Future Possible Use of Neutron and Synchrotron Sources by the Austrian ...€¦ · Future Possible...
Transcript of Future Possible Use of Neutron and Synchrotron Sources by the Austrian ...€¦ · Future Possible...
-
ii
Abstract Booklet
Future Possible Use of Neutron and
Synchrotron Sources by the Austrian
User Community
15th and 16th September 2016
Graz University of Technology
Organized by NESY
hosted by
TU Graz
-
ii
-
iii
Venue:
Graz University of Technology
Chemistry building
HS H "Ulrich Santner"
Kopernikusgasse 24
8010 Graz
Hosted by:
Prof. Dr. Horst Bischof , Vice rector for research TU Graz
Prof. Dr. Frank Uhlig, Dean TCVB, TU Graz
Editorial Team:
Heinz Amenitsch (Organizing committee TU Graz)
Gerhard Krexner (NESY Austria, Universität Wien)
Oskar Paris (MU Leoben)
Layout and production:
Heinz Amenitsch (TU Graz)
Barbara Sartori (TU Graz)
Barbara Seibt (TU Graz)
Cover: Image of the diffraction pattern of the rhombohedral phase of the phospholipid 1,2-Dioleoyl-sn-Glycero
3-Phospho-choline measured at the Austrian SAXS beamline of ELETTRA. (Rappolt, M. et al., Adv. Colloid
Interface Sci. 111, 63–77 (2004).)
-
iv
Supported by
-
v
Organizers:
Heinz Amenitsch (Organizing committee TU Graz)
Horst Bischof (Vice Rector TU Graz)
Frank Uhlig (Dean TCVB, TU Graz)
Gerhard Krexner (NESY Austria, Universität Wien)
Oskar Paris (MU Leoben)
Program committee:
Heinz Amenitsch (TU Graz, Elettra)
Klaudia Hradil (TU Wien)
Gerhard Krexner (Universität Wien)
Oskar Paris (Montanuniversität Leoben)
Julian Stangl (Universität Linz)
Advisory board:
Günther Bauer (Johannes Kepler Universität Linz)
Helmut Rauch (TU Wien)
Christoph Kratky (Karl-Franzens-Universität Graz)
Gero Vogl (Universität Wien)
Christian Köberl (Universität Wien)
Kristina Djinovic-Carugo (TU Wien)
Helmut Clemens (Montanuniversität Leoben)
Nicola Hüsing (Paris Lodron Universität Salzburg)
Günther Rupprechter (TU-Wien)
Herwig Peterlik (Universität Wien)
Ernst Bauer (TU Wien)
Silke Bühler-Paschen (TU Wien)
Christina Streli (TU Wien)
Ruth Prassl (Medizinische Universität Graz)
Walter Keller (Karl-Franzens-Universität Graz)
-
vi
-
vii
Welcome address organizers
In 2011 the first Austrian Synchrotron Radiation User Meeting was hosted by the (then) Austrian
Federal Ministry of Science and Research. This event was soon followed by another symposium at the
TU Vienna in 2013 extending also to the Austrian neutron community. Motivated by the success of
these earlier conventions the Neutron and Synchrotron Radiation (NESY) section of the Austrian
Physical Society (OePG) suggested to hold follow-up meetings at regular intervals starting in 2016,
preferably in Graz. The TU Graz (Vice Rector Horst Bischof and Dean TCVB Frank Uhlig) kindly
offered to host such a meeting and to provide also financial support.
The event was smoothly prepared in close cooperation of Program Committee, Advisory Board and
local Organizers. The success comes into view through the abstract booklet of this second Symposium
“Science at European Neutron and Synchrotron Facilities by Austrian Researchers”. The impact and
importance of large scale infrastructure in these fields are clearly recognizable from the large
attendance of the present event gathering over 70 abstracts for oral and poster contributions and
around 100 participants.
The scope of the meeting is primarily devoted to science. Keynote lectures by the scientific directors
of the facilities with formal Austrian association will provide an overview of current and future
possibilities at ESRF, ILL, ELETTRA and CERIC-ERIC. Two more keynote lectures will address the
two most important future sources, represented by delegates of the European X-ray Free Electron
Laser (X-FEL) and of the European Spallation Source (ESS). The remainder of the contributions will
provide a broad overview of Austrian NE&SY research and present activities at large scale
installations but also a perspective on new possibilities becoming available at new facilities within the
next years.
The scientific program will be complemented concisely by relevant information from the Austrian
Academy of Sciences and NESY, as well as from the Austrian representatives at the international
research facilities. An open round-table discussion about user needs and future demands will be held
on the evening of the first day of the symposium.
We are very happy that this symposium could be realized without having to collect a conference fee.
In this respect, we are deeply indebted to the TU Graz for providing all the facilities for free and for
bestowing, in addition, the most substantial financial contribution. We are also very thankful that the
keynote speakers were ready to travel on their own costs, and we wish to thank CERIC-ERIC,
ELETTRA, ESRF, ILL, ESS, and X-FEL explicitly in this context. Further, we thank all the Austrian
scientists for their contributions though it was not easy for some to attend. Finally, we wish to
acknowledge the continuous support from the Austrian Ministry BMWFW, with particular thanks to
MR Dr. Weselka, for his long-standing commitment to backing the NE&SY community.
We are confident that this meeting will effectively contribute to make the research achievements of
the Austrian NE&SY user community more apparent both to the public and within the deciding
bodies in the OeAW and the University Rectorates. We note that the size of the Austrian community
performing research in these fields as well as the number and international visibility of related
publications have steadily and significantly increased over the years. These facts convincingly
demonstrate that the scientific results obtained through participation in international facilities
definitely justify the financial engagement required to this end.
-
viii
Finally, it is a particular matter of concern to us to point out that for sustaining a position close to the
forefront of research it will, in the longer term, not suffice to maintain already existing Austrian
memberships in large scale infrastructure. Rather, this goal will additionally necessitate access to new
facilities and projects such as X-FEL, ESS and ELI. Once again, we have organized this event in the
hope to convince the Austrian funding institutions and notably the BMWFW to provide adequate
funding also in the future.
On behalf of the program committee
Heinz Amenitsch (chair of the organizing committee)
Gerhard Krexner (NESY chairperson)
-
ix
TABLE OF CONTENT
Program: NESY Workshop 1
Oral presentations 5
KN1 ILL - 50 years of neutrons and new opportunities 5
KN2 Progress in instrumentation and Science 6
T3 High Precision Experiments with Cold and Ultra-Cold Neutrons 7
KN4 European Spallation Source: Status and Opportunities 8
KN5 The Next Step in the Exploitation of Storage-Ring-Based High Energy X-ray Sources 9
T6 “X-ray colors” as 3rd dimension in crystallographic texture measurements of complex
materials 10
T7 NESY for Energy: Neutron and Synchrotron Radiation Characterisation of Nanostructures
for Energy Materials 11
T8 Diffractive optics for slow neutrons 12
KN9 Status and perspectives of Elettra and FERMI@Elettra 13
T10 Surface-Induced Phases of Small Molecules: Crystal Structure Solution from Thin Films 14
T11 Operando studies of working catalysts by synchrotron-based XPS and XAS at atmospheric
pressure: surface science and applied catalysis 15
T12 Structure and mechanism of respiratory complex I, a giant molecular proton pump 16
KN13 The CERIC-ERIC and ELI research Infrastructures 17
T14 X-ray absorption spectroscopy – a versatile tool to study multi-constituent functional
materials 18
T15 X-ray spectrometry with Synchrotron radiation 19
KN16 European XFEL: Unique Possibilities for Multidimensional Research 20
T17 The Nanoscopic Structural Face of Biomembranes 21
T18 Decoding the pathways of high-pressure transformations 22
Poster Presentations 23
Poster Abstracts 27
P1 Crystal structure of the Saccharomyces cerevisiae monoglyceride lipase Yju3p 27
P2 In-situ characterization of airborne nanoparticles with SAXS 28
-
x
P3 Membrane domains properties connections with their lipid composition and ions in the
aqueous phase 29
P4 Towards a pump-probe x-ray scattering setup at the Austrian SAXS beamline 30
P5 In-Situ Crystallization Study of the Drug Carbamazepine and its Precursor by Grazing
Incidence X-ray Diffraction 31
P6 Structure and Mechanism of Legumain: A Multicatalytic Enzyme 32
P7 Error-Disturbance Uncertainty Relations studied in Neutron Optics 33
P8 Structural characterization of thaumatin-like proteins from various species and comparison
with the structurally related plant-food allergens 34
P9 Joint SAXS/SANS Data Analysis of Membranes Exhibiting Lipid Asymmetry 35
P10 The high temperature stability of monoclinic Sr-lawsonite 36
P11 Enhanced phase detection in X-ray powder diffraction 37
P12 Characterisation of advanced intermetallic titanium aluminide alloys by means of diffraction
and scattering techniques 38
P13 Synchrotron radiation as a tool for in situ studies in catalysis 39
P14 Core-shell nanoparticles – insights in their growth and dynamic behavior by small-angle
x-ray scattering 40
P15 Bone structure and mineralization in response to bio-resorbable implants revealed by
synchrotron microbeam techniques 41
P16 X-Ray nanodiffraction pointing out formation limitations of c-AlN in nanolayered thin films 42
P17 Development of a 3D Mixing Device for Small Angle X-Ray Scattering Measurements 43
P18 Magnetic interactions in the Zn-Co-O system: tuning local structure, valence and carrier type
from extremely Co doped ZnO to ZnCo2O4 44
P19 Monitoring of Pentoxifylline Thermal Behavior by Novel Simultaneous Laboratory Small
and Wide X-Ray Scattering (SWAXS) and Differential Scanning Calorimetry (DSC) 45
P20 Observation of neutron Pendellösung interference in holographic nanostructures 46
P21 Towards the Complex Structure of a Gram-positive Type IV Secretion System 47
P22 The Proton Electron Radiation Channel PERC at FRM II 48
P23 Amphiphilic designer peptides and their propensity to interact with membranes of different
complexity 49
P24 Neutron holography to study local atomic arrangements 50
P25 20 years High-Pressure Cell for the SAXS-Beamline at ELETTRA 51
-
xi
P26 Particle shape alterations and lipid phase changes of low density lipoprotein induced by
high hydrostatic pressure 52
P27 Current projects at the Atominstitut 53
P28 Deep X-ray Lithography for interdisciplinary research 54
P29 Adsorption-induced deformation of hierarchical porous silica studied by in-situ neutron
and x-ray scattering 55
P30 The Neutron Alphabet at the ILL 56
P31 Application of Synchrotron-Based X-ray Computed Micro Tomography to Porous Media
Flows 57
P32 Regioselective para-Carboxylation of Phenols by a prFMN-Dependent Decarboxylase 58
P33 In-situ monitoring of protein adsorption layer thickness during protein-A chromatography
using SAXS 59
P34 Investigation of deformation induced defects in gamma phase polypropylene 60
35 Pore Shape and Lattice Deformation in Mesoporous Films 61
P36 In-operando SAXS as a novel method to understand ion electrosorption in confined
geometry 62
P37 Investigation of precursor-based formation routes towards metal sulfide nanocrystals by
time-resolved GISAXS and GIWAXS studies 63
P38 Realization of Ramsey-type Gravity Resonance Spectroscopy within qBounce 64
P39 A surface-induced phase of cellulose? 65
P40 Changing the chemoselectivity of an aldo-keto-reductase to a flavin-free ene-reductase 66
P41 The cap makes the difference: Investigation of the cap architecture in monoacylglycerol
lipases 67
P42 Aurone synthase: crystal structures of latent, active and inactive forms provide insights into
activation, inactivation and the catalytic mechanism of plant polyphenol oxidases 68
P43 Tuning the structure of silica mesoporous materials by precursors composition: solvents
effect studied in situ with SAXS 69
P44 Time-resolved X-ray detected ferromagnetic resonance with spatial resolution using
scanning X-ray microscopy 70
P45 Atomic scale diffusion in ordered intermetallics and glasses studied by X-ray photon
correlation spectroscopy 71
P46 Dislocation movement induced by molecular relaxations in isotactic polypropylene 72
P47 Weak Values in Neutron Interferometry 73
-
xii
P48 Crystal structure and strain in nanowires from XRD 74
P49 Snapshots of a Quantum Bouncing Ball realized with the qBounce gravity spectrometer 75
P50 Study of atomic motion in rubidium borate glasses 76
P51 Study of strain induced martensitic transformation in a Co-Cr-W alloy 77
P52 Effective interactions in protein-salt solutions approaching liquid-liquid phase separation 78
P53 The three-dimensional crystal structure of the allergenic wheat beta amylase 79
P54 XRD vs. Photo luminescence. A new class of devices to calibrate deformation potentials 80
P55 A cold neutron beam facility for particle physics at the ESS 81
P56 NoMoS: BSM Physics in Neutron Decay 82
Index 83
-
1
Program: NESY Workshop 15.09. – 16.09.2016
Do 15.9.2016
09:00 09:45 Registration
09:45 09:50 Welcome Address Organizers
Heinz Amenitsch (TU Graz)
09:50 09:55 Welcome Address TU-Graz
Horst Bischof (TU Graz)
09:55 10:00 Welcome Address OEAW Helmut Rauch (TU Wien & OEAW)
10:00 10:05 Welcome Address BM.WFW
Daniel Weselka (BM.WFW)
Time Top Name Chair Helmut Rauch
10:05 10:35 Talk representative ILL Mark Johnson (ILL, France) ILL - 50 years of neutrons and new opportunities
10:35 11:05 Béla Faragό (ILL, France) Progress in Instrumentation and Science
11:05 11:35 Hartmut Abele (TU Wien) High Precision Experiments with Cold and Ultra-Cold Neutrons
11:35 12:15 Talk representative ESS Günther Muhrer (ESS, Sweden) European Spallation Source: Status and Opportunities
12:15 13:25 Lunch
Time Top Time Name Chair Julian Stangl
13:25 14:05 Talk representative ESRF Harald Reichert (ESRF, France) The Next Step in the Exploitation of Storage-Ring-Based High Energy X-ray Sources
14:05 14:25 Helga Lichtenegger (Boku Wien) “X-ray colors” as 3rd dimension in crystallographic texture measurements of complex materials
14:25 14:45 Rainer Lechner (MU Leoben) NESY for Energy: Neutron and Synchrotron Radiation Characterisation of Nanostructures for Energy Materials
14:45 15:05 Martin Fally (Univ Wien) Diffractive optics for slow neutrons
-
2
15:05 15:50 Break/Poster Session
Time Top Name Chair Klaudia Hradil
15:50 16:30 Talk representative ELETTRA
Alfonso Franciosi (ELETTRA Sincrotrone Trieste, Italy)
Status and perspectives of Elettra and FERMI@Elettra
16:30 16:50 Roland Resel (TU Graz) Surface-Induced Phases of Small Molecules: Crystal Structure Solution from Thin Films
16:50 17:10 Günther Rupprechter (TU Wien) Operando studies of working catalysts by synchrotron-based XPS and XAS at atmospheric pressure: surface science and applied catalysis
17:10 17:30 Leonid Sazanov (IST Austria) Structure and mechanism of respiratory complex I, a giant molecular proton pump
Time Round Table Moderator: Frank Uhlig (TU Graz)
17:20 17:50 Intro Round Table: GroFo Österreich
Helmut Rauch (TU Wien & GroFo-OEAW)
ESRF Oskar Paris (MU Leoben & ESRF-Beirat)
ILL Gerhard Krexner (Univ Wien & NESY & ILL-Beirat)
ELETTRA/CERIC Heinz Amenitsch (TU Graz & ELETTRA)
17:50 19:00 Round Table
Time Poster Session
19:00 20:30 Dinner/Poster Session
20:30 - Get-together
-
3
Fr 16.9.2016
Time Top Name Chair Gerhard Krexner
09:00 09:40 Talk representative CERIC-ERIC
Carlo Rizzuto (CERIC-ERIC) The CERIC-ERIC and ELI research Infrastructures
09:40 10:00 Andreas Ney (Univ Linz) X-ray absorption spectroscopy – a versatile tool to study multi- constituent functional materials
10:00 10:20 Peter Wobrauschek (TU Wien) X-ray spectrometry with Synchrotron radiation
10:25 11:00 Break/Poster Session
Time Top Name Chair Heinz Amenitsch
11:00 11:40 Talk representative XFEL Serguei Molodtsov (European XFEL GmbH, Germany)
European XFEL: Unique Possibilities for Multidimensional Research
11:40 12:00 Georg Pabst (Univ Graz) The Nanoscopic Structural Face of Biomembranes
12:00 12:20 Ronald Miletich (Univ Wien) Decoding the pathways of high-pressure transformations
12:20 12:40 Concluding Remarks
-
5
Oral presentations
KN1 ILL - 50 years of neutrons and new opportunities
Mark Johnson
ILL, France
Institut Laue Langevin, Grenoble, France
In January 2017 the ILL will celebrate 50 years since the signing of the agreement between France
and Germany to construct the high flux reactor in Grenoble. The reactor went critical in 1971 and, in
1973, the UK joined the project as the third Associate. Subsequently about a dozen countries have
become scientific members creating a truly European facility. The facility was designed for neutron
beam experiments and to offer a user service to scientists. For almost 50 years, the ILL has provided
scientists with the most intense, continuous neutron beams in the world resulting in about 21 000
scientific publications to date.
Sustaining this performance has required regular upgrades of the reactor and the experimental
facilities. Reactor upgrades ensure that it can be operated safely in an ever more stringent context. In
the nineties, the reactor vessel was replaced, the new one being rated for 50 years of operation, each
of 200 days at full power. There is no technical reason why the reactor cannot be operated beyond
2040.
Many instruments and guide systems were upgraded in the Millenium programmes which started in
2000 and will conclude with the commissioning of WASP – the Wide Angle Spin Echo spectrometer
– at the end of this year. Instrument performance can typically improve by an order of magnitude each
decade allowing fundamentally new science to be performed with neutrons in the course of time. With
a view to operating for many years to come, the ILL has recently started phase one of the Endurance
upgrade programme for instrument and infrastructure upgrades (including sample environment and
software) for the period 2016-2018. The ILL is about to call for funds for phase two of Endurance for
the period from 2019 onwards.
The ILL has demonstrated remarkable longevity but the best is still to come!
-
6
KN2 Progress in instrumentation and Science
Béla Faragό
Institut Laue Langevin, Grenoble, France
The wise man said: “you can’t stand still!” The creation of the ILL as the strongest neutron source
created a lot of new science, but quickly “all the easy experiment are already done” became a reality.
New ideas, new materials keep emerging, present day science tackles more and more complex
problems.
The tremendous pressure on beam time request induced a natural motivation in ILL scientists ( and by
the in our users) to improve our instruments incorporating progress in technologies and computing.
This synergy of these two factors led to such improvements (10-50 times better instrument are worth
10-50 ILL reactors !) that funding bodies could not neglect. 50 years after the creation the ILL is still
in full swing, and continues to shape a complete and coherent instrument suite in field where neutrons
are the bests.
In this short time I will try to show some of our progresses, with illustrations of new science it
enabled and some of the ongoing projects with motivation behind.
-
7
T3 High Precision Experiments with Cold and Ultra-Cold
Neutrons
H. Abele
Atominstitut – TU Wien, Stadionallee 2, 1020 Wien, Austria
Contact email: [email protected].
The European Strategy Forum on Research Infrastructures (ESFRI) pursues various research
approaches in the field of particles and cosmology. In its 2016 roadmap, projects of pan-European
interest as ESFRI Landmarks are listed. The ESFRI report stresses the importance of neutron
instrumentation by targeting that “neutron sources can have a serious impact on strategic areas such as
particle physics, the fundamental quantum properties of the neutron, and cosmology”. With the
project ILL20/20 at Institut Laue-Langevin, ESFRI helps scientists to search for new fundamental
principles, interactions and unknown particles with neutrons.
In this talk, I will present precise symmetry tests of various kinds, which are coming within reach with
ILL20/20 and new neutron sources. We search for possible deviations from the Standard Model (SM)
of particle physics with cold and ultra-cold neutrons. The deviations are expected to be the
phenomenological outcome of more fundamental theories, unifying all forces induced shortly after the
Big Bang. Next, we present a novel direct search strategy with neutrons based on a quantum bouncing
ball in the gravity potential of the earth. The aim is to test the law of gravitation with a quantum
interference technique, providing constraints on dark matter and dark energy.
-
8
KN4 European Spallation Source: Status and Opportunities
G. Muhrer
European Spallation Source ERIC, Lund, Sweden
In July 2014, the European Spallation Source project entered the construction phase. As of end of
May 2016 the construction project has been 22.6% completed, with the plan on taking first beam at
the end of 2019. Early 2015 the decision was made on the moderator concept, which was followed a
few months later by a decision on the initial suite of 16 instruments. In late spring of 2016, the
accelerator tunnel has been topped off. Key target components, like the target wheel and the
moderator plug will enter the manufacturing phase later this year/early 2017. In the contribution an
update of the ESS project will be presented, as well as opportunities for partners during the
construction phase and future users of the facility.
-
9
KN5 The Next Step in the Exploitation of Storage-Ring-Based
High Energy X-ray Sources
H. Reichert
European Synchrotron Radiation Facility, 71Avenue des Martyrs
38000 Grenoble, France
The European Synchrotron Radiation Facility is Europe's premier hard X-ray synchrotron radiation
source serving 45 experimental stations for public use. The facility has just finished Phase I of an
ambitious upgrade programme (2009-2015) covering all aspects of the facility: photon production,
experimental facilities for users, user service, and X-ray technology development. The upgrade
benefits all areas of X-ray applications: Imaging, Spectroscopy, and Diffraction. A few examples will
be used to demonstrate first results from the new instruments.
In parallel we have started work for ESRF-EBS project (Phase II of the upgrade programme, 2015-
2022) focusing on the construction of a new storage ring with the goal to reduce the horizontal
emittance by at least a factor of 30 by 2020. The associated linear increase in brilliance and coherence
will enable new applications of X-rays in the study of soft and hard condensed matter [1]. After an
introduction of the main concepts behind the new source, the potential for new science will be
discussed.
[1] The ESRF Upgrade Programme Phase II (“Orange Book”)
http://www.esrf.fr/Apache_files/Upgrade/ESRF-orange-book.pdf
-
10
T6 “X-ray colors” as 3rd
dimension in crystallographic
texture measurements of complex materials
T.A. Grünewald(1,2)
, H. Rennhofer(1)
, P. Tack(3)
, J. Garrevoet(4)
, D.
Wermeille(5,6)
, P. Thompson(5,6)
, W. Bras(7)
, L. Vincze(3)
,
H.C. Lichtenegger(1)
(1) Institute of Physics and Materials Science, Department of Materials Sciences and Process Engineering,
University of Natural Resources and Life Sciences – BOKU, Vienna (Austria)
(2) Microfocus Beamline, ESRF Grenoble (France)
(3) Department of Analytical Chemistry, Ghent University (Belgium)
(4) Deutsches Electronen Synchrotron, Hamburg (Germany)
(5) XMaS -The UK CRG Beamline, ESRF Grenoble (France)
(6) Department of Physics, University of Liverpool (UK)
(7) Netherlands Organization for Scientific Research (NWO), DUBBLE@ESRF, Grenoble (France)
Many complex micro- and nanocrystalline materials of synthetic or biological origin (e.g.
biomineralized tissues) exhibit strongly preferred crystal orientation (crystallographic
texture). Conventionally, texture determination by x-ray diffraction (XRD) involves a number
of 2D diffraction images combined into 3D information by sample rotation. We have shown
that the photon energies (“x-ray colors”) in a white x-ray beam can be exploited to gain direct
3D crystallographic information in texture measurements. For this purpose we employed an
energy dispersive area detector to perform energy dispersive Laue diffraction (EDLD) on
carbon fiber samples containing different fiber orientations. We demonstrate that this
approach allows direct 3D reconstruction of crystallite texture and the acquisition of “one-
shot” pole figures without sample rotation. Proof of principle was also obtained for
biomineralized tissue. The major potential of this method lies in the direct 3D information
that could allow texture scanning of larger sample with complex sub-structures or following
texture changes in-situ during mineralization processes due to its inherent “one-shot” nature.
Figure 1: Crystallographic texture measurement by EDLD: a sample with locally different crystal orientations
(here displayed as fibers) is raster scanned with a polychromatic beam. The energy dispersive x-ray camera
delivers an energy spectrum in each pixel, which can be regrouped to obtain a stack of diffraction images at
energies. For each beam position on the sample the local 3D scattering pattern can be displayed directly.
[1] T.A. Grünewald, H. Rennhofer, P. Tack, J. Garrevoet, D. Wermeille, P. Thompson, W. Bras, L. Vincze,
H.C. Lichtenegger. Photon energy becomes the 3rd dimension in crystallographic texture analysis,
Angewandte Chemie Int. Ed., 55, DOI: 10.1002/anie.201603784, (2016).
-
11
T7 NESY for Energy: Neutron and Synchrotron Radiation
Characterisation of Nanostructures for Energy Materials
R.T. Lechner
Institut für Physik, Montanuniversität Leoben, Franz-Josef-Strasse 18, A-8700 Leoben, Austria
Novel material designs for future energy storage and production applications uses nanoparticles or
nanopores to further enhance the device performance.
The brilliant beams of modern synchrotron sources enables in-operando studies on the
behaviour of electrolyte-ions in nanopores of supercapacitors [1] and on the structural
changes of nanocrystals during cycling in Li-ion batteries. In combination with the unique
contrast variation capability of neutrons for water in porous materials [2], as well as advanced
computer simulations techniques, a better understanding of the underlying physical
mechanisms can be achieved.
Fig. 1: (a) Behaviour of electrolyte-ions in carbon nanopores of supercapacitors during electric cycling revealed
by in-operando synchrotron SAXS studies [1]. (b) Crystal phase transitions in chemically uniform PbS/CdS
core/shell nanocrystals revealed by anomalous SAXS and WAXS [3]. (c) In-situ SAXS study of the 3D self-
assembly of colloidal supercrystals using Bi-NCs (see inset TEM) as building blocks [6]
The optical emission of nanocrystals (NCs) used in solar cells can be drastically increased by
stabilising the core with a hard protective shell [3]. We have recently shown that metastable
crystal phases in the shell [4] as well as the NC shape influences significantly the optical
performance of the particle ensemble. This was only achieved by combining different
experimental techniques at several synchrotron sources with advanced data analysis [4, 5].
NCs can be also used as building blocks to form artificial solids with designed properties [3].
The NC’s shape, however, together with the synthesis conditions influence directly the
supercrystal structure of colloidal superlattices and hence its properties. This we have shown,
when we have investigated with in-situ synchrotron SAXS combined with Monte Carlo
simulations the 3D self-assembly of colloidal supercrystals by diffusion of a non-solvent into
a dispersion of faceted, elliptical Bi nanocrystals [6].
[1] C. Prehal, D. Weingarth, E. Perre, R.T. Lechner, et al.,& O. Paris, Energy Environ.Sci. 8, (2015), 1725-
1735
[2] M. Erko, D. Wallacher, A. Hoell, et al., & O. Paris, Phys. Chem. Chem. Phys 14, (2012), 3852-3858
[3] M. V. Kovalenko, L. Manna, A. Cabot, et al., & W. Heiss, ACS Nano 9, (2015), 1012-1057
[4] R.T. Lechner, G. Fritz-Popovski, M- Yarema, et al., & O. Paris, Chem. Mater. 26, (2014), 5914-5922
[5] M. Burian, G. Fritz-Popovski, M. He, et al., & R.T. Lechner, J. Appl. Cryst. 48, (2015), 857-868
[6] M.Burian, C. Karner, at al., & R.T. Lechner, to be submitted
-
12
T8 Diffractive optics for slow neutrons
M. Fally(1)
, J. Klepp(1)
, Ch. Pruner(2)
, P. Geltenbort(3)
, G. Nagy(4)
, L. Čoga(5)
, M.
Ličen(5)
, I. Drevenšek-Olenik(5),(6)
and Y. Tomita(7)
(1) Faculty of Physics, University of Vienna, Boltzmanngasse 5, A-1090 Wien, Austria
(2) Department Chemistry and Physics of Materials, University of Salzburg, A-5020 Salzburg, Austria
(3) Institut Laue Langevin, 71 avenue des Martyrs - CS 20156 - 38042 Grenoble Cedex 9, France
(4) Paul Scherrer Institut, CH-5232 Villigen PSI, Switzerland
(5) Jožef Stefan Institute, Jamova 39, SI 1001 Ljubljana, Slovenia
(6) Faculty of Mathematics and Physics, University of Ljubljana, Jadranska 19, SI 1000 Ljubljana, Slovenia
(7) Department of Engineering Science, University of Electro-Communications,
1-5-1 Chofugaoka, Chofu, Tokyo 182-8585, Japan
In recent years considerable effort has been devoted to design and develop neutron diffractive optical
elements (nDOE) for slow – i. e. cold and very cold – neutrons [1-4]. Progress was obtained by testing
new materials [5], optimizing and functionalizing them [6-7], as well as by improving the neutron-
optical techniques. We will discuss different nDOEs such as 2-port beamsplitters, n-port
beamsplitters, mirrors, polarizing elements and interferometers. A particular emphasis will be laid on
the materials and their properties as well as the techniques that are required to successfully prepare
nDOEs. Among the materials the most prominent are light-sensitive nanoparticle-polymer composites
or colloidal crystals from polymer beads. Another important issue that will be addressed are
diffraction theories and their implications on typical neutron optical experiments performed with very
cold neutrons using nDOEs. A recent example is the observation of Pendellösung interference fringes
occurring simultaneously for the broad incident wavelength spectrum of a very-cold neutron beam in
the periodic potential of holographic nanostructures. Finally, future prospects with respect to
interesting materials for applications as well as to fundamental experiments will be presented.
SEM-images and corresponding neutron diffraction patterns of colloidal crystals from polystyrene spheres
without/with inclusion of maghemite nanoparticles(left/right)
[1] M. Fally, J. Klepp, Y. Tomita, T. Nakamura, C. Pruner, M.A. Ellabban, R.A. Rupp, M. Bichler, I. Drevenšek
Olenik, J. Kohlbrecher, H. Eckerlebe, H. Lemmel, H. Rauch, Phys. Rev. Lett. 105, 2010, 123904
[2] J. Klepp, C. Pruner, Y. Tomita, K. Mitsube, P. Geltenbort, M. Fally, Appl. Phys. Lett. 100, 2012, 214104.
[3] J. Klepp, C. Pruner, Y. Tomita, J. Kohlbrecher, M. Fally, Appl. Phys. Lett. 101, 2012, 154104
[4] J. Klepp, C. Pruner, Y. Tomita, P. Geltenbort, J. Kohlbrecher, M. Fally, Materials 5, 2012, 2788
[5] Y. Tomita, E. Hata, K. Momose, S. Takayama, X. Liu, K. Chikama, J. Klepp, C. Pruner, M. Fally, J. Mod.
Optic 63, 2016, S11.
[6] J. Guo, R. Fujii, T. Ono, J. Klepp, C. Pruner, M. Fally, Y. Tomita, Opt. Lett. 39, 2014, 6743.
[7] R. Fujii, J. Guo, J. Klepp, C. Pruner, M. Fally, Y. Tomita, Opt. Lett. 39, 2014, 3453.
-
13
KN9 Status and perspectives of Elettra and FERMI@Elettra
A. Franciosi
Elettra-Sincrotrone Trieste S.C.p.A. and Department of Physics,University of Trieste, Trieste, Italy.
Elettra, one of the first third generation synchrotron radiation sources implemented in Europe, was
upgraded with a new full-energy injector and since six years routinely operates in top-up mode both at
2.0 and 2.4 GeV, with increased source stability and availability (over 97% of the scheduled
beamtime). This makes Elettra one of the only two sources that were not originally designed with top-
up in mind and were later successfully upgraded to this most efficient operating mode. The 26
beamlines available at Elettra now include a new x-ray fluorescence beamline (XRF), partially funded
by the International Atomic Energy Agency (IAEA), a new x-ray diffraction beamline (XRD2)
dedicated to protein crystallography and a new x-ray diffraction beamline (XPRESS) devoted to high
pressure studies. One of the beamlines with the highest productivity and in highest demand at Elettra
is the Austrian SAXS facility operated by TU-Graz. We will discuss the possible options for an
upgrade of the Elettra source that will produce a twentyfold increase on brightness above 1 keV and
would allow Elettra to remain competitive over the next decade. FERMI@Elettra, the only seeded
EUV-soft-x-ray free-electron laser (FEL) user facility currently operating worldwide, was
implemented by upgrading the S-band Linac - previously employed for injection into Elettra - to a
maximum energy of 1.8 GeV, adding an X-band module, and implementing APPLE-II insertion
devices as modulators and radiators in a single-stage FEL-1 source, and a two-stages FEL-2 source
currently under commissioning. All undulators were constructed by Kyma, a commercial spin-off
company of Elettra-Sincrotrone Trieste. Both sources afford jitter-free pump-probe capabilities using
two-colors configurations or exploiting the UV seed laser as a pump/probe. Full control of
polarization (from linear through circular) is also available. At the moment FEL-1 provides stable,
reproducible and fully coherent EUV pulses down to a 10 nm wavelength. We will illustrate the
present and projected operation parameters of the FERMI FEL-2 source, which is already producing
10 μJ pulses at a wavelength of 4 nm in the first harmonic. Possible extensions to higher photon
energies in the soft-x-ray range through the use of afterburners or specific radiator configurations will
be discussed.
-
14
T10 Surface-Induced Phases of Small Molecules: Crystal
Structure Solution from Thin Films
Roland Resel(1)
, Andrew O. F. Jones(1)
, Ingo Salzmann(2)
, Christian Röthel(3)
,
Oliver Werzer(3)
(1) Institute of Solid State Physics, NAWI Graz, Graz University of Technology, Petersgasse 16, 8010 Graz,
Austria
(2) Department of Physics, Humboldt Universität zu Berlin, Brook-Taylor-Straße 6, 12489 Berlin, Germany
(3) Institute of Pharmaceutical Sciences, Department of Pharmaceutical Technology, University of Graz,
Universitätsplatz 1, 8010 Graz, Austria
The presence of a surface during the crystallization process of a molecular material can induce new
polymorphs, as is frequently observed for organic electronic molecules and recently also in
pharmaceuticals [1,2]. One fundamental point of interest in such surface-induced phases is the crystal
structure, in particular the differences in the molecular packing from the bulk crystal structure.
However, surface-induced phases are only present within thin films and up to now there is not an
established procedure to solve crystal structures from thin films. One possibility is the use of grazing
incidence surface x-ray diffraction using synchrotron radiation. Within the talk, the progress in the
field of crystal structure solution from thin films will be introduced but also the difficulties, open
problems and limitations of the method will be discussed. Examples of crystal structure solution from
thin films will be introduced and the differences in the molecular packing between surface-induced
crystal structures and bulk structures will be discussed based on rod-like aromatic molecules,
conjugated molecules with flexible side chains and hydrogen bonded molecules [3-6].
[1] A. O. F. Jones, B. Chattopadhyay, Y. H. Geerts, R. Resel, Substrate-Induced and Thin-Film Phases:
Polymorphism of Organic Materials on Surfaces Advanced Functional Materials, 26, 2233-2255 (2016).
[2] D. Reischl, C. Rothel, P. Christian, E. Roblegg, H. M. A. Ehmann, I. Salzmann, O. Werzer,
Surface-Induced Polymorphism as a Tool for Enhanced Dissolution: The Example of Phenytoin
Crystal Growth & Design, 15, 4687-4693 (2015).
[3] A. Pichler, R. Resel, A. Neuhold, T. Dingemans, G. Schwabegger, M. Moret, C. Simbrunner, I. Salzmann, Crystal structure determination of organic thin-films: the example of 2,2 ': 6 ',2 ''-ternaphthalene
Zeitschrift für Kristallographie 229, 385-393 (2014).
[4] A. O. F. Jones, Y. Geerts, J. Karpinska, A. R. Kennedy, R. Resel, C. Rothel, C. Ruzie, O. Werzer, M.
Sferrazza, Substrate-induced phase of a [1]Benzothieno[3,2-b]benzothiophene derivative and phase
evolution by aging and solvent vapor annealing. ACS Applied Materials & Interfaces, 7, 1868-73 (2015).
[5] C. Lercher, C. Röthel, O. M. Roscioni, Y. H. Geerts, Q. Shen, C. Teichert, R. Fischer, G. Leising,
M.Sferrazza, G. Gbabode, R. Resel Polymorphism of dioctyl-terthiophene within thin films: The role of the
first monolayer Chemical Physics Letters 630, 12–17 (2015).
[6] M. Truger, O. M. Roscioni, C. Röthel, D. Kriegner, C. Simbrunner, R. Ahmed, E. D. Głowacki, J.
Simbrunner, I. Salzmann, A. M. Coclite, A. O. F. Jones, R. Resel Surface-Induced Phase of Tyrian Purple
(6,6′-Dibromoindigo): Thin Film Formation and Stability Crystal Growth Design 16, 3647–3655 (2016).
-
15
T11 Operando studies of working catalysts by synchrotron-
based XPS and XAS at atmospheric pressure:
surface science and applied catalysis
Günther Rupprechter, Karin Föttinger, Christoph Rameshan
Institute of Materials Chemistry, Technische Universität Wien, 1060 Vienna, Austria
Modern studies of catalytic reaction mechanisms are typically performed in the operando mode, i.e.
performing spectroscopy, microscopy and/or diffraction on the functioning (working) catalysts while
catalytic activity/selectivity are simultaneosly recorded. Only the operando approach guarantees
meaningful structure-activity/selectivity correlations because the active catalyst maybe different from
that after synthesis or during ex situ analysis.
Our group has a long tradition on using synchrotron-based operando methods to evaluate catalytic
processes [1-3]: atmospheric pressure X-ray photoelectron spectroscopy (AP-XPS), X-ray absorption
spectroscopy (XAS, NEXAFS, EXAFS) and X-ray diffraction (BESSY (DE), MaxLab (SE), SLS
(CH)). This is complemented by lab-based methods such as infrared (FTIR, PM-IRAS) and
vibrational sum frequency generation spectroscopy (VSFG) that are also performed at pressures up to
1 bar.
Another asset of the group is to examine catalytic surface reactions on heterogeneous catalysts via a
two-fold approach, employing both industrial-grade catalysts as well as surface science based planar
model catalysts. Very recent examples include:
i) methane reforming on Ni-ZrO2 and CuNi-ZrO2 [4,5] as well as on UHV-grown ultrathin ZrO2
layers on Pt3Zr(0001) and Pt(111) [6],
ii) CO oxidation and H2/CO/O2 reaction (PROX) on commercial materials and Co3O4 and CoO thin
films UHV-grown on Ir(100) single crystals [7],
iii) electrochemical water splitting on perovskite-type electrodes under potential control [8].
For all, the operando studies identify the relevant surface processes with the surface science model
studies providing further atomistic insight, such as the effects of layer thickness (nanometer scale), of
surface corrugation (atomic scale), of valence band structure, of surface and bulk oxidation state,
oxygen vacancy formation, adsorbed species, reaction-induced surface segregation or reconstruction,
etc.
[1] G. Rupprechter, Advances in Catalysis, 51 (2007) 133-263.
[2] G. Rupprechter, Textbook on Surface and Interface Science, K. Wandelt (Editor), Wiley-VCH, Weinheim,
2016, 459-527 (ISBN: 978-3-527-41158-0).
[3] K. Föttinger, G. Rupprechter, Accounts of Chemical Research, 47 (2014) 3071−3079.
[4] A. Wolfbeisser, B. Klötzer, L. Mayr, R. Rameshan, D. Zemlyanov, J. Bernardi, K. Föttinger,
G. Rupprechter, Catalysis Science and Technology, 5 (2015) 967-978.
[5] A. Wolfbeisser, O. Sophiphun, J. Bernardi, J. Wittayakun, K. Föttinger, G. Rupprechter, Catalysis Today, in
press. DOI: http://dx.doi.org/10.1016/j.cattod.2016.04.025.
[6] H. Li, J.J. Choi, W. Mayr-Schmölzer, C. Weilach, C. Rameshan, F. Mittendorfer, J. Redinger,
M. Schmid, G. Rupprechter, Journal of Physical Chemistry C, 119 (2015) 2462–2470.
[7] L. Lukashuk; K. Föttinger; E. Kolar; C. Rameshan; D. Teschner; M. Hävecker; A. Knop-Gericke; N. Yigit;
H. Li; E. McDermott; M. Stöger-Pollach; G. Rupprechter, Journal of Catalysis, in press (2016).
[8] A. K. Opitz, A. Nenning, C. Rameshan, R. Rameshan, R. Blume, M. Hävecker, A. Knop-Gericke,
G. Rupprechter, J. Fleig, B. Klötzer, Angew. Chem. Int. Ed., 54 (2015) 2628-2632.
Supported by the Austrian Science Fund (FWF) via SFB-F45 FOXSI, DK+ Solids4Fun, ComCat and DryRef.
http://link.springer.com/search?facet-creator=%22Onsulang+Sophiphun%22http://link.springer.com/search?facet-creator=%22Jatuporn+Wittayakun%22
-
16
T12 Structure and mechanism of respiratory complex I, a
giant molecular proton pump
Leonid Sazanov
Institute of Science and Technology Austria, Am Campus 1, Klosterneuburg, 3400 Austria
NADH-ubiquinone oxidoreductase (complex I) is the first and largest enzyme in the respiratory chain
of mitochondria and many bacteria. It couples electron transfer between NADH and ubiquinone to the
translocation of four protons across the membrane. It is a major contributor to the proton flux used for
ATP generation in mitochondria, being one of the key enzymes essential for life as we know it.
Mutations in complex I lead to the most common human genetic disorders. It is an L-shaped assembly
formed by membrane and hydrophilic arms. Mitochondrial complex I consists of 45 subunits of about
1 MDa in total, whilst the prokaryotic enzyme is simpler and generally consists of 14 conserved
“core” subunits. We use the bacterial enzyme as a “minimal” model to understand the mechanism of
complex I. We have determined first atomic structures of complex I, starting with the hydrophilic
domain [1], followed by the membrane domain [2] and, finally, the recent structure of the entire
Thermus thermophilus complex (536 kDa, 16 subunits, 9 Fe-S clusters, 64 TM helices) [3]. Structures
suggest a unique mechanism of coupling between electron transfer in the hydrophilic domain and
proton translocation in the membrane domain, via long-range (up to ~200 Å) conformational changes.
I will discuss our current work, which is aimed at elucidating the molecular details of the coupling
mechanism through determination of structures of the complex in different redox states with various
bound substrates/inhibitors, using both X-ray crystallography and new cryo-EM methods.
[1] L.A. Sazanov, P. Hinchliffe, Structure of the hydrophilic domain of respiratory complex I from Thermus
thermophilus, Science, 311 (2006) 1430-1436.
[2] R.G. Efremov, L.A. Sazanov, Structure of the membrane domain of respiratory complex I, Nature, 476
(2011) 414-420.
[3] R. Baradaran, J.M. Berrisford, G.S. Minhas, L.A. Sazanov, Crystal structure of the entire respiratory
complex I, Nature, 494 (2013) 443-448.
-
17
KN13 The CERIC-ERIC and ELI research Infrastructures
Carlo Rizzuto
Chair of the General Assembly of CERIC-ERIC
Director General ELI-DC
A presentation of the scope and activities of the Central European Research Infrastructure CERIC-
ERIC, operating in the Analysis and Synthesis in Materials and Biomaterials will be given, as well as
brief reference to the Extreme Light Research Infrastructure now being completed in high power
Lasers in the same part of Europe.
These two infrastructures are dedicated to the scientific service to external users and aim at supporting
the capabilities of European research. A general overview of the developments in this area will also be
given.
-
18
T14 X-ray absorption spectroscopy – a versatile tool to study
multi-constituent functional materials
Andreas Ney
Institut für Halbleiter- und Festkörperphysik, Johannes Kepler Universität, Altenberger Str. 69, 4040 Linz
X-ray absorption spectroscopy (XAS) has proven to be a powerful, element selective experimental
technique which relies on the full polarization control of synchrotron light. This will be demonstrated
for XAS at the near edge (XANES) which contains information of the valence state of the absorbing
atoms. In addition, the associated x-ray linear dichroism (XLD) contains information on the local
structural properties, which can be used, e. g., to determine in incorporation of dopant atoms in a
given host crystal by combining it with theoretical simulations [1]. Using circular polarized light, the
element specific magnetic properties can be studied using the x-ray magnetic circular dichroism
(XMCD) up to external magnetic fields of up to 17 Tesla, which allows, e. g., quantifying
antiferromagnetic interactions between magnetic dopant atoms [2]. XANES can also be coupled with
other external excitations of the sample, e. g., microwaves to measure the x-ray detected
ferromagnetic resonance (XFMR) [3]. Very recently XFMR has also been combined with the high
spatial resolution of a scanning transmission x-ray microscope (STXM). This combination offers an
unprecedented combination of element selectivity, and high temporal (~15 ps) and spatial (~30 nm)
resolution. Finally, it has recently been demonstrated that XANES in external electric fields can also
provide element selective information about the electrical polarization based on the x-ray variant of
the linear Stark effect [5]. Synchrotron based XAS is thus the “swiss army knife” to investigate a
large variety of multi-constituent functional materials.
[1] A. Ney, K. Ollefs, S. Ye, T. Kammermeier, V. Ney, T. Kaspar, S. Chambers, F. Wilhelm and R. Rogalev,
Phys. Rev. Lett. 100, 157201 (2008)
[2] A. Ney, V. Ney, F. Wilhelm, A. Rogalev, and K. Usadel, Phys. Rev. B 85, 245202 (2012)
[3] K. Ollefs, R. Meckenstock, D. Spoddig, F. M. Römer, Ch. Hassel, Ch. Schöppner, V. Ney, M. Farle, and A.
Ney, J. Appl. Phys. 117, 223906 (2015)
[4] Stefano Bonetti, Roopali Kukreja, Zhao Chen, Detlef Spoddig, Katharina Ollefs, Christian Schöppner, Ralf
Meckenstock, Andreas Ney, Jude Pinto, Richard Houanche, Josef Frisch, Joachim Stöhr, Hermann Dürr, and
Hendrik Ohldag, Rev. Sci. Instrum. 86, 093703 (2015)
[5] V. Ney, F. Wilhelm, K. Ollefs, A. Rogalev, and A. Ney, Phys. Rev. B 93, 035136 (2016)
-
19
T15 X-ray spectrometry with Synchrotron radiation
Peter Wobrauschek, Mirjam Rauwolf, Anna Turyanskaya, Josef Prost
and Christina Streli
TU Wien, Atominstitut, 1020 Wien, Stadionallee 2
Hard X-ray spectrometry covers mainly energy dispersive XRS (EXRS) as well as X-ray absorption
spectroscopy (XAS). X-ray spectrometry deals with the emission of characteristic photons after
excitation of atoms with hard X-ray photons (E> 2 keV) and is used for qualitative and quantitative X-
ray analysis. Energy dispersive detectors are used to measure simultaneously the radiation
emitted/scattered from the sample. Absorption spectroscopy probes the fine structure of the absorption
edge of an element and is divided into XANES (X-ray absorption near edge structure) and EXAFS
(Extended X-ray absorption fine structure). XANES allows the determination of the chemical
compound, EXAFS allows to determine the nearest neighbors and coordination shells. XAS spectra
can be acquired in absorption or fluorescence mode.
Synchrotron radiation as excitation source in combination with advanced X-ray optics leads to a
development of special XRS techniques as micro-XRS (with resolutions below 100 nm) and total
reflection XRS (TXRF) extending the trace analysis capability in the fg (10-15 g) level. Using two
focusing optics between source and sample as well as sample and detector (confocal XRS) allows 3D
imaging without any reconstruction mechanism, but with limited spatial resolution to about 10 µm.
Combining EXRS with XAS measured in fluorescence mode allows to extend the applicability of
XAS down to the trace element level as well as to spatially resolved information about the oxidation
state.
Fundamentals of SR induced EXRS as well as XAS will be presented and an introduction to the
special techniques will be given. The field of applications is very wide, some examples from medicine
(analysis of trace elements in bone) will be presented as well as applications from environmental
analysis (analysis of airborne particles) and nanotechnology (surface contamination of Si wafer
surfaces, depth profiling and thin film analysis).
-
20
KN16 European XFEL: Unique Possibilities for
Multidimensional Research
Serguei Molodtsov
European XFEL GmbH, Holzkoppel 4, 22869 Schenefeld
The European X-ray free electron laser (XFEL) is a new international research installation that is
currently under construction in the Hamburg area in Germany. The facility will generate new
knowledge in almost all the technical and scientific disciplines that are shaping our daily life –
including nanotechnology, medicine, pharmaceutics, chemistry, materials science, power engineering
and electronics.
The ultra-high brilliance femtosecond X-ray flashes of coherent radiation will be produced in a 3.4-
kilometre long facility. Most of it will be housed in tunnels deep below ground. In its start-up
configuration, the European XFEL will comprise 3 self-amplified spontaneous emission (SASE) light
sources – undulators operating in energy ranges 3 – 25 keV (SASE 1 and SASE 2) and 0.2 – 3 keV
(SASE 3), respectively. The world-unique feature of this free electron laser is the possibility to
provide per second up to 27.000 ultra-short (10 – 100 fs), ultra-high brilliance flashes that makes this
facility particular suitable for multidimensional research in the range of moderate and hard X-ray
photons.
In this presentation, selected examples of experiments will be given and plans for implementation of
dedicated instrumentation at the European XFEL will be described.
-
21
T17 The Nanoscopic Structural Face of Biomembranes
Georg Pabst(1,2)
(1) University of Graz, Institute of Molecular Biosciences, Biophysics Division, NAWI Graz, Graz, Austria
(2) BioTechMed-Graz, Graz, Austria.
Biological membranes, such as cellular envelopes, are actively involved in diverse physiological
processes and consequently are in the spotlight of medical/pharmacological applications. A significant
part of our knowledge on biomembrane function originates from biophysical studies on membrane
mimetic systems of reduced complexity. In particular, lipid-only membranes are tractable and
commonly applied systems for an array of biophysical techniques.
Research in our lab is focused on the physical properties of complex lipid mixtures, including domain
formation, asymmetric membranes and their coupling to macromolecular interactions, protein
function and drug activity. This requires structural insight on the sub-nanometer level, which we
achieve by a joint analysis of small-angle x-ray and neutron scattering experiments including various
isotopic labelling schemes to achieve optimum structural contrast. I will highlight recent
achievements from our group and discuss potential near future applications of scattering techniques in
the field.
-
22
T18 Decoding the pathways of high-pressure transformations
Ronald Miletich(1)
, Thomas Pippinger(1,2)
, Yongjae Lee(3)
, Przemek Dera(4)
and
Robert T. Downs(5)
(1) Institut für Mineralogie und Kristallographie der Universität Wien, Althanstrasse 14, A-1090 Wien, Austria
(2) Fa. STOE & Cie GmbH, Hilpertstrasse 10, D-64295 Darmstadt, Germany
(3) Department of Earth System Sciences, Yonsei University, Seoul 120749, Korea
(4) Hawaii Institute of Geophysics and Technology, University of Hawaii at Manoa, Honolulu, U.S.A.
(5) Department of Geosciences, University of Arizona, Tucson, U.S.A.
Pressure and temperature shape our planets and extraterrestrial bodies and turn everyday liquids and
gases into condensed solids, unexpected molecular compounds or exotic metals. Polymorphism under
non-ambient conditions and associated structural transformations is the the typical response of
crystalline solids under changing P,T conditions. Scientific investigations of materials and their
transformation at static or dynamically changing conditions have produced a wealth of insights into
the chemical and physical properties of condensed matter. A particular challenge for experimental
approaches consists in understanding the transformations that lead to the formation of short-lived or
intermediate metastable phases. These processes are typically characterized by rapid transitions
between long-lived structures often passing through a sequence of several transient intermediates.
Identifying the detailed pathways followed during such transformations is of crucial importance for
understanding and controlling transformation processes. In this presentation we show the current tools
employed to investigate such high-pressure transformations, i.e. the applicability of time-resolved or
time-optimized X-ray diffraction experiments using synchrotron radiation sources. Apart from
demonstrating the tools and the adaption of techniques for measurements, examples of structural
phase transitions under high-pressure conditions will be shown. These examples include transitions in
CaCO3, BaMg(CO3)2 and Be(OH)2.
-
23
Poster Presentations
Presenter Poster Title
P1 Aschauer Philipp Crystal structure of the Saccharomyces cerevisiae monoglyceride lipase Yju3p
P2 Bauer Paulus In-situ characterization of airborne nanoparticles with SAXS
P3 Belicka Michal Membrane domains properties connections with their lipid composition and ions in the aqueous phase
P4 Burian Max Towards a pump-probe x-ray scattering setup at the Austrian SAXS beamline
P5 Christian Paul In-situ crystallization study of the drug Carbamazepine and its precursor by grazing incidence X-ray diffraction
P6 Dall Elfriede Structure and Mechanism of Legumain: A Multicatalytic Enzyme
P7 Demirel B. Error-Disturbance Uncertainty Relations studied in Neutron Optics
P8 Eder Markus Structural characterization of thaumatin-like proteins from various species and comparison with the structurally related plant-food allergens
P9 Eicher Barbara Joint SAXS/SANS Data Analysis of Membranes Exhibiting Lipid Asymmetry
P10 Ende Martin The high temperature stability of monoclinic Sr-lawsonite
P11 Ende Martin Enhanced phase detection in X-ray powder diffraction
P12 Erdely Petra Characterization of advanced intermetallic titanium aluminide alloys by means of diffraction and scattering techniques
P13 Föttinger Karin Synchrotron radiation as a tool for in situ studies in catalysis
P14 Grünewald Tilman Core-shell nanoparticles – insights in their growth and dynamic behavior by small-angle x-ray scattering
P15 Grünewald Tilman Bone structure and mineralization in response to bio-resorbable implants revealed by synchrotron microbeam techniques
P16 Hahn Rainer X-Ray nanodiffraction pointing out formation limitations of c-AlN in nanolayered thin films
P17 Haider Richard Development of a 3D Mixing Device for Small Angle X-Ray Scattering Measurements
P18 Henne Bastian Magnetic interactions in the Zn-Co-O system: tuning local structure, valence and carrier type from extremely Co doped ZnO to ZnCo2O4
P19 Hodzic Aden Monitoring of Pentoxifylline Thermal Behavior by Novel Simultaneous Laboratory Small and Wide X-Ray Scattering (SWAXS) and Differential Scanning Calorimetry (DSC)
P20 Klepp Jürgen Observation of neutron Pendellösung interference in holographic nanostructures
P21 Kohler Verena Towards the Complex Structure of a Gram-positive Type IV Secretion System
P22 Konrad Gertrud The Proton Electron Radiation Channel PERC at FRM II
P23 Kornmuller Karin Amphiphilic designer peptides and their propensity to interact with membranes of different complexity
-
24
P24 Krexner Gerhard Neutron holography to study local atomic arrangements
P25 Kriechbaum Manfred 20 years High-Pressure Cell for the SAXS-Beamline at ELETTRA
P26 Leofer Bernhard Particle shape alterations and lipid phase changes of low density lipoprotein induced by high hydrostatic pressure
P27 Mach Wilfried Current projects a t the Atominstitut
P28 Marmiroli Benedetta Deep X-ray Lithography for interdisciplinary research
P29 Morak Roland Adsorption-induced deformation of hierarchical porous silica studied by in-situ neutron and x-ray scattering
P30 Moser Daniel The Neutron Alphabet at the ILL
P31 Ott Holger Application of Synchrotron-Based X-ray Computed Micro Tomography to Porous Media Flows
P32 Pavkov-Keller Tea Regioselective para-Carboxylation of Phenols by aprFMN-Dependent Decarboxylase
P33 Plewka Jacek In-situ monitoring of protein adsorption layer thickness during protein-A chromatography using SAXS
P34 Polt G. Investigation of deformation induced defects in gamma phase polypropylene
P35 Popovski Gerhard Pore Shape and Lattice Deformation in Mesoporous Films
P36 Prehal Christian In-operando SAXS as a novel method to understand ion electrosorption in confined geometry
P37 Rath Thomas Investigation of precursor-based formation routes towards metal sulfide nanocrystals by time-resolved GISAXS and GIWAXS studies
P38 Rechberger Tobias Realization of Ramsey-type Gravity Resonance Spectroscopy within qBounce
P39 Resel Roland A surface-induced phase of cellulose?
P40 Reisenbichler A.M. Changing the chemoselectivity of an aldo-keto-reductase to a flavin-free ene-reductase
P41 Riegler-Berket Lina The cap makes the difference: Investigation of the cap architecture in monoacylglycerol lipases
P42 Rompel Annette Aurone synthase: crystal structures of latent, active and inactive forms provide insights into activation, inactivation and the catalytic mechanism of plant polyphenol oxidases
P43 Sartori Barbara Tuning the structure of silica mesoporous materials by precursors composition: solvents effect studied in situ with SAXS
P44 Schaffers Taddäus Time-resolved X-ray detected ferromagnetic resonance with spatial resolution using scanning X-ray microscopy
P45 Sepiol Bogdan Atomic scale diffusion in ordered intermetallics and glasses studied by X-ray photon correlation spectroscopy
P46 Spieckermann Florian Dislocation movement induced by molecular relaxations in isotactic polypropylene
P47 Sponar Stephan Weak Values in Neutron Interferometry
P48 Stangl Julian Crystal structure and strain in nanowires from XRD
P49 Thalhammer Martin Snapshots of a Quantum Bouncing Ball realized with the qBounce gravity spectrometer
P50 Tietz Christoph Study of atomic motion in rubidium borate glasses
-
25
P51 Weißensteiner Irmgard Study of strain induced martensitic transformation in a Co-Cr-W alloy
P52 Wolf Marcell Effective interactions in protein-salt solutions approaching liquid-liquid phase separation
P53 Hofer G. The three-dimensional crystal structure of the allergenic wheat beta amylase
P54 Ziss Daniel XRD vs. Photo luminescence. A new class of devices to calibrate deformation potentials
P55 Konrad Gertrud A cold neutron beam facility for particle physics at the ESS
P56 Konrad Gertrud NoMoS: BSM Physics in Neutron Decay
-
26
-
27
Poster Abstracts
P1 Crystal structure of the Saccharomyces cerevisiae
monoglyceride lipase Yju3p
Aschauer P.(1),Rengachari S.(1), Lichtenegger J. .(1), Schittmayer M. (2,3), Das
KMP. (1)
, Mayer N. .(1)
, Breinbauer R. (4)
, Birner-Gruenberger R. (2,3)
, Gruber CC.
.(1), Zimmermann R.
.(1), Gruber K. .
(1), Monika O.
(1)
(1) Institute of Molecular Biosciences, University of Graz, Humboldtstraße 50/3, 8010 Graz, Austria
(2) Research Unit Functional Proteomics and Metabolic Pathways, Institute of Pathology, Medical University
of Graz, Stiftingtalstrasse 24, 8010 Graz, Austria
(3) Omics Center Graz, BioTechMed-Graz, Stiftingtalstrasse 24, 8010 Graz, Austria
(4) Institute of Organic Chemistry, Graz University of Technology, Stremayrgasse 9, 8010 Graz, Austria
Monoglyceride lipases (MGLs) are lipases which catalyze the breakdown of monoglycerides (MGs)
resulting in free fatty acids and glycerol molecules. MGLs are predominantly specific towards MGs,
yet are not reported to show any region- or stereo-specificity (1-, 2- or 3-MGs). MGLs are present in
all species and execute different biological functions in different species and tissues. In mammals,
MGLs are actors in energy homeostasis and play a role in lipid signaling by regulating the levels of
the endocannabinoid 2-arachidonoyl-glycerol. In Pathogenic bacteria, including M. tuberculosis,
enzymes involved in degradation of host cell lipid depots may be essential in providing energy and
precursors for cell wall synthesis. Due to these different biological roles, MGLs are interesting
subjects for drug targeting.
Even though biochemical data about monoglyceride lipases are available for several decades the only
experimentally determined 3D structures are those of human MGL (hMGL) and MGL from Bacillus
sp. H-257 (bMGL). Two features are especially remarkable in those structures, namely the similarity
of the overall shape of the cap regions and its conformational flexibility [1]. We focused on Yju3p,
the MGL ortholog from Saccharomyces cerevisiae which was reported to also degrade fatty acid ethyl
esters and was suggested to play a role in non-oxidative ethanol metabolism [2]. In the course of this
study a soluble variant of Yju3p (s-Yju3p) could be crystallized and by measuring these crystals using
high intensity x-ray radiation from a synchrotron source we were able to obtain diffraction data
resolutions sufficient for processing. Regrettably the phase problem for these diffraction data sets
could not be solved via Molecular Replacement, therefore we resorted to heavy metal soaking and
Multiple Wavelength Anomalous Dispersion making a tune-able x-ray source crucial for the success
of this project.
Ultimately, we present crystal structures of s-Yju3p in its free form and in complex with an inhibitor
mimicking the tetrahedral intermediate of a C20:0 MG during hydrolysis. s-Yju3p harbors a cap
region similar to those of hMGL and bMGL. Interestingly, the structure of the inhibitor complex
revealed differences in the mode of substrate binding in s-Yju3p compared to the other two MGLs.
Analysis of the MG hydrolase activity of s-Yju3p unveiled differences in substrate preferences with
respect to the saturation state of the MG substrate [3].
[1] Rengacari S and Aschauer P et al, Conformational Plasticity and Ligand Binding of Bacterial
Monoacylglycerol, J Biol Chem (2013), 288 (43): 31090-31104
[2] Heier C, et al, Monoacylglycerol Lipases Act as Evolutionarily Conserved Regulators of Non-oxidative
Ethanol Metabolism, J Biol Chem (2016), 291(22):11865-11875
[3] Aschauer P et al, Crystal structure of the Saccharomyces cerevisiae monoglyceride lipase Yju3p, BBA -
Molecular and Cell Biology of Lipids (2016), 10.1016/j.bbalip.2016.02.005
-
28
P2 In-situ characterization of airborne nanoparticles with
SAXS
Paulus S. Bauer(1)
, Heinz Amenitsch(2)
and Paul M. Winkler(1)
(1) Faculty of Physics, University of Vienna, Boltzmanngasse 5, 1090 Wien, Austria
(2) Institute of Inorganic Chemistry, Graz University of Technology, Stremayrg. 9/IV, 8010 Graz, Austria
Here we report first experiments on airborne nanoparticle characterization by SAXS at concentrations
of about 106 cm-3. The experiments were conducted at the Austrian SAXS beamline at the Elettra
synchrotron in July 2015. To provide a representative environment for aerosols a flow tube was
operated at ambient pressure and room temperature conditions. The experimental setup has been
amended and optimized from previous measurement campaigns [1]. We analyzed high molecular
weight tungsten oxide particles exhibiting a high scattering contrast compared to the air background.
For direct comparison of the SAXS data to conventional aerosol measurements a Differential Mobility
Particle Sizer (DMPS) and a Condensation Particle Counter (CPC) were run in parallel. Figure 1
illustrates SAXS scattering curves for aerosol and particle free background conditions, respectively.
The size information obtained from the corresponding fits agrees reasonably well with the size
distribution measured by DMPS. These results show that SAXS can be used to obtain in-situ size
information of nanoparticles at close-to-ambient concentrations [2].
Figure 1. Scattering curves averaged and background subtracted. The black background curve oscillates around
zero, after the average background is subtracted. The smooth curves are fits with a Schultz distribution for
polydispers spherical particles to determine the mean particle radius and the relative distribution width
[1] P. S. Bauer, H. Amenitsch, P. M. Winkler, SAXS Annual Report 2014.
[2] P. S. Bauer, H. Amenitsch, P. M. Winkler. manuscript in preparation (2016).
-
29
P3 Membrane domains properties connections with their
lipid composition and ions in the aqueous phase
Michal Belicka(1,2)
, Santosh Prasad Gupta(1,2)
, Bing Sui-Lu(3)
, Rudolf
Podgornik(3,4)
and Georg Pabst(1,2)
(1) Biophysics Division, Institute of Molecular Biosciences, NAWI, University of Graz, Graz, Austria,
(2) BioTechMed-Graz, A-8010 Graz, Austria,
(3) Department of Theoretical Physics, Jozef Stefan Institute, SI-1000 Ljubljana, Slovenia
(4) Department of Physics, Faculty of Mathematics and Physics, University of Ljubljana, SI-1000 Ljubljana,
Slovenia.
Plasma membranes form natural semipermeable barriers in living cells defining inter- and
intracellular compartments. One of their specific features is the lateral inhomogeneity of their lipid
bilayers manifested by the presence of liquid-like disordered (LD) and ordered lipid domains (LO),
called also “rafts”. Similar behavior can be mimicked by ternary lipid model mixtures. In the present
work we simulated raft-like phase separation with the mixture of dioleoylphosphocholine (DOPC),
palmitoyloleoylphosphocholine (POPC), distearoylphosphocholine (DSPC) and cholesterol (Chol),
which is known to exhibit co-existing LD/LO domains. It is already known that replacement POPC
for DOPC in DOPC/DSPC/Chol mixture tunes the size of LD/LO domains from macroscopically
large those to LD/LO domains with typical size of nanometers. In the present work we focused on the
lipid bilayer structural changes caused by the above mentioned exchange. In addition, we considered
the bilayer structure changes in macroscopic LD/LO domains originated from the interactions of
monovalent ions (Cl-, Br-, I-) with LD/LO domains. Here we hydrated lipid films with aqueous
solutions of NaCl, NaBr and NaI with concentrations ranging between 5 and 400 mM. All
investigated monovalent ions followed previously published tendencies in the d-spacing concentration
dependencies. On the other side NaI displays significantly different behaviors in other observed
parameters than NaCl and NaBr, primarily in the central part of the concentration range, where the
bilayers correlation structure is almost completely destroyed.
-
30
P4 Towards a pump-probe x-ray scattering setup at the
Austrian SAXS beamline
Max Burian(1)
, Benedetta Marmiroli(1)
and Heinz Amenitsch(1)
(1) Institute of Inorganic Chemistry, Graz University of Technology, Stremayergasse 9/V, 8010 Graz, Austria
Through the advent of free electron lasers as well as ultrafast lab-based laser systems, highly time
resolved methods have risen to be essential tools to study the interaction between light and condensed
matter. [1] However, both of the named techniques lack the ability to directly track structural changes
on the atomic scale, immediately after irradiation. The pulsed nature of synchrotron light, on the other
hand, opens up a window at exactly these time- and length-scales: filming sub-nanometer structural
changes of liquid- and solid-state systems with picosecond time resolution.[2]
We are implementing such an optical-pump hard-x-ray-probe setup at the Austrian SAXS beamline at
the Elettra. A custom radio-frequency circuit that is in phase with the storage-ring-cavity synchronizes
all necessary devices and delivers the gating pulses required for x-ray bunch discrimination at the
detector. Further, a femtosecond laser will be installed to deliver high-power pulses in the VIS-IR
range to initiate light-induced phenomena in liquid and solid samples. We will present the detailed
setup with its specifications and provide an overview of the current challenges we are facing.
[1] B. W. J. McNeil, N. R. Thompson, Nature Photonics 4, 2010, 814-821.
[2] K. Jeongho, K. H. Kyung, … H. Ihee, Chemmical Communications 52, 3734-3749.
-
31
P5 In-Situ Crystallization Study of the Drug Carbamazepine
and its Precursor by Grazing Incidence X-ray Diffraction
Paul Christian(1)
, Christian Röthel(2)
, Roland Resel(1)
and Oliver Werzer(2)
(1) Institute of Solid State Physics, Graz University of Technology, 8010 Graz, Austria
(2) Institute of Pharmaceutical Sciences, Department of Pharmaceutical Technology, University of Graz, 8010
Graz, Austria
Amorphous films of the anticonvulsant drug carbamazepine are easily accessible by various methods
while the crystallization into specific polymorphs represents a challenging and time-consuming task.
In this work, the crystallization of drop cast carbamazepine at silica surfaces is investigated by atomic
force microscopy and both in-situ and ex-situ grazing incidence X-ray diffraction (GIXD).[1] The
pristine films grow with low crystallization rates into a triclinic polymorph, exhibiting poor
orientational order within films. However, if iminostilbene, a chemical precursor of carbamazepine, is
added to the solution, enhanced crystallization rates result. The individual components crystallize
phase-separated upon solvent evaporation without the formation of co-crystals. Iminostilbene reduces
the timescale of carbamazepine crystallization from several hours to minutes. Besides the change in
crystallization dynamics, iminostilbene induces order to the carbamazepine crystallites, evident as a
110 texture. In-situ diffraction data of intermixed solutions demonstrate that iminostilbene
crystallization occurs first (see Figure 1). The iminostilbene crystals then act as templates for
carbamazepine growth, whereby fully epitaxial growth is suggested from the data. The findings
motivate such an approach for other systems, as this solution processed, intrinsic epitaxial behavior
might be employed in up-scaled manufacturing processes.
Figure 1. Crystallization of a solution-cast carbamazepine/iminostilbene mixture as followed by in-situ grazing
incidence X-ray diffraction. Selected detector images (left) and the evolution of the diffracted signal with time
(right) are shown. The data show on-sets and crystallization dynamics of the two individual compounds.
[1] P. Christian, C. Röthel, M. Tazreiter, A. Zimmer, I. Salzmann, R. Resel, O. Werzer, Cryst. Growth Des.
16(5), 2016, 2771–2778.
-
32
P6 Structure and Mechanism of Legumain: A Multicatalytic
Enzyme
Elfriede Dall(1)
, Julia C. Fegg(1)
, Florian B. Zauner(1)
, Peter Briza(1)
, Hans
Brandstetter(1)
(1) Department of Molecular Biology, University of Salzburg, Billrothstraße 11, A5020 Salzburg, Austria.
Peptide ligases expand the repertoire of genetically encoded protein architectures by synthesizing new
peptide bonds, energetically driven by ATP or NTPs. Here, we report the discovery of a genuine
ligase activity in human legumain (AEP) with important roles in immunity and tumor progression that
were believed to be due to its established cysteine protease activity. Defying dogma, the ligase
reaction is independent from the catalytic cysteine but exploits an endogenous energy reservoir that
results from the conversion of a conserved aspartate to a metastable aspartimide [1]. Legumain’s dual
protease-ligase activities are pH- and thus localization controlled, dominating at acidic and neutral
pH, respectively. Their relevance includes reversible on-off switching of cystatin inhibitors, enzyme
(in)activation, and may affect the generation of 3d MHC epitopes. The aspartate-aspartimide
(succinimide) pair represents a new paradigm of coupling endergonic reactions in ATP-scarce
environments.
[1] E. Dall, J.C. Fegg, P. Briza, H. Brandstetter, Structure and mechanism of an aspartimide-dependent peptide
ligase in human legumain, Angew Chem Int Ed Engl 54 (2015) 2917-2921.
-
33
P7 Error-Disturbance Uncertainty Relations studied in
Neutron Optics
B. Demirel(1)
, S. Sponar(1)
, and Yuji Hasegawa(1)
(1) Atominstitut – TU Wien, Stadionallee 2, 1020 Vienna, Austria
It is an ineluctable feature of quantum mechanics that simultaneous measurements of certain pairs of
observables are impossible. This is reflected in the famous Heisenberg uncertainty principle,
published in 1927 [1], which is without any doubt one of the cornerstones of quantum physics. In its
original formulation, illustrated by Heisenberg`s famous gamma-ray microscope gedankenexperiment
(which is solely based on the Compton effect), it gives a rather heuristic estimate for the product of
the inaccuracy (error) of a position measurement and the disturbance induced on the particles
momentum. Shortly after, the uncertainty relation was reformulated in terms of standard deviations of
position and momentum, focusing only on the limitation of preparing a quantum system without
taking the accuracy of the measurement device into account [2]. Robertson generalized this relation
between standard deviations to arbitrary pairs of observables A and B [3]. The corresponding
generalized form of Heisenberg’s original error-disturbance uncertainty relation for arbitrary
observables however has been proven to be formally incorrect. A correct formulation of the error-
disturbance uncertainty relation (EDUR), including the unavoidable recoil of the measuring apparatus,
was given by M. Ozawa in 2003 [4]. The poster gives an overview of our neutron optical approaches
towards investigations of errordisturbance uncertainty relations via a successive measurement of
incompatible neutron spin observables, applying a polarimetric setup [5]. Though universally valid
Ozawa’s relations is not optimal. Recently, Branciard has derived a tight EDUR, describing the
optimal trade-off relation between error and disturbance, which is demonstrated in our experimental
results [6]. In addition, an information-theoretical or entropic approach of a tight noise-disturbance
uncertainty relation, including our neutron-optical experimental realization [7], is presented.
[1] W. Heisenberg, Z. Phys. 43, 1927, 172.
[2] E. H. Kennard, Z. Phys. A 44, 1927, 326.
[3] H. P. Robertson, Phys. Rev. 34, 1929, 163.
[4] M. Ozawa, Phys. Rev. A 67, 2003, 042105.
[5] J. Erhart, S. Sponar, G. Sulyok, G. Badurek, M. Ozawa, and Y. Hasegawa, Nat. Phys. 8, 2012, 185.
[6] S. Sponar, G. Sulyok, J. Erhart, and Y. Hasegawa, Advances in High Energy Physics 2014, 2014, 735398.
[7] G. Sulyok, S. Sponar, B. Demirel, F. Buscemi, M.J.W Hall, M. Ozawa and Y. Hasegawa, Phys. Rev. Lett.
115, 2015, 030401.
-
34
P8 Structural characterization of thaumatin-like proteins
from various species and comparison with the
structurally related plant-food allergens
M. Eder (1)
, J. Wortmann (1)
and W. Keller (1)
(1) Institute of Molecular Biosciences, University of Graz, Humboldtstraße 50, 8010 Graz, Austria
Thaumatin-like proteins (TLPs) exist in many plants, fungi, animals and bacteria and play important
roles in host defense, developmental processes and stress response. A lot is known about their
function in plants but only little about their tasks in other organisms. In general, TLPs seem to
participate in binding or degradation of β 1-3 glucans. TLPs consist of 200 to 250 amino acid residues
including up to 16 conserved cysteine residues. The TLP fold is composed of three domains. Domain
1 is a highly conserved β-sandwich, which is the core structure of the TLP molecule, followed by a
less conserved α-helical part (domain 2) and a small β-sheet (domain 3).
We are working on thaumatin-like proteins from so far neglected organisms such as Sgre1 from
Schistocerca gregaria (desert locust) and Arif from the bacterium Amycolatopsis rifamycinica. Our
aim was the expression of properly folded proteins and their structural characterization. To date the
vast majority of structurally characterized TLPs are plant food allergens. In this project we want to
elucidate the putative role of TLPs from organisms other than plants as allergens or aero-allergens. In
addition we investigate putative allergenic TLPs from mite (Tyrophagus putrescentiae), fungi
(Puccinia graminis) and TLPs from cedar pollen (Juniperus ashei, Cryptomeria japonica) which are
already characterized as allergens.
Since TLPs contain several disulfide bonds, expression is not trivial and therefore His-tagged TLPs
were expressed in E. coli ΔtrxB, Δgor. The recombinant TLPs were purified by IMAC
chromatography, followed by size exclusion chromatography, subsequent characterization by CD
spectroscopy and finally by crystallography.
For Sgre1 and Arif size exclusion chromatography verified the monomeric state of the proteins. CD
spectroscopy confirmed the mainly β-sheet structure and the proper folding of them. Crystallization
enabled us to get an insight into the structures of an insect and a bacterial TLP for the first time. Both
structures were solved at a resolution of 1.9 Å and showed that Sgre1 is quite similar to known plant
TLP structures, whereas Arif differs especially within domain 2. Work on the other TLPs is still in
progress. By now, no properly folded protein was obtained from these TLPs and refolding resulted in
soluble but mainly unfolded protein. Ongoing experiments focus on the expression of these proteins in
Pichia pastoris.
The recombinant TLPs will allow us to investigate their role as allergens as well as possible cross-
reactivities and their role as putative allergens.
-
35
P9 Joint SAXS/SANS Data Analysis of Membranes
Exhibiting Lipid Asymmetry
Barbara Eicher (1,2)
, Drew Marquardt (1,2)
, Frederick A. Heberle (3)
, Milka
Doktorova (4)
, John Katsaras(3)
and Georg Pabst(1,2)
(1) University of Graz, Institute of Molecular Biosciences, Biophysics Division, NAWI Graz, Graz, Austria.
(2) BioTechMed-Graz, Graz, Austria.
(3) Biology and Soft Matter Division, Joint Institute for Neutron Sciences, and Biosciences Division, Oak Ridge
National Laboratory, Oak Ridge, Tennessee 37831, USA.
(4) Department of Physiology and Biophysics, Weill Cornell Medical College and the Tri-Institutional Training
Program in Computational Biology and Medicine, New York, NY, USA.
Mammalian plasma membranes consist of an asymmetric lipid distribution along the two leaflets, in
other word the inner leaflet is compositional different from the outer. The asymmetry of the bilayer is
expected to affect various membrane properties, such as membrane potential, permeability, surface
charge, and stability. Bilayer asymmetry is also hypothesized to affect structural properties of the
membrane, like bilayer thickness and thickness of the single leaflets for example. However, due to the
difficulty of preparing asymmetric vesicles the majority of model membrane studies have been
performed on symmetric bilayers, where inner and outer membrane leaflets are identical in
composition. Of recent, we developed new protocols for the construction and characterization of
asymmetric vesicles amiable for scattering and NMR experiments with a well-defined inner and outer
leaflet composition. Quantification of bilayer composition and degree of asymmetry enables the
determination of transverse structural parameters, such as, area per lipid and the bilayer thicknesses of
the various phases in each leaflet. We are able to determine these structural parameters through a joint
analysis of small angle neutron scattering (SANS) data exploiting D/H contrast variation and small
angle X-ray scattering (SAXS). Here we report on the first probe-free analysis yielding insights into a
transbilayer coupling mechanisms. First results have shown a decrease in lipid packing density at
room temperature of the DPPC-rich phase (outer leaflet) compared to typical gel phase packing,
indicating a disordering effect from coupling to the fluid inner leaflet. Further, our analysis of fluid
DPPC/POPC asymmetric vesicles revealed that inner and outer membrane layers are not coupled to
each other.
This work is supported by the Austrian Science Fund FWF, Project No.P27083-B20 (to
G.P.).
-
36
P10 The high temperature stability of monoclinic Sr-lawsonite
Ende Martin(1)
(1) University of Vienna, Department of Mineralogy and Crystallography, Althanstraße 14, A-1090 Vienna
After the breakdown of amphibole and even talc, the main hydrous phase that can hold higher
amounts of hydrogen in the subduction zones of the Earth at higher P and T is considered lawsonite
e.g. [1]. After the investigation of the structure and p/T behavior of lawsonite in several publications,
previously, the RT-structures of itoigawaite (Sr-lawsonite) and Pb-la