Pressure-jump apparatus for time-resolved and static X-ray diffraction studies of conformational/phase transitions & structure in soft matter

Lead Research Organisation: Diamond Light Source
Department Name: Science Division

Abstract

There is currently a pressing need for the development of techniques that will allow experimentalists to probe the time-dependent structural behaviour of out-of-equilibrium soft condensed matter systems. An ideal technique for monitoring and triggering the structural evolution of such transformations within the millisecond timescale is time-resolved X-ray scattering, employing pressure as the triggering variable. The p-jump technique can be applied quite generally to the study of soft condensed matter and biomolecular phase transformations, such as lyotropic liquid crystal phase transitions, micelle-vesicle transformations, DNA unwinding, and protein folding. To this end we aim to develop and construct a millisecond pressure-jump X-ray cell for use at the Non-Crystalline Scattering beamline I22 at Diamond. We will also develop user-friendly apparatus control, integrated with the beamline software currently under development for I22. Although this apparatus is primarily designed for pressure-jump experiments, it can also be used for rapid scanning of pressure in the range 1 bar - 5 kbar, allowing pressure-temperature phase diagrams to be determined rather efficiently. It should also be noted that the cell will be capable of holding a fixed pressure for specific experiments.

Publications

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Brooks NJ (2010) Automated high pressure cell for pressure jump x-ray diffraction. in The Review of scientific instruments

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Richardson R (2011) Columnar Phases in Liquid Crystal Dendrimers: Variable Pressure X-Ray Diffraction in Molecular Crystals and Liquid Crystals

 
Description A high pressure cell for small and wide angle X-ray diffraction measurements of soft condensed matter samples has been
developed, with a fully automated pressure generating network. The system allows both static and pressure-jump
measurements in the range 0.1 - 500 MPa, and pressure-jumps can be performed in 5 ms both with increasing and
decreasing pressure. Key developments include: operating the pressure system has been made as simple as possible,
with a fully graphical remote user interface, which allows operation by an extremely broad user base with little previous
knowledge of high pressure technology and removes the need for lengthy training. Samples are loaded into the cell via a
dedicated port without moving the X-ray windows, facilitating accurate subtraction of background scattering, which can be
highly dependent on the window orientation. Pressure is generated by a motorized high pressure pump, so that the
operator does not need physical access to the high pressure equipment during use, improving safety, minimizing
installation time and allowing greater automation of the system. Highly configurable interfaces to the pressure system
allow simple integration with any synchrotron beamline but additionally, development in collaboration with beamline I22 at Diamond Light Source has allowed more extensive integration with this beamline, giving full sample environment data logging alongside the recorded X-ray patterns.
We have established a website dedicated to the pressure system (www.imperial.ac.uk/pressurecell/), which has kept the
user community informed about progress throughout the project, and will now provide a platform for information about the system and a repository for training documents, user manuals, etc.
Exploitation Route First experiments at I22 by a non-collaborating user (Prof. Rob
Richardson, University of Bristol) were very successful, with excellent quality data obtained from the samples
investigated. The sample environment is now available for routine operations and available to any user who requests it.
Sectors Chemicals,Environment,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology,Transport

URL http://www.imperial.ac.uk/pressurecell/
 
Description This Facility Development project has successfully delivered a p-jump cell for use on I22. It has not only been utilised by the originating academic group, Imperial College, but also in collaboration with I22 staff, groups from Bristol and Dortmund Universities.
First Year Of Impact 2010
Sector Chemicals,Healthcare,Pharmaceuticals and Medical Biotechnology
Impact Types Economic

 
Title P-Jump Cell 
Description p-jump cell capable of pressure jumps from atmosphere to 5kbar in 10ms. Temperature control also available between 0-120C 
Type Of Material Improvements to research infrastructure 
Year Produced 2010 
Provided To Others? Yes  
Impact Paper published by 1st external user group - Richardson, R. M., Hanna, S., Brooks, N., Gauthe, B., Pizzey, C., Agina, E., Boiko, N. & Shibaev, V. P. (2011). Molecular Crystals and Liquid Crystals 541 (1), 
URL http://www.imperial.ac.uk/pressurecell/index.htm
 
Description Open Days/Public Visits 
Form Of Engagement Activity Participation in an open day or visit at my research institution
Part Of Official Scheme? No
Geographic Reach National
Primary Audience Public/other audiences
Results and Impact At Diamond's open days, visitors are able to engage with scientists and engineers as part of a visit to the facility. They encounter researchers discussing their work, and are able to see the potential future impact of the research activity, for example, the potential applications of solar technology. The beamline takes part in open days for the public and for schools. Events provoke discussion with visitors, and raise awareness of current research For the beamline. Families often bring children to the facility, who are exposed to a range of science and engineering careers outside of the usual lab environment.

The open days at Diamond aim to change the perception of scientists, and how different areas of science interact and support one another. Feedback is regularly received that visitors encounter new areas of science which they were previously unaware of, which they now express an interest in. Teacher feedback of our schools events reports that visiting the facility increases engagement with their subjects and enables students to consider careers in science. I22 regularly participates in the days relating the work carried out in both grant held projects such as the OPV project and Pressure Cell Project as well as other User driven science projects carried out on the beamine.
Year(s) Of Engagement Activity 2006,2007,2008,2009,2010,2011,2012,2013,2014
URL http://www.diamond.ac.uk/Home/Events/Inside-Diamond---Public-Open-Days.html