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A journey through ISIS A behind the scenes look at using neutrons and muons for cutting-edge science A journey through ISIS

Contents Welcome to the journey!

The start of the journey Page ISIS at the STFC Rutherford Appleton 1 Neutrons and muons for science ...... 2 Laboratory in , UK, provides unique sources of both The journey’s aim pulsed neutrons and muons for 2 Exploring drug delivery ...... 6 exploring the properties of matter by Different routes to take measuring the locations of atoms and the forces between them. 3 The ISIS instrument suite ...... 8 Permission to travel ISIS employs more than 300 highly- 4 Submitting a proposal for ISIS beam-time ...... 12 qualified scientists, technicians, engineers and administrative staff, Getting ready to go who have unique skills. Their work 5 Preparing for the experiment ...... 14 ensures that the science carried out by research groups is first-class. ISIS Support along the way teams looking after the accelerator, Operating ISIS ...... 18 6 beamlines, instruments and computers The heart of the journey work around the clock to ensure that 7 Running the experiment ...... 22 experiments are successful.

At journey’s end We will follow the journey that one 8 After the experiment ...... 26 research group makes as they use ISIS to further their research goals – from Helping others to travel the initial idea for an experiment, 9 Training for ISIS users and staff ...... 28 through submitting a proposal, to ISIS Scientists ...... 30 carrying out the experiment and analysing the results. Along this Further information ...... 32 journey, we go behind the scenes to meet the people who work at ISIS and learn about how the facility operates.

1 e start of the jo A journey through ISIS Th urney…

Extracted proton beam WISH 800 MeV SYNCHROTRON

offSPEC INTER Neutrons and muons polREF

SANS2d for science MICE Extracted proton beam NIMROD – HRPD 70 MeV H Linac LET

ISIS is a world-leading research centre serving the UK Neutron techniques and international scientific community have distinct EC Muon Facility benefits: MuSR HiFi • Neutron studies can Research carried out at the science, environmental and RIKEN Muon Facility ENGIN-X What do neutrons tell us? EMU range from the distances microscopic scale – whether into the geological sciences, and increasingly ARGUS between atoms natural world or manmade materials the life sciences. Neutrons are one of the two (0.1 nanometres) to those – has been responsible for many of constituents, along with protons, of TOSCA associated with the the major improvements in our The UK has a major facility, ISIS – HET HiPr atomic nuclei. Fired into samples, INES GEM structures of large quality of life. based at the Rutherford Appleton IRIS they can tell us where atoms are and POLARIS molecular arrays (over Laboratory near and operated how they are moving deep inside MARI OSIRIS 500 nanometres). Sample objects can now be studied by the Science and Technology materials. LOQ with various kinds of radiation to Facilities Council – which provides MERLIN • Neutrons are penetrating CRISP SXD reveal the locations of atoms and neutron beams for research. This atom’s-eye view helps us to SURF enough to reach deep the forces between them at the Academic research groups from explain why substances have the VESUVIO inside a sample. ROTAX atomic and molecular levels. An across the UK, and further afield, can MAPS properties they do – for example, PRISMA • They are non-destructive increasingly important approach is apply for ‘beamtime’ at ISIS. how they conduct electricity, why SANDALS so can be used on the use of beams of electrically they have particular magnetic delicate biological neutral subatomic particles – ISIS experiments provide detailed properties, or how tough they are – samples. neutrons – which can scatter off insights into the arrangement and and so can help us make new materials in a way that gives just behaviour of atoms and molecules in substances that are useful in • Neutrons are very such information. Neutron scattering a material, which are not obtainable everyday applications. sensitive to light atoms techniques are now applied across by other methods. such as hydrogen. many scientific disciplines – physics, When neutrons interact with the • Atoms such as hydrogen, chemistry, engineering, materials atoms in a solid or liquid, they in a selected sample scatter off the nuclei in a component, can be characteristic manner that depends substituted by a variant on the atomic positions. The angles with a different number at which the neutrons emerge from of neutrons in the nucleus the sample tell us the distances – an isotope – which between the atoms. Any changes in scatters differently and the neutron energies as they pass so picks out that through the samples also reveal the component. motions of atoms and molecules. • The structure of surfaces and interfaces can be revealed by bouncing neutrons off them – the technique of neutron reflectometry. • Because neutrons have a magnetic moment, they are sensitive to the often subtle electronic structures of magnetic and superconducting materials. The newly-built ISIS Second Target Station The ISIS synchrotron 2 accelerator 3 start of the The journey A journey through ISIS

Neutrons and muons The ISIS pulsed muon source Muons offer an ingenious way of exploring atomic-scale structure in solids and liquids, for science providing complementary information to that gleaned from neutron experiments Muons are produced from a thin them once inside affects their graphite target when the spins in a way that provides energetic proton beam from the atomic-level information. Muons Making a neutron beam A wide range of A bright future for ISIS ISIS accelerator passes through. can be used to study a broad experiments and They survive for only two range of materials, including millionths of a second but that is magnetic and superconducting Neutrons can be released by firing instruments A second target for neutron bursts of accelerated protons at a production – Target Station 2 – with a long enough to carry out samples, molecular systems and metal target, knocking out, or suite of new beamlines and experiments with them. The chemical reactions, Once the neutrons escape from the spallating, neutrons from the target’s instruments, will increase capacity muon beams are steered to semiconductors, battery target, they are slowed down nuclei. This spallation neutron and widen research potential at ISIS. seven experimental areas, three materials, organic materials used (a process called moderation) and approach has been extremely Further novel improvements are being in the ISIS European muon in displays – to name but a few. directed along beamlines to some successful. It is being taken up made to increase the intensity of the facility and four in the Japanese- 20 instruments where experiments elsewhere in the world and will neutron pulses, so ISIS users can look run RIKEN-RAL facility. The RIKEN-RAL facility also take place. carries out studies including Muon beamlines of certainly be the basis of any future forward to the prospect of carrying the ISIS European international neutron facility. out even more exciting science. The main technique employed muon-catalysed fusion – an muon facility Each instrument is designed for a using muons relies on the fact exotic mode of nuclear fusion specific type of experiment. For …and muons that they have a spin and so which happens at low example, large polymer networks are behave like minute magnets. temperatures, though not yet studied using an instrument which Muons readily implant efficient enough to provide As well as producing neutrons, the measures neutron scattering at small themselves in samples, and the energy – and other atomic and proton pulses are also directed at a angles (small angle neutron magnetic environment around nuclear investigations. target designed to produce muons, scattering, SANS). which are another useful probe of the properties of materials (see opposite).

The basic requirement for producing neutrons and muons is a powerful accelerator system to generate an energetic proton beam. ISIS has several accelerator stages, culminating in the circular synchrotron accelerator 50 metres across. This produces protons travelling at 84 per cent of the speed Adrian Hillier of light. inspects one of the muon spectrometers

ISIS science covers a wide range of length scales – from the distances between atoms in crystals to large molecular structures and magnetic domains

Neutron experiments can be used to study:

• Advanced materials such as • Compounds with exotic • Proteins, DNA and cell catalysts, hydrogen-storage magnetic and electronic membranes materials, battery materials properties, including high- • Complex biomedical materials temperature superconductors • Nano-materials and structures • Disordered materials and liquids such as magnetic thin films • Engineering stresses and strains used in computer applications in components and welds • Rocks and minerals – terrestrial and planetary geology • Molecular materials such as • Plastics, detergents, food 4 pharmaceuticals products and paints • Archaeological artefacts 5 The journey’s aim A journey through ISIS

Exploring People spotlight drug delivery

The complex structure of mucin, found in the respiratory, gastro-intestinal Understanding the basic behaviour of soft matter and reproductive tracts. Researchers want to know how drug-delivery agents move through it is one of many research areas that benefit from The mucus barrier addition of the polymer? Does the Peter Griffiths polymer bind to the gel? neutron scattering studies Peter has been working with During the past two years, Peter has polymers and other systems that been working with one of his PhD SANS carried out on appropriately self-organise at the nanoscale, such deuterated samples, together with A growing area of ISIS research is the tissue environment affected their students Paola Occhipinti on a as detergents and colloids, for Now you see it... measurements of viscosity, rates of nearly 20 years. He did his PhD at study of ‘soft matter’ in which weak rates of diffusion. A combination of particular drug-delivery issue. diffusion, and nuclear magnetic the University of Bristol in 1991, electrostatic interactions play a experiments which include small One technique that neutron studies becoming a lecturer at Cardiff in Organs such as the respiratory, resonance studies, can build up a significant role in creating complex angle neutron scattering (SANS) have to offer is that of isotopic 1995 and then Reader in 2004. gastrointestinal and reproductive picture of polymer-mucin interaction. structures and behaviour. Soft matter could provide some answers. substitution combined with ‘contrast tracts are coated with a layer of includes polymers, surfactants and matching’, in which specific parts of mucus, tens of micrometres thick, Recently, they carried out Paola Occhipinti biochemical materials, and so its The power of neutrons a complex molecular assembly can which may pose a significant barrier experiments at ISIS investigating the study is important in health and be highlighted. This is done by Paola came to Cardiff after to drug delivery agents. In the case of interaction of mucin with a typical finishing a Master’s at the biological research. SANS can probe structures at scales substituting selected hydrogen atoms diseases like cystic fibrosis, the mucus model polymer polyethylene glycol University of Catania in Italy. from around 1 nanometre to more with deuterium (D), which scatters (PEG), and also with “I was always interested in Peter Griffiths and his research layer may be many times thicker. than 100 nanometres, which makes differently. a dendrimer – a chemistry applied to biological group in the Chemistry Department at it ideal for studying the conformation systems so I applied to work on Mucus is composed of mucin, a small but Cardiff University investigate soft and behaviour of synthetic polymers, For example, in a two-component this project. I thought it would be gel-like network of glycoproteins, highly challenging as it involved new matter and are frequent ISIS users. as well as biomaterials. system such as a protein mixed with and Peter and Paola were interested branched techniques to learn,” says Paola. a polymer in water, a proportion of in what factors affected how various polymer. One of those techniques was Six years ago, Peter heard a colleague Neutrons are particularly effective at the aqueous solvent may be neutron scattering at ISIS. “The polymers diffuse through it. Does Ruth Duncan give a talk on polymer homing in on the positions of the substituted with heavy water (D O) first time I visited ISIS I was 2 the structure of mucin change on amazed at the size of the site; therapeutics – using long-chain hydrogen atoms. The locations of such that its scattering strength molecules to ferry small drug I was very impressed with the surrounding water molecules can matches that of one of the facility, she adds.” molecules into cells. Targeted delivery also be established, as they have a components. This component is then of pharmaceuticals and genes to significant role in modifying the rendered invisible so that only the particular locations in the body is a conformation and activity of other component is seen (see below). key area of medical research but is biomolecules. “We make as much use of this difficult to achieve. approach as we can,” says Peter.

Professor Duncan commented that there was a lack of fundamental information on the three-dimensional arrangements of the polymer chains Contrast matching to highlight shell and core components (their conformation) and how quickly they diffused in biological tissues. of surfactant particles dissolved in water Peter realised he had the experience No contrast matching Surfactant shells Deuterated surfactant and experimental tools to uncover contrast-matched with cores contrast-matched the information needed. a mixture of normal with deuterated and deuterated solvent solvent In collaboration with Cardiff’s School Surfactant shell Surfactant core of Pharmacy, Peter started looking at factors affecting how a polymer- bound therapeutic negotiates the complex delivery-pathway from initial injection, or absorption, to the The genetic disease targeted cellular structure. The cystic fibrosis results in central issue was how interactions Mixture of normal and increased production of Deuterated water Deuterated water 6 between polymers and the local deuterated water mucin, making drug 7 treatment difficult erent routes Diff to take A journey through ISIS

The ISIS People spotlight instrument suite

Target Station 2 “We had to learn how to move a ISIS has dedicated instruments suitable for ‘mountain’ to put up the building, Target Station 2 is ideal for the study as well as designing and building a wide range of experiments of complex materials at longer the proton beamline, target station, length-scales. Neutrons are neutron beamlines and Richard Heenan instruments, but it’s gone to budget produced by the proton pulses Richard Heenan has been LOQ and schedule,” he says. ISIS currently has over 30 neutron Small angle neutron 4 metres away, which can detect the hitting a tungsten target surrounded instrument scientist ever since it and muon instruments which scattering with LOQ positions and times of arrival of the by novel solid-hydrogen/solid started operating in 1984. He had provide diverse and complementary impinging neutrons. “The methane moderators which slow the already gained considerable information on samples. These advantage,” says Richard Heenan neutrons down in just the right way. experience in diffraction About 40 different research groups techniques during his PhD at the include diffractometers designed to one of the scientists responsible for carry out an average of 80 University of Reading and later as a analyse atomic-level structures, and the instrument, “is that you can Harry Jones, head of the ISIS Target experiments a year on the SANS postdoctoral researcher. Not reflectometers for studies of surfaces probe a large range of distances in Division, has been responsible for surprisingly, Richard knows the diffractometer LOQ – of which Peter and interfaces. A suite of the samples in a single project-managing the construction SANS user community well and is Griffiths’ team is one. able to offer considerable expertise spectrometers measuring the measurement.” of TS-2, including all the civil to help new users. energies of scattered neutrons engineering. LOQ is a relatively simple provides rich information about instrument, consisting of a 11-metre Continuous improvement atomic motions and magnetic and evacuated beamline down which the electronic behaviour in advanced neutrons fly towards the sample. ISIS instruments are continuously materials. being upgraded. This is carried out in Once scattered by the sample, they Gemma Newby from the University of hit a fixed two-dimensional detector, partnership with the user community Reading University preparing LOQ for who will always aim to stretch measurements of polymer flow. instrument capabilities to their limit. Providing access to distance scales from 1 to 100 nanometres, LOQ is used to At the moment, the length-scales investigate the shape and structure of large molecules and molecular available with LOQ do not reach those assemblies including polymers, particle relevant to understanding the suspensions and biomolecules behaviour, for example, of large protein assemblies in cell membranes. The ISIS Second Target Station has Harry Jones been designed to overcome this Harry Jones has worked at the limitation as well as to greatly Rutherford Appleton Laboratory for increase the number of neutrons 42 years, starting off at the age of 22 produced. as a craftsman. He was supported for four years to study mechanical engineering at Oxford Polytechnic (now Oxford Brookes University), subsequently becoming one of the first engineers in the laboratory graduate training scheme. Harry worked on a variety of high-energy physics equipment, and by 1984, became responsible for ISIS project engineering. He is now in charge of both target stations.

Anne Terry of ISIS with members of the Silk Group 8 during an experiment on LOQ to study 9 spider silk proteins erent routes Diff to take A journey through ISIS

The ISIS People spotlight instrument suite

SANS2D

The Second Target Station will feed seven new instruments, with more to be added over coming years. One of David Turner the first is a new state-of-the-art David Turner came to ISIS four SANS instrument, designed by years ago, having spent 10 years Richard Heenan in conjunction with at Siemens, which also sponsored the user community to measure over him to do an engineering-design degree. Coming from industry, an even wider range of distance David says he was surprised to scales. It will provide spectacular find how much technical gains for researchers studying soft information was shared with matter, complex materials and other facilities. “There’s also a lot biological samples. of direct liaison with the The SANS2d vacuum tank arriving at ISIS scientists and it’s very much designing in a team,” he says. "The increased flux and resolution “What I like most is that of TS-2 will enable us to study even Two 1-metre square detectors can be aircraft doors, that close up the everything you design is unique; more challenging systems, in independently moved inside a gaps between the moving parts,” it makes the job very interesting.” particular to probe the dynamics of 13-metre-long vacuum tank he comments. self-assembly processes. This is a according to experimental needs. great and much needed boost for Once the design and manufacture UK science," says Peter Griffiths. Project engineer, David Turner, were completed, the installation turned the scientists’ sketches and team took over. ISIS engineer specifications into reality, drawing up Jeremy Moor works on instrument detailed engineering drawings and installation. “The layout starts from arranging manufacture. “One of the the location of the sample and the technical challenges was floor is marked out from designer’s maintaining a vacuum between the drawings”, he says. “We work with moving sections of beam the drawing office and ‘heavy gang’ collimation in front of the sample. in building a whole beam-line and We came up with inflatable vacuum instrument from scratch.” seals, based on those used in Jeremy Moor

Jeremy Moor did a mechanical apprenticeship at AERE Harwell and has a background particularly in survey work. He has applied his skills in various ISIS departments, presently focusing on the Japanese RIKEN- RAL muon facility (p.5), particularly gas handling and cryogenics, together with working on the muon production target. Jeremy says there is always a lot to learn: “You can’t help getting interested in the experiments. The scientists are always very appreciative of your efforts and their enthusiasm rubs off on you.”

Debbie Greenfield, head of the ISIS Instrumentation Division, at the David Garland from Alstec during the 10 Second Target Station construction of the detector frame for the 11 Second Target Station NIMROD instrument ion Permiss to travel A journey through ISIS

The ISIS online People spotlight Submitting a proposal proposal system

All proposals have to be for ISIS beamtime submitted via a Web-based system. Guidelines are given on the ISIS website, and users are asked for the number of days required, details of the Other forms of access sample and sample Once a research team has decided on an ISIS environment, information on • Rapid access: if samples have a previous publications from experiment, it is time to put in a proposal short shelf-life or the research is ISIS work, together with a exceptionally high-priority, two-page description giving John Evans researchers can choose the the science case and John Evans, who has been Chair of Access to an ISIS instrument is free to The ISIS website provides detailed ‘rapid access’ route, whereby a experimental details. This the Crystallography Panel for two university researchers. Academic instructions on proposal proposal can be submitted at approach not only helps years, is Professor of Chemistry at groups must first put in a proposal, requirements and the online any time and reviewed by Panel the review process but also Durham University and researches outlining the scientific case for an submission process. In just two sides into a wide range of scientifically members, and then scheduled allows sample-safety issues and industrially important experiment, against one of two of A4, researchers must explain why as soon as possible. to be assessed. materials. He says he reads every deadlines a year – in April and and how they want to carry out the proposal submitted to his Panel – October. One of seven Facilities experiment. • Xpress access: some This automated proposal “at least two whole weekends’ Access Panels, composed of national instruments including LOQ offer system creates a database work”. He adds that the Panel puts in a huge amount of time in and international experts, reviews the John Evans, who chairs the a service whereby a few that will benefit users in the reviewing the applications: “We proposal, after which days may be Crystallography Facility Access samples suitable for routine future. Tom Griffin, one of try to be as fair as possible.” allocated for the experiment during Panel, says that users must analysis can be sent by courier the software developers the next operational run of ISIS. communicate the excitement of the for measurement. responsible, has also been science being done. He stresses the Andrew Willis (University College ) working on taking the system discussing a crystallography proposal Key to being awarded beam-time is importance of providing the right • Programme access: UK further. The aim is to have a good preparation of the proposal. Less amount of experimental detail, the researchers can apply for fully searchable web-based experienced users should always first number of days needed, as well as Usually about 60 days are available beamtime to carry out a series system that ties up all the seek advice on the experiment’s evidence of any supporting on each instrument for each period, of experiments that are part of information regarding an technical feasibility. Steve King, who laboratory work carried out. and so beamtime is then allotted a research programme funded experiment, from proposal is also a LOQ instrument scientist, “Groups who prepare excellent until the time is filled. In the case of by a grant. stage to completion. At the advises that they should make contact well-argued and clear proposals an unsuccessful proposal, the Panels moment, the system is being as soon as possible. “We can then stand the highest chance of being always give feedback on the reasons road-tested before being start to flesh out what the awarded beam-time,” he notes. for rejection. They also aim to made available to the researcher really wants to do,” says achieve a balance across subject community. “The system has Steve. “For example, we can advise Assessing proposals areas. Panel members enjoy the tremendous potential, on deuteration of sample scientific interactions of panel especially if we could Tom Griffin components. We try to help new include experimental The Panels consist of academics, meetings and look forward to Tom Griffin first worked at ISIS four users as much as possible and will each with expertise in representative attending. results,”says Tom. years ago during a sandwich year provide feedback on the draft scientific areas. Each of the 500 or as part of his degree course at proposal,” he adds. so proposals submitted in each UMIST (now amalgamated with the University of Manchester). After his allocation period is read by members degree he returned to a permanent of the relevant Panel. The Panels job at ISIS as a software engineer. then meet over a couple of days, The Diffraction FAP in mid-debate during which the scientific excellence of each proposal is discussed.

Members of the Large Scale Structures FAP 12 reviewing proposals 13 Getting ready to go A journey through ISIS

Preparing People spotlight for the experiment

Once a proposal has been approved, preparations

for the experiment begin in earnest Steve King

Steve King is one of 70 instrument scientists who help visiting teams Following the recommendations of over a range of temperatures may components, often has to make to get the best out of their the Facility Access Panels, the require furnaces or cryogenic special sample-holders for users, for experiments. Their role is to ensure instrument scientists start to plan equipment, while others might need example, a narrow cell to contain a that the beamline is always in the schedule for the next ISIS run. pressure cells or an atmosphere of a liquid. “Scientists tend to provide “tip-top condition” and to give visitors full support when carrying particular gas. ‘fag-packet’ drawings of what they out the experiments. Like all the “We try to be flexible and ask users want,” he laughs. “One scientist instrument scientists, Steve has a when they would like to come,” Chris Goodway, head of the section wanted a crystal to be suspended PhD, in his case in polymer and says LOQ instrument scientist Steve supplying pressure, furnace and gas- in the beam without anything colloid science from the University King. “We may find that people handling systems, says: “We like to touching it. Using pictures, we of Bristol. He first came to ISIS as a University of Bath researchers Adrian Hawley and Ben O'Driscoll in the ISIS sample student in 1986, later joining the have to delay because samples are know the requirements before the established how to achieve what preparation laboratory during their studies of polymer-surfactant interactions ISIS staff in 1989. taking a long time to make, but if a experiment is scheduled so that we he wanted.” Jim says he’s machined student is finishing a PhD soon, we can ensure we have the equipment a vast array of materials from plastic will try to accommodate the available.” He and his colleagues to gold, including preparing samples experiment quickly.” also look after the equipment while of “weird and wonderful” alloys in use, instructing the users if used in aircraft wings. Sample environment necessary, and remaining on-call during the experiment. One of the instrument scientists is also assigned as the local contact for Sometimes a new piece of kit has to the visiting team, and will discuss be specially designed and made in the experiment in more detail. the ISIS machine shop. Jim Buckel, Experiments involving measurements who specialises in machining small Chris Goodway

Chris Goodway has been working at ISIS since 1991, having done an apprenticeship in mechanical engineering at Harwell. After working in the support workshops, he was eventually promoted to technician grade in the sample environment laboratory. “I enjoy the work enormously,” he says. “Each experiment is completely different and we can help the scientists achieve their goals.”

Jim Buckel

Jim Buckel (left) did his apprenticeship at Harwell, like many ISIS technicians, and he has worked in the machine shop for more than 20 years. Jim enjoys the fact that the work is non-repetitive. “I do like a challenge.” he says, Vicky Kett of the University of Belfast Arjan Houtepan of the University of and is most proud of a graphite-tile working on protein samples for studies Delft mounting his semiconductor cleaver he designed and made for of the effects of freeze-drying on LOQ nanocrystal samples for muon studies one of the beamlines.

14 15 Getting ready to go A journey through ISIS

Preparing People spotlight for the experiment

Sample preparation versions of the polymers were mixed “We are also available to help The user has to fill in a COSHH with mucin in deuterated water such with making sure samples are (Control of Substances Hazardous to Scientists usually prepare their that the SANS experiments would appropriate for neutron scattering Health) form, and, if necessary, Steve samples in advance of the highlight the structure of the mucin experiments. Many biological advises on the correct way to handle experiment. For Peter Griffiths’ in the presence and absence of the experiments aren’t as successful as and transport the material. Another Cameron Neylon polymer so as to probe any changes they should be due to issues with important aspect is radiological research, this might include buying Cameron Neylon, who is senior deuterated water and polymers. in its structure. The rest of the sample concentration or purity. safety. A neutron beam can induce scientist for biomolecular sciences, Many standard deuterated samples were then prepared on-site SANS in particular requires high radioactivity in samples, and the started as a biochemist at the compounds are commercially using sample-preparation concentrations and very good potential for this is considered. Australian National University in available but more particular laboratories at ISIS. sample homogeneity and we can Canberra studying protein-DNA and help to get that right,” enzyme-substrate binding. He materials need a specialist supplier or The User Office realised the potential of neutron in many cases to be made to order. The facility has five laboratories for Cameron comments. scattering to probe these crucial preparing samples. New facilities are At the ‘creature-comfort’ end of interactions, so took up the “We try and do as much sample being built for TS-2. One lab is Sample safety preparing for an ISIS experiment are challenge offered at ISIS to develop dedicated to the needs of biological the application of neutron preparation beforehand as we the ISIS User Office staff, who diffraction and spectroscopy in the can,” says Peter. “Usually there’s a experiments. Peter Lock of University College London All samples and sample regularly check the experiment life sciences. Opportunities in this period of frenetic activity in the sealing phenol-clay into a high-pressure, environments for experiments have scheduling in the online proposal area will expand as more “We can help with biological high-temperature can for neutron instruments are built and week leading up to the experiment. studies of molecular diffusion to be evaluated for safety, and this is system and send out emails to The polymers may take a few hours sample preparation issues including commissioned on the Second carried out by Steve Roberts, visiting groups confirming Target Station. to dissolve; we prepare the samples working with users to express and support laboratories manager. “We experiment dates and reminding for the first day’s measurements prepare biomolecules in bacteria look at the standard chemical them to send back the COSHH form the day before so they are on a large scale, or just helping properties such as toxicity, together with their accommodation reasonably fresh.” out with choosing the right flammability and corrosiveness, and and travel requirements. sample cells,” says whether special sample-handling Accommodation is available on site To obtain some of the mucin Cameron Neylon, whose equipment is needed,” he says. at Ridgeway House or off-site at the samples, Peter and his team had to role is to help biologists to Cosener’s House in Abingdon. extract material from the lining of carry out neutron pigs’ stomachs – “not nice material experiments successfully. to work with”, he says. Deuterated

Steve Roberts

Jennifer Riesz from the University of Steve Roberts trained in applied Queensland preparing samples of chemistry at Kingston University, melanin precursors for study on the working in both the paint and oil Tosca instrument industries before coming to work at ISIS. Like many ISIS support staff, he is on a 24-hour call-out rota. “Sometimes it’s a student who just wants to know how to switch something on, but that’s part of the interest of the job. Working with academics is much more interesting than working in industry. They love talking about their work and you find out about a wide range of things from archaeology to materials for hydrogen storage and solar Katarzyna Morawa from the panels,” he says enthusiastically. University of Reading and Dario Stacchiola from MPI Berlin warming their cryostat during experiments to 16 study catalysis on Tosca 17 port along Sup the way A journey through ISIS

Operating ISIS People spotlight

While preparations for experiments are being made, Dan Faircloth specialist teams of physicists, engineers and Dan Faircloth has a PhD in high- voltage electrical engineering and technicians work hard to ensure that the production Ben Pine and Bryan Jones of the ISIS synchrotron group has been working at ISIS for six discussing beam diagnostics modelling years. “ISIS is a lovely place to work. When new people join us of neutron beams operates reliably at optimum I always tell them that the job is Setting up and “We provide on-call 24-hour what you make of it,” he says. monitoring the support for any operational efficiency 24 hours a day, 7 days a week problems,” says Dean. We establish accelerator where the problem is and call out the relevant crew to fix it.” Producing neutron beams by the sources last for between 20 and 30 “Special suits and breathing Maintaining the machine spallation method involves a days before they have to replaced. apparatus are required while we performance is essential to providing Sarah Whitehead and Tony complex engineering infrastructure “Keeping the source in optimum equip the cells with tools and optimum experimental conditions Kershaw of the Diagnostics Section to accelerate particles to high condition is often called ion cameras,” says Dave Haynes of the for users. The job of Dean Adams monitor the location of every proton energies. Each section of the ISIS sourcery,” says Dan. “We have to Targets Section. “Changing the and his team is to set up the pulse via beam monitors situated machine is looked after by a highly maintain the discharge in chaotic moderator is complicated but we’ve accelerator for each user run. The along the synchrotron. “If there are skilled and experienced team. equilibrium to produce as many H– done it so many times that it is whole facility works under three consecutive pulses that are Dave Haynes extremely tight tolerances. The ions as possible. If you switch off routine,” notes Dave. outside the tolerances, we switch Dave Haynes is another Harwell The process starts with an ion source the ion source and then start it up proton beam must remain very the machine off,” says Tony. “We apprentice who is now to produce negative hydrogen ions again, its behaviour changes. They stable, which means that, for aim for at least 90-per-cent Experimental Halls Group leader (two electrons bound to a proton, H–) are fickle beasts, which is what example, power supplies must availability of the machine for over with wide responsibilities. “I might which are injected into a chain of makes the ion-source technicians remain constant to within 0.01 per have ended up working in a car the 40 to 50 days of user time,” factory but instead I’ve got a linear accelerators. Then stripped of superstitious. They don’t like to talk cent. Any loss of beam as a result of he adds. better job than I ever thought the electrons by a thin piece of about a source because they think it it hitting the accelerator sides will I could have,” enthuses Dave. aluminium oxide foil, the bare protons can hear you,” he jokes. directly affect the quality of the final “The work is interesting and enter a circular accelerator 50 metres experimental beams, as well as everyone is helpful.” across called a synchrotron. A collection of 10 sources, which are damaging the machine. made at ISIS, is kept ready to go. “We During acceleration they go round are building up a database of 10,000 times before being kicked operating conditions and failure out of the synchrotron towards the modes so we can improve targets where neutrons and muons reliability,” says Dan. are produced. Protons on target Ion sourcery Neutron production also depends Sarah Whitehead Originally based on Russian upon the target systems being kept technology, the ISIS ion source in good condition. Although a target Sarah Whitehead read physics at University of Manchester and works by generating a discharge lasts up to five years, the surrounding specialises in the software side of plasma in hot hydrogen gas fed with liquid methane moderators (for TS1), beam diagnostics, interpreting data caesium vapour. This creates the H– which slow down the neutrons, do from the monitors. ions which offer the easiest way of degrade and have to be changed feeding particles into the every other run cycle. Because the Tony Kershaw synchrotron accelerator. whole system becomes radioactive, The ISIS synchrotron accelerator at changing the moderator requires a Tony Kershaw (left) has been at the point where the proton beam is ISIS since just after it was “We are now the leading operators remote-handling cell. extracted to the target stations and developers of this type of ion commissioned, having done an electronics apprenticeship at source,” says Dan Faircloth, head of Tony Kershaw assesses Harwell and has worked in the the ion source section. The ion TS-2 beam production in Diagnostics Section for 16 years. 18 the ISIS main control room 19 port along Sup the way A journey through ISIS

Operating ISIS People spotlight

Mikie Ruddle inspects the Staying In control ISIS uses several kinds of chopper, Scintillating work TS-2 target and moderator the simplest being a blade which sits during assembly The routine running of the just beyond the target and rotates at Each neutron instrument consists of accelerator is monitored from the the same frequency as the neutron many components, each of which is Tom Noone ISIS Main Control Room by a duty pulses. It eliminates high-energy, looked after and developed by officer and three assistants working fast-moving neutrons while letting groups within ISIS. For example, ISIS Tom Noone has been a duty officer the bulk of them through. Further for four years and has a in three daily shifts, 365 days a year. develops its own neutron detector background in electronic down the beamlines are disc arrays, which comprise mainly gas engineering of control systems: Duty officer Tom Noone says to choppers with slots that allow and scintillating devices. The latter “The first six months of being a maintain the machine at maximum neutrons in selected energy bands to consist of material that emits light duty officer were quite stressful pass, whilst other choppers might be because you suddenly realise that efficiency requires experience and is when neutrons impinge on it. The the buck stops here! But I do a bit of a ‘black art’. “You know set up to allow only every other light is then transmitted via enjoy it and I’ve taken a deep how the machine should run and I pulse through. thousands of optical fibres encoded interest in ISIS.” might give it a ‘tweak’ from time in a position-sensitive way. to time depending on how it’s Tim Carter designs, develops and running.” he says. maintains the chopper drive-systems Brian Holland, who has been including new designs for TS-2. “ISIS working on detector designs at ISIS One of the team regularly tours the is leading the way in chopper for a decade, has been involved in site carrying out routine checks on development. We have upgrading the detectors. components such as the dramatically improved their “Scintillators are a bit of a moderators. “We are all electronics reliability – essential for achieving speciality here; they are massive engineers so if a piece of good experimental results,” and require very careful work but equipment goes off in the middle he comments. are great fun to build,” he enthuses. of the night, we will attempt a first fix before calling in a specialist”, Tim Carter adds Tom. Tim Carter did a degree at the University of Durham and then Neutrons for the chop went on to work on industrial robotics at Culham and Harwell. Once the neutron beams are He joined ISIS five years ago and has been developing a drive that generated, they must be in the right works with all in-house-designed energy range for a particular choppers. experiment. This is achieved by using rotating devices called choppers which block unwanted neutrons. Brian Holland

Brian Holland (left) has worked on the site for 33 years. After a Harwell apprenticeship, he worked as an engineer supporting an endurance motor-racing team. “Here at ISIS, it’s also a team effort, which I like,” he says.

20 21 e heart of the Th journey A journey through ISIS

Running People spotlight the experiment

On arriving, visitors must first The experiment Once samples, accelerator, instrument and sample register at the User Office. “The students who come are often The SANS experiment being carried environment are ready, the experiment can begin nervous and shy especially if they out by Peter Griffiths and Paola are from overseas. We always Occhipinti required two days, with Emma Roberts smile and try to make them feel each of the 40 samples taking about Emma Roberts has worked in the at home,” says Emma Roberts an hour to run on the LOQ ISIS User office for eight years of the User Office. instrument. An automated sample- looking after the needs of visiting changer allowed the researchers to researchers: “I make sure that they plan the programme and leave it know that they can come to us Safety first with any query, no matter how running for 12 hours. While the first unusual. For example, we had Understanding safety is an important set of samples was running, the next someone who developed really aspect of working at ISIS, so new day’s samples could be prepared. bad-toothache and we were able users have to go through safety- to direct him to a dentist.” training. This involves viewing an on- “I used the ISIS laboratory facilities line tutorial explaining, for example, quite a lot,” explains Paola. “It’s the interlock system of shutters that nice because you meet lots of protects users when accessing people and can exchange ideas.” experimental areas. They then take a test – a series of short multiple- Experiments are carried out over the choice questions – on the use of full 24 hours to make full use of ISIS. chemicals, alarm systems, radiation The ISIS support staff for the hazards. “They get three chances to instrument, sample environment, pass. We’ve never had anyone fail – accelerator and beam-line are although some have taken the always available at the end of a three attempts!,” says Emma. Each telephone. user is given a radiation monitoring badge and a swipe card for secure “It’s quite intensive and tiring; you access to the experiment hall. don’t even know whether it’s night or day,” Paola comments. “It’s a The instrument scientist will then very high pressure environment for Supriyo Ganguly and Dimitrios Bakauos (University of Manchester) meet the visiting team, and take a student,” agrees Peter.“ It’s a using ENGIN-X for examination of them to the experimental cabin. chapter of the PhD thesis so the residual stress around welds in an “If researchers are inexperienced, experiment has got to work.” aircraft wing spar specimen I usually sit down with them and discuss their samples. We try to give them the largest-diameter neutron beam we can for a sample to get the best statistics,” says Steve King. “Students usually come with their supervisors, but if not, we spend time running through the experimental set-up and explaining the control software.”

Instrument scientists provide all the scientific support that the visiting team needs in order to get the best from their experiment.

22 23 e heart of the Th journey A journey through ISIS

Running People spotlight the experiment

“The software also allows you to The experiment gives a two- Collecting the data Experiment control Philip Cornier (Mount Alison University, look at the data live as it is dimensional pattern of the scattered Canada) using muons on EMU to probe collected, so you can quickly check neutron intensity which can then be radiation chemistry in ionic liquids Once the experiment starts, data are Users need to be able to control Freddie Akeroyd collected using specialist hardware if the instrument is working manipulated in a number of ways. In their experiments easily, and this can and become available for the properly.” the case of Peter and Paola’s be done remotely using a computer Freddie Akeroyd joined the Facility researchers to examine. The arrival experiments, a plot is derived which interface. This is where Kathryn 15 years ago after completing a of each neutron at one of the In a typical SANS experiment, the reveals the required information Baker of the ISIS Computing Group PhD in theoretical chemistry. He thousands of detecting elements raw data can be reduced to about polymer conformation. steps in. She and her colleagues says this involved ‘scattering meaningful results immediately theory and a great deal of comprising the detector area must develop and monitor the software computing’, so providing an ideal be ‘time-stamped’. These events are using a ‘tried and tested’ computer “We obtain just enough for manipulating all aspects of the background for working on data counted and this raw data is program that has been developed information to make any necessary experiment, including temperature, acquisition and software transferred to the instrument’s over the years. Instrument scientists adjustments to the next set of and movement of the samples and development at ISIS. dedicated computer. such as Richard Heenan and Steve samples,” says Peter. When the final equipment. Users are presented with King are on hand to give advice. “If datasets are ready, they can be put a visual display generated with a Freddie Akeroyd is one of the necessary I’ll log on to the data at onto a CD or memory stick and graphical programming language computing group who maintain home in the evening and give the taken back to the user’s laboratory called LabVIEW. “It’s all ‘drag and these computers and provide users a phone call. Sometimes I’ll for further analysis. A copy of the drop’ with a mouse,” explains software to control the data capture. come back in and we will go data is also archived at ISIS. Kathryn. “Settings for a variety of through the data-reduction parameters, such as sample process,” says Richard. Sample safety temperature, can be specified in command files for overnight An important practicality of neutron running,” says Freddie. scattering is to check the sample for Kathryn Baker radioactivity once the experiment Kathryn Baker did a sandwich has finished. Neutrons can activate placement at ISIS while a student samples through nuclear reactions. If usually decay rapidly,” says at the University of Glamorgan the dose rate is above a predeter- Paul Wright who is the ISIS health studying computer systems mined level, a member of the ISIS engineering. She says she enjoyed physicist and radiation protection the academic atmosphere, where Toby Perring (ISIS) and Andrew Walters (UCL/ISIS) reviewing health physics section collects the officer. After a few days, the sample “science is more important than their MAPS data of high-energy spin excitations in iron sample for storage in shielded can normally be released for return money,” and after a few years of locations. “Activated samples to the user’s laboratory. working in commerce, was “more than happy” to came back when a job became available.

Paul Wright

Paul Wright (left), a nuclear physicist by training, advises the Rutherford Appleton Laboratory on all aspects of radiation hazard management including safety protocols for maintenance of the facility, shielding, samples, and handling of radioactive equipment, as well as protection of users and staff. “It is extremely important that regulations are followed and the protocols are fit for purpose to minimise risks to facility staff and visitors,” says Paul.

24 25 At journey’s end A journey through ISIS

After Results 100 Mucin 5 wt% pH 7.0 the experiment d-PEG in mucin 5 wt% pH 7.0 10 1 -

1 m c / ) Q

Once the experiment has been run, the task of ( I , y t i s

n 0.1 e

analysing and interpreting the data can begin t n I

0.01 To uncover how the polymers Peter and Paola are now preparing The Cardiff team has already put in interact with mucin, Peter and Paola their results for publication. a proposal for the next neutron “The results must look at their data in detail. As Experiments performed at ISIS result experiment. “The results always 0.001 with all other stages of an in around 500 publications each give you a new idea,” says Peter. always give you 0.01 0.1 experiment, their ISIS local contact year, as well as conference papers, “We want to look at interactions 100 can always be called upon to help posters and seminars. Users also with other uncharged polymers a new idea,” Mucin 5 wt% pH 7.0 with the analysis and interpretation. have to send in a report giving such as dextrin, and a negatively PAMAM G2 in mucin 5 wt% pH 7.0 experimental details and its outcome charged dendrimer, and also in says Peter 10

So what did the SANS experiments – the Facility Access Panels use the presence of agents that 1 - reveal? The PEG polymer does not these reports to assess previous chemically break down mucin, show any interaction with the mucin experiments when users apply for such as N-acetylcysteine.” 1 m c /

and diffuses through quite easily, further beam-time. ) Q ( I

while the smaller dendrimer, which , y t i

has a positive charge depending on s

n 0.1 e t

the pH, interacts electrostatically n I with the negatively-charge gel, so its movement is retarded. “The 0.01 scattering indicates that the mucin structure collapses in the presence of the polymer,” says Paola. 0.001 0.01 0.1 Wave vector, Q/Å

Small-angle neutron scattering from 5-per-cent-weight mucin solutions as a function of pH in the presence and absence of synthetic polymers, as models for polymer therapeutics

“The scattering indicates that the mucin structure collapses in the presence of the polymer,” says Paola

26 27 lping others to A journey through ISIS He travel

Training for ISIS users and staff

• One-year sandwich ISIS runs various courses and schemes to ensure student placement Students can apply for specific that users get the most from a facility supported one-year placements at ISIS as part of their university courses. by staff of the highest quality These offer an excellent opportunity to build skills and experience in areas such as software or detector Richard Heenan working on LOQ Learning how to use Employment development and to get a inside with students during an ISIS neutron training course neutron and muon view of what it is like to work in methods As part of the Rutherford Appleton a facility relying on cutting-edge Laboratory, ISIS participates in technology. several training schemes supported ISIS runs regular training courses for by the STFC. These offer a unique postgraduate and postdoctoral • Vacation placement opportunity to young people at all researchers from the UK and EU in Students can also apply to stages of education to build up both neutron scattering and muon work at the Laboratory during engineering, technical and techniques. The aim is to give them vacations for between 6 and computing skills to the highest level. the necessary grounding to carry out 12 weeks. experiments at ISIS successfully. • Graduate training scheme • Engineering Advanced Graduates with good degrees in The five-day courses include lectures Apprenticeship Scheme mechanical, electrical and on theory, safety and radiation School-leavers and others with electronic engineering are eligible protection, the ISIS accelerator and five grade-C GCSE passes for the Graduate Mechanical targets, the instruments and the including English, mathematics Engineer and Graduate Electrical techniques used, combined with and science, can apply for an and Electronics Engineer Training hands-on activities. The ISIS website apprenticeship in electrical, Schemes. These are four-year also has extensive information – electronic or mechanical PhD students from the programmes involving a mix of manuals, lectures and hand-outs – engineering, which provides an Max Planck Institute, Germany, formal and tailored training, which supplements the courses. ideal start to career in the during their visit to ISIS placements and project work. advanced technology sector. The apprenticeship, which lasts four years, is considered one of the best in the country. Once qualified, an apprentice may stay on at the Laboratory as a technician or may embark on a full or part-time university degree course.

• Ongoing Learning ISIS provides numerous opportunities for the research community to discuss results, learn about new techniques and shape future ISIS instrument developments. These include regular user meetings, science- School trips are an important way to based workshops and ISIS scientists encourage the next generation of conferences run by facility staff Sean Giblin and scientists. Here we see students from alongside community scientists. Iain McKenzie loading Blue Coat School in Reading touring a cryostat with the ISIS experimental hall students on the ISIS 28 muon training course 29 A journey through ISIS

ISIS Scientists

ISIS scientists provide a huge range of expertise in the application of Chemistry Magnetism and superconductivity neutron scattering and muon spectroscopy to condensed matter and molecular science. They can be contacted to discuss how these • Catalysis: Stewart Parker • Magnetic structure determination: Laurent Chapon; Aziz Daoud-Aladine techniques might be useful in research programmes, and to give advice • Radical chemistry applications of muon spectroscopy: Iain McKenzie • Lattice dynamics, phase changes: Chris Stock on facility capabilities and proposal writing. They are listed here by • Microemulsions and micelles: • The role of magnetism in high temperature science area, to give an indication of particular research interests. Richard Heenan; Sarah Rogers superconductivity: Toby Perring • Structure and dynamics of liquids and solutions, • Superconductor properties using neutrons and All ISIS scientists can be contacted by email using including complex liquids and confined fluids: muons: Adrian Hillier Alan Soper; Daniel Bowron; Silvia Imberti; [email protected] • Heavy Fermions and quantum phase transitions: Felix Fernandez-Alonso; Franz Demmel Devashibhai Adroja; Chris Stock • Structure refinement in liquids, complex fluids, • Molecular magnetism and superconductivity confined fluids, and disordered solids: Alan studied by muons: Francis Pratt; Peter Baker Soper; Daniel Bowron; Silvia Imberti; Rowan Hargreaves • Colossal magneto-resistance: Toby Perring • Hydrogen bonding: John Tomkinson • Nanoscale electronic phenomena (with both Materials • Structure of glassy materials and neutrons and X-rays): Christian Kinane; • Vibrational spectroscopy of small molecules and disordered crystals: Alex Hannon; Emma Barney Timothy Charlton; Sean Langridge • Hydrogen storage, hydride materials: oligomers: John Tomkinson; Stewart Parker Timmy Ramirez-Cuesta; Bill David; • Dynamics in disordered materials: • Frustrated magnetism: Laurent Chapon; • Environmental chemistry: Steve King Steve Bennington Steve Bennington; Jon Taylor Ross Stewart • Electrochemistry: Rob Dalgliesh • Proton mobility in fuel cell materials: • Powder diffraction and structure solution • Magnetic and electronic properties studied with Felix Fernandez-Alonso with X-rays and neutrons: Bill David • Fibres: Steve King muons and neutrons: Sean Giblin • Ionic conductors using muons: • Single crystal diffraction: Matthias Gutmann • Relaxation in localized and itinerant moment Soft matter, biology James Lord; Steve Cottrell • Negative thermal expansion: Matt Tucker systems: Mark Telling • Carbon for hydrogen storage and • Atomic momentum distributions, particularly • Polymers: Jeff Penfold; Steve King; • Magnetic and electronic properties studied with other applications: Steve Bennington applied to helium: Jerry Mayers; Mark Adams John Webster; Ann Terry neutrons and X-rays: Jon Taylor • Hydrogen behaviour in semiconductors • Surfactants: Jeff Penfold; Richard Heenan; Theory and techniques using muons: Philip King Geology, Engineering, Archaeometry John Webster; Stephen Holt; Ann Terry; Sarah Rogers • Nano-structured materials: • Mineral physics with relevance to terrestrial • Theory of neutron scattering, density functional Felix Fernandez-Alonso; Steve King; Sean Langridge and planetary geology: Kevin Knight • Complex biological systems: Cameron Neylon; theory: Nikitas Gidopoulos Stephen Holt; Arwel Hughes; Victoria Garcia-Sakai; • Superionics, piezoelectrics, ferroelectrics, • Theory of strongly correlated quantum matter: • Residual stresses, welding and structural Luke Clifton particularly order-disorder: integrity: Anna Paradowska Jorge Quintanilla Steve Hull; Dave Keen • Colloids, adsorption at interfaces, self-assembly, • Archaeometry: Winfried Kockelmann • Density functional theory: Keith Refson • Multiferroics: Laurent Chapon mesophase structures: Jeff Penfold; Stephen Holt; • Radiation effects in electronics: Chris Frost Ann Terry; Maximilian Skoda • Polarised gasses: Chris Frost; Ross Stewart • Dielectric ceramics: Richard Ibberson • Biopolymer fibres and polymer morphology: • Monte Carlo neutron transport calculations: • Structure of phase separated alloys and Ann Terry Stuart Ansell porous materials: Richard Heenan • Dynamics of biomolecules: Mark Telling

30 31

Further information

A journey through ISIS

A journey through ISIS was produced for the ISIS Facility, For more information contact: STFC Rutherford Appleton Laboratory, Harwell Science and Innovation Campus, Didcot, Oxfordshire, OX11 0QX, UK ISIS Pulsed Neutron and Muon Source Science and Technology Facilities Council ISIS Director: Andrew Taylor 01235 446681 Rutherford Appleton Laboratory ISIS User Office 01235 445592 Harwell Science and Innovation Campus ISIS Facility Web pages www.isis.stfc.ac.uk Didcot OX11 0QX UK Writer: Nina Hall Editor: Philip King ISIS User Office Designer: Ampersand Design Ltd, Ardington Telephone: +44 1235 445592 (01235 861444) Fax: +44 1235 445103 Printed by: ESP Colour Limited and STFC Photographic and Email: [email protected] Reprographic Services URL: www.isis.stfc.ac.uk

May 2009 © Science and Technology Facilities Council 2009

Enquiries about copyright, reproduction and requests for additional copies of this report should be addressed to: STFC Library and Information Services, Rutherford Appleton Laboratory, Harwell Science and Innovation Campus, Didcot, Oxfordshire, OX11 0QX email: [email protected]

Neither the Council nor the Laboratory accept any responsibility for loss or damage arising from the use of information contained in any of their reports or in any communication about their tests or investigations.

32 ISIS PULSED NEUTRON AND MUON SOURCE Science and Technology Facilities Council, Rutherford Appleton Laboratory, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0QX, UK T: +44 (0)1235 445592 F: +44 (0)1235 445103 E: [email protected] www.isis.stfc.ac.uk

Head office: Polaris House, North Star Avenue, Swindon SN2 1SZ, United Kingdom. Establishments at: Rutherford Appleton Laboratory, Oxfordshire; Daresbury Laboratory, Cheshire; UK Astronomy Centre, Edinburgh; Chilbolton Observatory, Hampshire; Isaac Newton Group, La Palma; Joint Astronomy Centre, Hawaii.