The reestablishment of the "OXI" XRF standard analysis method at Sheffield Hallam University.

A.M.T.Bell, Materials and Engineering Research Institute, Sheffield Hallam University, Sheffield, S1 1WB.

Abstract:

The "OXI" XRF analysis method of Giles, Hurley and Webster [1] uses calibration standards to determine proportions of elements (present as oxides) in XRF fused bead samples.

We recently re-established this method at Sheffield Hallam University using standard samples made using a Claisse LeNeo fused bead maker. This presentation describes how the standards were made and "OXI" was reinstalled on our PANalytical MagiX PRO XRF spectrometer. Giles, Hurley and Webster describe how this method was set up for 20 elements; we have extended this to include more elements and even more elements may be included in the future.

[1] H.L. Giles, P.W. Hurley and H.W.M. Webster, X-ray Spectrometry, 24, 205-218 (1995).

Applications of Mapping by WD-XRF

Malcolm Haigh, Scimed.

Abstract:

Mapping of elemental concentrations in materials is a new development for WDXRF spectrometers. This novel approach opens up new avenues for investigators and researchers alike.

Generally, XRF mapping is available in two forms; EDXRF and WDXRF. This presentation gives insight into the WDXRF version to show the enhanced capability of using XRF mapping and focuses on what WDXRF can achieve and where this would differ from ED-XRF.

Data will be shown for general mapping and using light elements analysis mapping (LEAM). The capability of WDXRF in measuring coatings and multilayers and how performance for Oxygen and Nitrogen analysis on a WDXRF instrument can open up a new approach for detailed surface mapping of materials where existing techniques are not suitable.

XRF Determination of Silver in Photographic Emulsion

Dr David Beveridge, HARMAN technology Limited

Abstract:

Photographic emulsion is a dispersion of silver halide particles in aqueous gelatin: the particle size is typically 0.1 – 1 µm. The standard method for the determination of silver in such samples has long been the thioacetamide titration described by Bush et al. in 1959. This generally works well, but uses a rather toxic reagent and tends to give problems with samples of high iodide content, because the titration curve shape changes and the endpoint is significantly shifted. An XRF method, analysing samples in the liquid phase, was therefore devised; this has been used extensively and has been found satisfactory. This method was designed to be immune from some of the potential radiolytic problems of liquid samples.

How to make sure your XRF delivers reliable results from day one until the end of its life?

Dr. Rainer Schramm, FLUXANA GmbH & Co. KG, Borschelstr.3, 47551 Bedburg-Hau, Germany

Tel. +49 2821 48011-10, Fax +49 2821 48011-99, www.fluxana.com, info@fluxana.com

Abstract:

FLUXANA is operating an xrf laboratory which works under ISO 17025 accreditation. The main focus of the lab work is traceability of the xrf results. Therefore it is very important within any method development that variability caused by the actual spectrometer becomes negligible. Based on this experience FLUXANA will present its findings in terms of the essential approach required to ensure that xrf methods optimized in a way that precision, reproducibility and long term stability are set up from first used and maintained throughout the life of the XRF spectrometer. The importance of sample preparation will be presented and illustrated with a specific focus on fused bead technology and the impact on high precision applications. Finally the benefit of automation in the sample preparation is shown as one important parameter for precision and long term stability.

The Analysis of Suspended Particulate Matter using ED-XRF

Andy Scothern, Malvern Panalytical Ltd.

Abstract:

The presence of toxic pollutants in the air has been a subject of research for many years in both developed and developing nations. In the United States, air quality standards are governed by the ‘Clean Air Act’ and administered by the US Environmental protection Agency (EPA). One of the key areas of concern for the EPA is the Suspended Particulate Matter (SPM) of air. Research on the health effects of SPM in ambient air has focused increasingly on particles that can be inhaled into the respiratory system i.e. particles of aerodynamic diameter of <10um. These particles are referred to as PM10 (2.5 – 10um) and PM2.5 (<2.5um). As well as chemical toxicity, these particles are a significant threat to health.

The elemental analysis of the SPM on these air filters is traditionally performed by energy dispersive x-ray fluorescence spectrometry (EDXRF) using EPA method IO-3.3, which outlines the protocol of the analysis of 44 elements on air filters.

This presentation will outline the capability of bench top EDXRF spectrometers as an analytical tool for the analysis of air filters according to the US EPA and make links to standards and issues affecting air quality in the UK.

Biasing pitfalls in sample preparation for XRF analysis,

Martin Lischka, HERZOG Maschinenfabrik GmbH.

Abstract:

In this talk we share some experience when designing automated laboratories and sample preparation equipment. Those highlight the urgent need to understand the whole pathway from primary sample to aliquot for a low Total Sampling Error (TSE) and Sample Preparation Error (SPE). Analytical characterization often involves multiple material handling procedures, when applying the four sampling unit operations (SUO), namely composite sampling, particle size reduction, blending and representative mass reduction. Segregation and material loss of certain size fractions can impact accuracy and precision of the XRF results significantly.

How to accomplish optimally todays analytical tasks with latest XRF! A guideline how to evaluate current XRF technologies!

Dr. Kai Behrens, Frank Portala, Dr. Adrian Fiege, Dr. Jan Stelling , Bruker AXS GmbH, Oestliche Rheinbrueckenstr. 49, D- 76187 Karlsruhe

Abstract:

Despite the fact that XRF is a mature analytical method there were still recent technological developments in the past ten years for both, energy- and wavelength dispersive XRF. Especially new detectors and new analyzer crystals paired with a more efficient excitation beam path has led to significant analytical performance for almost all classes.

Especially with the latest generation of Si-Drift detectors energy-dispersive XRF instruments are competing in many applications with wavelength dispersive XRF. Closing the gap in count rate capability, resolution and overall analytical precision it is time to evaluate and rate these new components to revise traditional decisions which XRF instruments to select. While the group of elements, concentration ranges and required analytical precision remains almost the same, the presence of a single additional element will put a different technology or component in favor.

Latest XRF technologies will be presented and their characteristics will be discussed based on typical industrial applications for quality control. Examples will be given on raw materials, intermediates and final products from minerals, metals and petrochemistry.

USP<232> AND ICH Q3D ELEMENTAL IMPURITY STANDARDS FOR X-RAY FLUORESCENCE ANALYSIS.

Y. Xiao , M. Zoontjes, T. Soteriou, L. Kempenaers , Malvern Panalytical B.V. Lelyweg 1 (7602 EA), PO Box 13, 7600 AA Almelo, the Netherlands, L. Grimsley , M. Ingham, Malvern Panalytical Nottingham, Tollerton hall, Nottingham, NG12 4GQ, UK

After the recent publication (USP 37-NF 32) of USP chapter <735> X-ray fluorescence (XRF) spectrometry there has been increased interest in this technique in the pharmaceutical industry [1].

One of the key applications of interest is using XRF to determine elemental impurities according to USP<232> and ICH Q3D [2]. Due to this interest and current lack of XRF calibration standards for these elements in the ranges required, it was decided to investigate the possibilities of producing calibration standards for this analysis.

Automated Sample Preparation in the Analytical Laboratory - the TOS Advantage

M. Lischka, J Herzog, K.H. Esbensen

Automated Sample Preparation in the Analytical Laboratory - the TOS Advantage.