This workshop will be held in the Geology Department Sylvester Bradley Room. (Bennett Building Room G86). The represented companies will each have 5 minutes to describe their company and its products. This will be followed by 5 minutes each to cover selected topics as outlined in the following table. There will be time for questions and to visit companies stands during the exhibition breaks.
Order Manufacturer/supplier Presenter Topic
1 Bruker Colin Slater Calibration basics
2 Niton Chris Calam Quality control
3 Olympus (Delta) James Parker Drift Correction
4 Spectro Steve Allott Safety
5 Oxford Instruments Richard Kilworth Sample/specimen requirements
Kev Solman, Andrew Turner, Sean Comber, Aldous Rees, Dimitrios Gkiokas. Plymouth University
The high concentrations of some metals in boat paints can present an environmental risk and health hazard. The need for a rapid and accurate chemical characterisation of flaking and discarded paint fragments has been recognised in recent years. To date, determination of metals has mainly been undertaken following acid digestion, using analytical techniques such as inductively coupled plasma-mass spectrometry, but this approach has its own problems, and is often incomplete because of the poor solubility of some paint matrices under acidic conditions.
Field portable X-ray fluorescence is a non-destructive, rapid, multi-element technique whose application to boat paints has so far been extremely limited. A range of boat paints, collected from abandoned boats, slipways, harbours and yards from across the EU were analysed and the results compared to those obtained using traditional aqua-regia digestion and ICP-MS.
Despite several problems still to overcome with this technique FP-XRF is proving to be a very useful reconnaissance tool in analysing old boat paint fragments.
Ros Schwarz, Consultant.
Sixteen laboratories analysed an unknown sample (DOT-1) by their routine methods. The sample was composed of a blend of material from a genuine brown field site with low levels of silver, material from a mining area in South-West England and two spikes of lanthanide elements. The sample preparation methods used will be discussed and the results obtained summarised, with some examples. Participants in the exercise will be invited to comment.
David Beveridge, HARMAN Technology Ltd.
Following on from the success of the geological sample DOT-1 last year, we have decided to offer a second sample which is completely different in character to DOT-1. DOT-2 is an organic compound which contains three major elements that are easily detectable by XRF. The proportion of these elements is critical to the performance of the substance, and their determination by traditional methods is not easy. We hope that you will find an easy and successful XRF approach to this analysis.
For a little bit of fun, we decided to offer a small prize for the person who can tell us of the most unusual or eccentric sample(s) they have ever analysed by XRF. This could be something which has to be prepared for analysis in an unusual (for XRF) way, a sample which is of inherent interest, or something which was just plain odd. It could be anything - the odder or the more interesting the better! Obviously this will depend to a large extent on the technique used - hand-held instruments make it very easy to analyse samples which would be extremely awkward using a benchtop machine.
How to Enter: All delegates will be sent an Entry Invitation by E-mail a few weeks before the meeting. To enter the competition, simply reply to this E-mail giving a title and sentence to explain the content of the entry. Competition entries will not be accepted after 09:00 9th June. NOW EXTENDED to 9am on Wednesday 11th June.
All delegates registered in time will get a vote: A list of entry titles and descriptions will be E-mailed to all delegates who will then get one vote for their favourite entry. Voting will close at 09:00 13th of June and the winner will be informed as soon as the votes are counted. This will allow the winner time to prepare a short presentation to give at the meeting.
The competition winner will be announced and their prize presented at the meeting.
This workshop will be held in the Geology Department Sylvester Bradley Room. (Bennett Building Room G86). The represented companies will each have 5 minutes to describe their company and its products. This will be followed by 5 minutes each to cover selected topics as outlined in the following table. There will be time for questions and to visit companies stands during the exhibition breaks.
Order Manufacturer/supplier Presenter Topic
1 Spectro Steve Allott Detection limits
2 PANalytical Steve Davies Light elements
3 Rigaku Garry Smith Calibration basics
4 Bruker Colin Slater Quality control/drift correction
5 Olympus James Parker Sample/specimen requirements
Garry Smith, XRF Applications Specialist, Scimed XRF, a division of Scientific and Medical Products Ltd
The accurate analysis of individual components in materials where the sample matrix is variable or not completely characterised can present problems for the analyst. Matrix correction by the application of theoretical alpha corrections or fundamental parameters may not always be suitable (or even possible) in such cases.
Given the correct circumstances of sample type and preparation method, the introduction of an internal standard into the sample provides an alternative approach which can yield extremely reliable results
.
Here we will discuss the general requirements for selection of a suitable internal standard: where their use is and is not applicable, criteria for selection, sources of error, and practical examples.
Calibration strategies for XRF applications using sample preparation by borate fusion – Practical example for chlorine analysis in the cement industry.
Mathieu Bouchard, Alex Milliard and Sébastien Rivard, Corporation Scientifique Claisse®, Québec, Canada
For more than half a century, sample preparation by borate fusion combined with XRF analysis has been used for the analysis of different industrial materials. As a first step, this paper discusses the difficulties that spectroscopists encounter when developing an XRF calibration.
Then, different calibration strategies will be suggested according to the possibilities that the borate fusion allows for: no particle size effects, no mineralogical effects, lower inter-elemental interactions / need to apply mathematical corrections and the possibility to create synthetic standards made of pure chemicals and/or pure oxides as a complement to the use of Certified Reference Materials (CRM).
Finally a specific example of the development of a calibration for chlorine in cement materials will be discussed. Building a chlorine calibration curve is a challenge as very few Certified Reference Materials (CRMs) are available with good certified values and interesting concentration of chlorine.
Andrew Scothern, Saint Gobain.
Occasionally the samples we are asked to analyse are simply too small for our conventional Wavelength and Energy Dispersive Systems. By using an EDX system attached to our Scanning Electron Microscope we are able to prepare tiny samples, or target small spot sizes of larger samples, for analysis. The talk will cover the set-up of the instrument, sample preparation, pros and cons of this approach and review some real problems that XRF data generated this way has helped to solve.