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2010 Diamond

BCA Industrial Group Autumn Meeting at Diamond

This year’s BCA Industrial Group (IG) Autumn meeting was held on the 3rd and 4th of November at Diamond Light Source.  With over 40 delegates at the meeting discussions were lively.  The meeting report below was written by the winners of the student bursaries for the meeting.
Day 1

The IG Autumn meeting at Diamond certainly had an eye on the trend for practical applications of synchrotron science.  Welcomes from the meeting organisers, Dr Elizabeth Shotton and Dr Matthew Johnson, as well as the BCA vice-president Dr Dave Allan were followed by an introduction to Diamond from Prof. Trevor Rayment, the Physical Sciences Director at Diamond.  After providing some of the background to the applications of synchrotron science, Trevor encouraged everyone to review the proposals for the Phase III beamlines and to contribute to the shortlisted proposals, which focus on imaging, high throughput solutions, and the electronic structure of materials.

Dr Emily Longhi, an insertion device physicist at Diamond, guided us through the inner workings of a synchrotron, highlighting the importance of precision and angles as the final destination of the X-rays produced from the LINAC is to form a 100 micron beam targeted at a 100 micron sample!  It was very interesting to learn that the majority of the 5MW electricity is spent on powering and cooling for the 240 quadrupole magnets, 168 sextupole magnets and 48 dipoles.  3MW of electricity is used when the magnets are not powered, i.e. just for cooling the water. There are also two RF cavities (eventually there will be three).

The merits of high resolution powder X-ray diffraction were extolled by Dr Julia Parker, senior support scientist on the PXRD I11 beamline at Diamond.  High intensity, and high resolution powder diffraction are powered by an undulator, operating at 15 kEV, and data are detected by the multi-analysing crystals detector, with 9 crystals on five 2θ arms. Time resolved powder diffraction can be obtained through the use of the position sensitive detector, which has 90˚ coverage. The development of a High-Throughput Continuous Hydrothermal (HiTCH) flow synthesis reactor by Cockcroft et al. was aided by the rapid characterisation of a series of 66 unique nanoceramic samples with composition varying around CexZryYzO2-δ generated via this technique.  High resolution PXRD diffraction were acquired for the entire heat-treated library in <1 day, enabling the characterisation of a complete ceria−zirconia−yttria ternary phase diagram.

“Big opportunities for small molecules” were presented by Dr Harriott Nowell, beamline scientist on the single crystal X-ray diffraction beamline I19 at Diamond.  A broad range of experiments were presented, including a series of high-capacity hydrogen storage materials by Blake et al.  The ever-present issue (for this crystallographer at least!) of very small and weakly diffracting crystals benefited greatly from the high flux on I19, and sensible and solvable data were obtained.  The growing choice of sample environments will soon include a tuneable laser and chopper for performing pump-probe experiments, as well the installation of a Pilatus detector in EH2.  

Dr Michael Engel, the industrial liaison scientist for macromolecular crystallography (MX), enlightened us on the structure of proteins, and emphasized the many degrees of freedom which hindered facile structure solution for macromolecular crystals.  The somewhat small  complication of contending with secondary, tertiary and even quaternary structures is brought about via hydrogen bonding in the ‘local’ ordered structure.  This layered issue was highlighted in the structure solution of the Baculovirus polyhedra on I24 (Microfocus MX beamline), where the virus was packed so tightly around the protein that is almost impossible to break apart.  Other work on protein-ligand interaction and binding on I04-1 (fixed λ MX side station) is attempting to target structure based drug design.

An adventure into the strange world of microstructure and small angle X-ray scattering (SAXS) was led by Dr Claire Pizzey (industrial liaison scientist for scattering).  SAXS data gives an average of the entire bulk of the sample, and is particularly good for in-situ measurement and for non-volatile or opaque samples.  Data are complementary to microscopy, which gives an image of a single local area.  Studies carried out so far have included proteins, biomaterials, colloids, surfactants and catalysts.

Dr Michael Drakopoulos (Principal Beamline Scientist on I12) provided an excellent introduction to the very recently launched beamline I12, which is for joint engineering and environmental processing science (JEEP).  High energy X-rays (50-150 KeV) and a large beam size allow access to a wide range of diffraction and imaging techniques.  The ability of these energies to penetrate up to 20 mm of steel is very impressive, and recent studies of turbine blades by Rolls-Royce in EH2 highlighted the potential for improved characterisation and understanding of materials on an industrial scale.  A recent publication by Korunsky et al. highlighted the quantification of strain partitioning between phases and grain orientations within polycrystalline two-phase titanium alloy Ti–6Al–4V from white beam energy-dispersive diffraction patterns on I12, and the resulting data achieved a strain measurement accuracy better than 50 × 10−6.

Dr Anna Kroner-Niziolek (industrial liaison scientist-spectroscopy) introduced the wide range of spectroscopic techniques available at Diamond, and focused on the power of the photoelectric effect to describe the local structure of a wide range of materials.  Information about the elemental distribution, chemical speciation in the local environment and long range order can be acquired for complex inhomogenous materials and systems under realistic conditions.  A recent paper by Hart et al used data from beamline I18 (Microfocus XAS) to study the role of the chemical form of metal species in the unexplained failure of metal-on-metal hip arthroplasties.  The speciation of the metal was observed to be unrelated to the hip type, blood level of metal ions nor the method of tissue preparation, and so future research can potentially be focused on the human synovial tissue response to Cr(III)PO4.

Day 2
The meeting started with a tour of the facilities at Diamond.  Delegates were able to visit the beamlines which had been presented on day one of the meeting as well as getting to visit the inner workings of the synchrotron including the storage ring.  The tours stimulated a lot of discussion about applications of Diamond to various crystallographic problems. 
      
Left Photo: Dr. Alison Burke (Huntsman) on beamline I03                                                                        Right Photo: Dr. Julia Parker (Diamond) and Rebecca Sheridan (Pilkington Group Limited) on beamline I11.
Prof. Bill David (ISIS/University of Oxford) presented a talk entitled ‘From pharmaceutical research to the low carbon economy: the potential of powder diffraction’ discussing the advantages and multi use of powder diffraction.  The talk focused on 2 different drug molecules: paracetamol and zoplicone hydrates illustrating how the phase transitions involved with these compounds can be seen and analysed through the use of powder diffraction and the structures indexed and solved. The talk ended with a discussion of how powder diffraction data can aid the research into hydrogen storage in which an ammonia storage system is promising due to it being safe and efficient at room temperature, with powder diffraction investigating the variation of stoichiometry and polymorphism.

Prof. Chris Frampton (Pharmorphix) followed with a talk entitled ‘Structural Characterisation of Pharmaceutical Materials: Application of Synchrotron Methods’ in which the multi use of single crystal along with its advantages and disadvantages were outlined and how the use of synchrotron methods can overcome some of these problems.  The talk focused on a discussion about sodium diclofenac (an anti-inflammatory) in which only one structure was previously known, however a further two hydrate forms have been discovered. In this case the bright X-rays created at the synchrotron allowed enough data to be collected from a small weakly diffracting crystal to determine one of the diclofenac crystal structures. This in turn led to greater understanding of the stability of the sodium diclofenac drug phase.

‘Conformational Change of Mammalian Serine Racemase upon Inhibitor Binding’ was the title of the talk presented by Dr Myron Smith (Evotec) investigating the possibility of forming a mammalian serine racemase (protein in the brain).  After screening 3000 possible conditions, the optimised crystallisation conditions were discovered and the structure was solved using synchrotron X-ray crystallography, showing a closed conformation with both a large and small domain.  An alternative form was discovered under different conditions which had an open conformation, again solved using synchrotron X-ray crystallography.

The afternoon session commenced with Dr Emyr Macdonald (Cardiff University) presenting a lecture entitled the ‘Grazing incidence diffraction studies of in-situ thermal processing of organic photovoltaic film’.  Photovoltaic films have the benefits of being inexpensive, flexible and with the ability of covering large surface areas they are ideal substitutes to silicon in the capture of solar energy.  By using GI-WAXS, the annealing process was tracked in real time at 140˚C revealing a number of interesting trends regarding, crystallinity, domain size, disorder and expansion, all important factors when developing future energy sources.

Prof. Dave Rugg of Rolls-Royce gave an interesting and timely lecture, entitled ‘Crystallography and safety critical structures’ in which we are reminded of the role material science plays in the area of aerospace.  Designing and manufacturing gas turbines with the capacity to move 1.2 tonnes of air/sec and a reliability of 1:100 million flights place heavy demands upon both engineers and scientist.  It is clear that the understanding of macrostructure, in particular the residual stress, elasticity and grain orientation is critical for this to be achieved.  Through the use of such techniques as high resolution topography, it is possible to track the growth of cracks and with EBSB providing information on grain orientation, it is clear that high powered analytic technique have a central role to play within this area.

Dr Gemma Newby (University of Warwick/ESRF) lectured on ‘Pluronic Properties and Applications’.  The structural properties of these block polymers, which are widely used in biomedical and personal care products due to their biocompatibility and unique gel properties were discussed; SAXS and SANS, in addition to a unique rheo-SAS system, were employed for the investigation of shear alignment.  The effect of varying temperature and concentration were investigated using SAXS, with phase diagrams constructed based upon the combination of these results.

The final lecture of the day was given by Prof. Gopinathan Sankar (UCL) on the ‘Application of Synchrotron Radiation Techniques for the Determination of Structure of Industrial Catalytic Material’.  The lecture focused on aluminophosphate frameworks and the incorporation of transition metals in a high oxidation state, eg Co, Mn, Fe within the structure.  The crystallisation of CoAlPO-5 provided an eloquent example of how analytical techniques including EDXRD, SAXS and WAXS can be used in tandem to reveal to structural changes occurring within the system. 
Delegates at the BCA Autumn Group meeting held at Diamond

 Claire Murray (University of Reading), Laura Johnson (University of BIrmingham), Catherine Greenan (Queen’s University of Belfast)

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