Reports on Industrial Group Meetings Nov 2000 - 2001

• Autumn Meeting Crystallography in IndustryRoche Discovery,Welwyn 2nd November 2000
• Industrial Group Award David DysonRoche Discovery,Welwyn 2nd November 2000

BCA IG Autumn Meeting

Crystallography in Industry

2^nd November 2000, Welwyn

Morning Session

Brett Cooper (Merck Sharp & Dohme) opened the meeting with a case study showing how powder diffraction, although not often the technique of choice, can be used as a quantitative tool for monitoring polymorphic conversion in both drug substance and product. He discussed the inherent problems of powder diffraction for this application, such as preferred orientation, and how this had been approached. He concluded with an insight into the thermodynamic relationship between the two forms, and evidence suggesting that the conversion arose from recrystallisation in the presence of water rather than a solid- state transition.

Progress in indexing powder diffraction patterns was presented by Robin Shirley (University of Surrey). This included an introduction to why indexing can be difficult and a comprehensive survey of the algorithms available and their relative strengths and weaknesses, and an update on the progress of Industrial CrysFire. He concluded with a demonstration of CrysFire.

Chris Frampton (Roche Pharmaceuticals) presented recent zopiclone results as an update to his presen tation at the Spring Meeting. This included elucidation of the crystal structure of the anhydrous monoclinic form from synchrotron powder data, enabling comparison with the previously obtained single crystal structures of the monoclinic dihydrate and orthorhombic anhydrate. Comparison of the two monoclinic forms clearly demonstrated the dramatic changes that can result from ingress of water into channels in the structure. The changes in inversion symmetry for the anhydrous forms suggest that there m ay be a racemic to enantiomeric transition.

The BCA representative to ICDD, David Taylor, described the role of the
ICDD and how its membership is made up. He then gave a report on recent
developments within ICDD. These included the move away from paper products
to a range of Relational Database CD-ROM's thus reducing costs, electronic
purchasing, workshops and conferences, and new licences.

Clare Anderton
GlaxoSmithKline

Af ternoon Session:

Following lunch, provided by Roche Discovery, the afternoon session opened with Dr Steve Norval who presented the Industrial Group Award to Dr David Dyson for his contribution to the field of X-ray diffraction. The Industrial Group Award Lecture which followed gave an fascinating insight into the life of a practitioner of X-ray diffraction over the years with an emphasis on the measurement of texture.

Steve Norval (ICI) then provided an u pdate on the progress towards the release of an EU Standard covering X-ray diffraction. A standard is required as there is currently no National or International point of reference to encourage good practice, and to act as a point of reference. The General Principles section will be the first part to be released; possibly this year. Its release will impact on all uses of X-ray equipment working in a regulated arena.

Judith Shackleton (Manchester Materials Science Centre) provided a report on the Structural Materials Workshop held earlier in the year. The workshop was seen as a big success in bringing together people who work in this field and covered the pros and cons of sample preparation techniques. Finishing, Judith made a request for ideas to be made for future meetings.

Dr Liz Town-Andrews (DARTS) reported on the workshop held in October to communicate their objectives to industry. Liz related that a lot had been done to make the facility much more accessible to industr y and that they now able to offer a service based on a charge per sample or problem. An example of this service is afforded by station 9.8, which deals with micro diffraction. They will now, on the basis of no success no charge, attempt to solve the crystal structure from very small crystals (>20m m in all dimensions); the cost of success £4000.

Paul Tattersall (NRPB) gave an update on the impact of IRR-99 which became effective from 13^th May 2 000.

The legislation covers employers intending to use electrical equipment to produce X-rays for industrial radiography, processing of products, research and finally exposure of persons for medical treatment accelerators (except electron microscopes).

The regulation covers Prior Authorisation, Notification of Work, Prior Risk Assessment, Restriction of Exposure, Engineering Controls, Dose Limitations and Contingency Plans.

Philip Lake
GlaxoSmithKlin e

Industrial Group Award

David Dyson (right) being presented with the award by Steve Norval

David Dyson was presented with an Industrial Group Award during the 2000 Autumn Meeting at Roche Discovery, Welwyn. David has been associated with BCA Industrial Group from its inception. He has contributed widely to group activities and served on the committee as an ordinary member, vice-chair and chair between 1989 and 1996.

David's involvement with crystalline materials and industry began when he joined G.E.C from university, characterising reactor graphite materials. That developed an interest in high temperature studies, crystallite size and strain using camera and diffractometer methods.

18 months later, David returned to his native Yorkshire to work with United Steel Companies, which later became British Steel. This brought together interests in electron and x-ray diffraction that David has pursued ever since. Early studies covered phase analysis in oxide systems that led to the identification of a number of new phases appearing in the powder diffraction file. In the 60s, he developed the diffractometer method for analysing dust on air filters and contributed to the MDHS standard used since for environmental monitoring.

David was one of the first people in industry to recognise the importance of computers in the XRD l aboratory for data collection and analysis. A large suite of programs followed covering a variety of aspects of his work. He developed means for the quantitative analysis of a number of products in the steel industry and contributed to development of profile fitting methods. He became very interested in the effects of solid solution and preferred orientation, both of which are common in the steel industry. David has also contributed to British Standards in Texture Analysis of steels. He was responsi ble for setting up the BS in the early 70s and developed the software. The use of ODF saw him talking to and advising suppliers on how to output the data.

There was a series of BS reports on electron diffraction that subsequently appeared as a book - still selling world wide (He says it needs updating and re-issuing!) This introduced him to single crystal work and geometry of diffraction with the stereographic projection became one of his most useful tools. Installation of a 1000KV HVEM at Rotherham enabled him to study phase transformations and orientation changes in situ during straining and at high temperatures via diffraction studies.

An area of David's activity that has become very familiar in recent years is his strong interest in quality assurance, especially in relation to NAMAS / UKAS. Several of us have benefited from his regular and thorough assessment visits!

There are inevitably many important things missed here from David's many contributions to indust rial crystallography. He has published well over 100 papers and given many lectures both at home and abroad. But I hope it will be very clear that David is a very worthy a recipient of this award.

Dr Steve Norval