September 2004 Newsletter.

Contents

Download a PRINTER FRIENDLY 190Kb PDF version of the paper edition.

1. Editorial
2. Low Angle Instrument Calibration Round Robin Launched
3. Check your Instrument Calibration with an automated spreadsheet
4. Pharmaceutical SIG 5th October 2004, AstraZeneca, Alderley Park - Programme
5. Autumn Meeting, DIY Crystallography, 4th November 2004, Birkbeck College, London - Call for papers
6. XRF content at 2005 Spring Meeting Spread the News!
7. 2005 Spring Meeting First announcement
8. PANalytical User Symposium - 28th/29th April 04 Report
9. 2004 Spring Meeting Reports
10. Newsletter and E-mail notice mailing lists
11. Nominations required for Industrial Group Award.
12. Committee Members and Addresses (2004-5)

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Forthcoming Events

Pharmaceutical Special Interest Group
4th October 2004, AstraZeneca, Alderley Park.

INDUSTRIAL GROUP AUTUMN MEETING 'DIY Crystallography'
Birkbeck College, London 4th November, 2004

BCA SPRING MEETING, Loughborough. 12th - 14th April 2005

Editorial

Welcome to this latest issue of the IG newsletter. In this issue we have our usual reports, including the excellent Spring Meeting, along with details of some exciting forthcoming events. Please do try and come along and support these. The Industrial Group Committee would welcome your comments and ideas for future meetings. The Industrial Group is organising a 'DIY Crystallography' meeting this autumn and need some contributions urgently. I'm sure that many of you have come up with novel solutions to problems with sample preparation, sample holders and even data analysis. Why not share it with others. As part of this meeting there will also be a session on Public Domain Software. If you know where to look, there is a lot of excellent software available, which can meet all your requirements. So please come along in November and find out more. Another worthwhile exercise is the low angle round robin and the instrument calibration test, details of which are in this newsletter. Both of these exercises will help provide you with information about the alignment of your x-ray diffractometer. Finally a big thank-you for all the contributions and as always, I would ask that you write a report for the newsletter if you attend any x-ray related meeting.

Articles Wanted:
Why not put pen to paper and write a short article for our next Newsletter. There are lots of examples to give you some ideas in our Hints & Tips section on the WEB. Don't forget, if you attend a conference, please send in an article about it.
We are also looking to expand the range of Industrial Applications of XRD on our WEB Site. All we need are a few well-chosen pictures and a few words. How about something on CEMENTS, MINERALS, MUSEUMS, PHOTOGRAPHY, DETERGENTS, PIGMENTS, POLYMERS

Philip Holdway
Editor

Newsletter Mailing list.

To keep cost down and to ensure that the newsletter gets to the appropriate people it is essential that we know your correct address. Also if there is a more appropriate contact in your organisation or if you no longer require a copy please let us know by contacting any of the committee officers. If you would like an e-mail notification of the WEB posting rather than a paper copy, then send an e-mail to [email protected] - with the title SUBSCRIBE WEB NEWS

E-mail Mailing list.

The IG sends about six E-mail notices each year to anyone who expresses an interest. These inform of Newsletter postings and the various meetings we organise each year. You can now register for our mailing list online and we always offer an opportunity to be removed from the list with each posting we make. REGISTER NOW!! - follow the link from the IG home page

PANalytical User Symposium - 28th/29th April 04

Note an expanded version of this report is available in PDF format: FULL REPORT

The meeting was held at Dunchurch Park, Nr. Rugby - a former manor set in 30 acres of picturesque woodland and grassed areas. The symposium combined a series of technical presentations on the X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) techniques with the UK launch of the Axios XRF Spectrometer.

Robin Aird (PANalytical Ltd) described the new X'Pert Highscore Plus XRD software available from PANalytical. Robin said the software is a complete powder pattern analysis tool, covering phase identification, cystallographic analysis and Rietveld calculations. All of the common and many of the less common data formats can be imported into the software and it supports the internationally recognised CIF format for the publication of XRD data. The Reporting interface has MS Word compatibility.

Leain Grimsley (British Geological Survey), spoke about her work in the sampling and analysis of soil in the Tavistock district of Devon. The PANalytical MiniPal 2 energy dispersive (ED) XRF instrument was used to measure As and Zn in soil. The MiniPal showed good accuracy at the 0.1% level. Portable XRF's can analyse up to 40 samples per day

Chris Staddon(Nottingham University) described his work on 'Spintronic' materials which consist of alternating layers of low temperature and high temperature GaAs and GaMnAs. A Materials Research Diffractometer (MRD) is used to obtain reciprocal space maps and to obtain strain measurements. Chris said that strain has been seen to relax as the coating thickness goes above a critical limit. Annealing the coatings produces changes in the XRD pattern which provides insights into diffusion mechanisms.

Rob Foster (Exposure control section, H&S Laboratories) described the XRF metal rubbing technique in which diamond coated 'lapping' paper is used to obtain specimens from metal surfaces. The technique is non-destructive, can be used on any size of item and does not require the metal item to be taken to the lab. Rob said that 0.003mg of Cr, Ni, Mn and Fe could be determined within 1% of certified values.

Richard Morris (Huntsman Surface Sciences) talked about a sugar based structured surfactant system is a novel aqueous delivery system that comprises surfactant, carbohydrate and water. Sugar induced 'Lamellar' sheets are formed with a spacing in excess of 500 angstroms. Richard explained how SAXS is used to measure the bi-layer spacing, to 'tune' formulations and to determine thermal stability. These systems suspend solid particles and and allow the system to flow as a normal liquid.

Cyril Marchant(PANalytical Ltd) explained that instrument breakdowns and performance problems fall mainly into three catogories: vacuum, water and software, with the majority of situations relating to the first two. He gave a number of basic 'ground rules' to reduce running costs. Ensure that the gas bottles (e.g. He and Ar) don't run completely empty before they are replaced. Check gas bottles for leaks at regulators and unions (use soapy water and watch for bubbles). Ramp up the kV and mA when the tube is cold and don't switch it off from high power (ramp it down slowly). Use sleep and dose channels when the instrument is not being used and tube 'breeding' to run up slowly. The water supply needs to be set-up correctly and maintained. Periodically top-up a circulating water system and check external water filters. Solid samples should be clean and dry.

Martijn Fransen (PANalytical Ltd) spoke about non-ambient measurements using the X'Pert Pro instrument. Martijn addressed some issues concerning non-ambient chambers. Sample height should be measured before heating and corrected 'on the fly' or afterwards. Parallel beam optics are better than focussing optics since sample height can move over a mm without a change of d-spacing. A d-spacing can be measured as a function of temperature and compared with literature values or a temperature calibration point defined where a known phase transition takes place.

Philip Russell(PANalytical Ltd) discussed detection limits of difference XRF instruments. WDXRF instruments (broadband excitation and selective detection) provide the best detection limits, generally for light elements especially those lighter than zinc. Detection limits for 'sequential systems' (those that scan elements one at a time) are a function of the total number of elements detected. EDXRF instruments (selective excitation and broadband detection) have best limit of detection for elements with atomic number >40 (Nb and higher). Practical limit is a function of the complexity of the system - e.g. presence/absence of major elements in the vicinity of the elements of interest.

Mark Russell(Queens University) described his work on Portland cements. He uses an Anton Paar Humidity chamber to control the temperature and moisture environment of his cement samples. The hydration characteristics of new and blended cements are determined which are then used to predict reactions and design new mixes.

Heather Harrison(British Geological Survey) described the use of the Epsilon 5 polarised EDXRF for the measurement of soil samples in the Merseyside and North Wales areas. The high excitation voltage gives good results for high Z elements. 300 samples per week are measured and have produced a geographical map containing 35,000 samples!

Reg Nichols(PANalytical Ltd) announced the UK launch of the Axios-Advanced spectrometer, an instrument equipped for 'ultimate precision and demanding light element applications'. He said it delivers unmatched performance incorporating numerous cutting-edge technologies such as the SST-Max tube. Phil Russell (PANalytical Ltd) gave Users more detail about the instrument. It contains a Rh-anode SST-Max tube which provides tube stability all the way up to 160mA improving analytical performance in the light element range. There is an integrated sample changer and a choice of loading mechanics which can be used to analyse up to 168 samples at a time. It can measure and analyse a variety of samples including solid pieces, pressed and loose powders, fused beads, liquids, foils, granules and thin films. There is also He flushing and a dust collection device. The software includes SuperQ 4, IQ+, Pro-trace, EP-multi, EDS and SPC. Phil said that with a minimum of training, most day-to-day operation is a push-button exercise.

Mark Farnworth
Pilkington European Technical Centre