRA

4


HRD(1) diffraction beamline (1995 version)

5

source

slits

monochromator

refocussing mirror

sample stage

filter


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.


• 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.


Structural biology lab

Molecular biology

Large scale proteinexpression

Protein purification

Protein characterisation

Biophysical analysis

Biochemical analysis

Crystallisation


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


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


Molecular biology lab


Bacterial protein expression


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


Crystallization lab


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


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

16


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

17


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

18


1010

1011

1012

1013

Photo

ns/

s/0.1

%bw

(/2

mra

d h

ori

z /0

.27 m

rad v

ert.

)

103

2 3 4 5 6 7 8 9

104

2

Photon Energy (eV)

1010

1011

1012

1013

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

19


1010

1011

1012

1013

Photo

ns/

s/0.1

%bw

(/2

mra

d h

ori

z /0

.27 m

rad v

ert.

)

103

2 3 4 5 6 7 8 9

104

2

Photon Energy (eV)

1010

1011

1012

1013

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)

20

MCX optical design : source


• High-transmission Filter-window assembly

• Collimating Pre-mirror

• Wide range monochromator with II crystal bender for dynamical sagittal focusing

• Bendable focusing mirror

21

MCX optical design : outline


Sagittal Focussing

22

Grazing incidence reflection optics:• geometrical loss • small acceptances• difficult to manufacture• expensive

bent II crystal


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

23


The Elettra Hard X-ray Monochromator

24

Andrea Lausi – 20-21 April 20157° ILSF Users’ Meeting – Qazvin Anrea Lausi The CX project… 25

Front-end Hutch


First mirror

•26


0.5 µrad slope errormeasured on the ElettraLong Trace Profilometer

First mirror

•27


0.65 µrad slope error

•28


From the Optical to the Experimental Hutch

•29


Experimental Station

•30



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

•31


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...

• ...

•32



•33



•34


Instrumental profile (capillary)

•35


Instrumental profile (flat plate)

•36


Instrumental profile (capillary)


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


Furnace Design


Furnace Design


Detection system

Images recorded on

translating imaging plate

Translation controlled by

Labview program

Measurements in

contiunuous and discrete

mode

Data integration using fit2d


Capillary holder



•Phase identification

•Residual stress •Micro-structural analysis

•Structure determination

•43


The SCW beamlines cluster

•44


•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


The new SCW compared to the permanent magnetwiggler of the existing Diffraction beamline (xrd1)

1010

1011

1012

1013

1014

1015

1016

Bri

llia

nce

(p

ho

ton

s/s

/0.1

%B

W/m

m2/m

rad

2)

101

102

103

104

105

Photon energy (eV)

E=2.4GeV; I=100mA SCW

W 14.0

A factor 14 higherbrilliance at 25 keV !!

Multipole Superconducting Wiggler


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


XRD2 – general layout


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


SCW Front-end mask


Beam splitter


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


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


XRD2 status


XRD2 status

THANK YOU FOR YOUR ATTENTION

Documents

Status of the crystallography beamlines at Elettrailsf.ipm.ac.ir/News/2015-04-20-7thUsersMeetingFull/7thUs... · 2015-05-25 · 7° ILSF Users’ Meeting –Qazvin Andrea Lausi –