Rainer Schramm, FLUXANA® GmbH & Co. KG, Borschelstr. 3, D-47551 Bedburg-Hau, Germany
Part 1 : liquid sample preparation: cups, films, etc.
For XRF liquid samples are prepared in a sample cup which is covered with a film window. We will present different preparation methods including a variety of cups and films. Special applications like multiphased liquids will be presented as well.
Part 2: solid sample preparation: pressed pellets
The easiest way to prepare solid samples is to make a pressed pellet. However different tools and accessories will influence the analytical result. A variety of binders, aluminium cups, useful pressures, mixing procedures and preparation methods are presented.
Part 3: solid sample preparation: fused beads
Fusion as preparation method will give the highest precision. We will explain which parameters like fluxes, additives, fusion conditions, platinum ware, etc. are important.
Proper Sample Preparation is vital for obtaining accurate analytical results.
Frederic Davidts, Socachim. The aim of this workshop is to present innovative machines and creative techniques for specimen preparation.
In this session some of the instruments and accessories available will be presented.
Bench Top Ring Mill
Automatic Pellet Press with the new “Easy handle “ pellet die
Electrical and Gas fusion machines
Polishing system for platinum labware
During the session problems encountered by participants will be discussed.
Comparative Study between the Standard Method ISO 9516-1 for Analysis of Iron Ore and a Global Methodology Using Calibration Based on Certified Reference Materials.
Anne-Catherine Breton1, Mathieu Bouchard1, Charles-Olivier Arsenault1, Sébastien Rivard1, Sharon Ness2.
1.Corporation Scientifique Claisse®, Quebec City, Canada
2.Intertek Genalysis, Perth, Australia
Large mining companies are vulnerable to any bias in the total iron analysis process; their very survival may depend on the assays run on exploration samples, concentrate, internal standard and/or reference material, be they high-grade hematite, low-grade hematite or magnetite. The current ISO Method, still widely accepted, is “Iron ores -- Determination of Various Elements by X-ray Fluorescence Spectrometry -- Part 1: Comprehensive Procedure” (ISO 9516-1:2003). However, there are several proven limitations to the predominant version of this standard; it cannot cope with recent advances in fusion sample preparation and wavelength-dispersive XRF.
We consider the results of a survey on ISO 9516-1:2003, which tried to understand how our customers use this standard and how they cope with its limitations.
We present a ‘lite’ version of the standard method for iron ore analysis based on calibration standards prepared using pure chemicals. A very wide range of worldwide iron ore types can be prepared using the one fusion method.
We describe the use of certified reference materials for preparation of calibration curves using the previous fusion methodology and analytical line parameters.
We show how laboratory, spectrometry and quality control processes may be simpler, more specific, efficient and user-friendly. Furthermore, all collected data using these procedures will be compared to the analytical requirements of ISO 9516-1:2003. Deviations from the standard method parameters (calibration, standards, flux, fluxer, etc.) will also be pointed out and discussed.
Dr Colin Slater, XRF Applications Scientist, Bruker UK Limited
Mr Michael J Dobby, XRF Applications Scientist, Bruker UK Limited
The need to be able to run XRF measurements without a matrix matched calibration is becoming more apparent with researchers and analysts requiring a ‘what’s in my sample’ type approach to a measurement. Users might not have access to standards for that particular type of material or need to look at methods that screen for the entire periodic table (as far as is possible) when monitoring product quality and production methods.
Modern standardless analysis packages are capable of offering such a measurement, but the reliability of the data can vary depending on how much information you have given to the standardless analysis package beforehand, or during the post measurement processing.
This brief talk aims to go through the basics of how modern standardless analysis packages for both WD and ED XRF work and some of the common pit-falls and problems that arise as a result of a user not appreciating the requirements of the packages, and how data quality can be greatly improved with a few simple steps.
Nick Marsh, University of Leicester
XRF analysts are increasingly being asked to obtain chemical quantifications on smaller and smaller amounts of material (<<100mg). The newer generations of spectrometers have provided significant enhancements in performance especially for the lighter elements in the periodic table. Fluxes and other sample preparation reagents are now of reliable purity and high quality. So just how small a sample can we analyse and get usable quantitative data from? Do we need to re-visit the ways we evaluate our assessment of quantitative data at these low levels? In extreme circumstances what might ‘fitness for purpose’ be taken to mean. Perhaps it is a pertinent time to reflect and discuss some of these issues?
Steve Davies - PANalytical, Regional Specialist UK - XRF
At the Durham X-ray Conference of 1995, a callow youth gave a paper on a subject that had been concerning him since he started using WDXRF back in 1984 to analyse oils and fuels. Eighteen years later, he revisits the subject to see if anything has changed.
Garry Smith, XRF Applications Specialist, Scimed XRF, a division of Scientific and Medical Products Ltd
The “ideal” XRF sample is a true solution where analyte distribution is completely homogeneous. At first glance a sample of liquid waste, waste oil, or effluent might seem to fall into this category as a relatively straightforward analysis.
However, liquid waste samples present a number of challenges and pitfalls. For example:
Samples may be multi-phase, either liquid/solid (suspended sediments) or liquid/liquid (aqueous components in waste oil)
Analytes may be subject to high dilution factors with requirements for low LLD’s (effluent water) Industry, and in particular the waste industry, requires fast and relatively accurate analysis of these types of sample in the face of ever-tightening controls and legislation. This brief talk will discuss the potential effects these issues may have on the accuracy of XRF analysis, and some of the practical strategies the analyst can employ to minimise them.
Chris Calam, Thermo Scientific Portable Analytical Instruments
The use of portable x-ray fluorescence (P-XRF) in mining and mineral exploration projects has accelerated in the last decade. In the conventional application of P-XRF, samples are simply “shot” (scanned) with the instrument to produce results in seconds. However, due to sample heterogeneity the results are closer to semi-quantitative rather than quantitative, and light elements analysis (Mg-S) is almost impossible.
Demand in the field for quantitative P-XRF analysis, typically in remote locations with no power, led to the development of portable and battery powered sample preparation tools, namely:-
Direct Rock Sampler Kit
Electric Hammer Mill Kit
This talk compares and contrasts typical performance of direct rock analysis, finely ground powder and pressed pellets performed in the field with battery powered tools and reviews what new applications could be opened up.
The IG XRF subcommittee are offering, free of charge, aliquots of a sample for analysis by participants in the meeting. It is intended to assist in method development and training and not as a reference material or proficiency test. We are asking you to determine as many or as few elements as you like by any suitable XRF method, or by complementary techniques such as ICP, and to send them to us by 30th September 2013. We will compile the results and give you feedback highlighting (confidentially) any issues and potential solutions.
The sample is material from a “Brownfield“ site and contains elements at ppm levels in an aluminosilicate matrix, to help you develop the versatility of your instrumentation. If it is favourably received, we will make it the first of a series.