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Minerals
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X-ray Fluorescence Spectrometry in Mineral and Glass Analysis
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X-ray Fluorescence Spectrometry in Mineral and Glass Analysis

A special issue of Minerals (ISSN 2075-163X). This special issue belongs to the section "Crystallography and Physical Chemistry of Minerals & Nanominerals".

Deadline for manuscript submissions: closed (10 November 2020) | Viewed by 16752

Special Issue Editor

Dr. Anthony Bell

E-Mail Website
Guest Editor
Materials and Engineering Research Institute, Sheffield Hallam University, Sheffield S8 7DN, UK
Interests: minerals; glasses; nuclear waste glass materials; X-Ray Fluorescence; X-Ray powder diffraction; synchrotron radiation; rietveld method; leucite mineral crystal structures

Special Issue Information

Dear Colleagues,

X-ray Fluorescence (XRF) is an extremely useful analytical technique that can be used for chemical element analyses on materials such as minerals and glass samples. For high Z elements, the limit of detection of the XRF technique can approach parts per million under ideal conditions. This technique is particularly suited for the characterisation of glass samples, such as glasses used as potential hosts for nuclear waste storage. In these materials, all of the elements of interest should be completely dissolved in the glass matrix. Therefore, there should be no crystalline component, making characterisation by diffraction techniques unsuitable.

This Special Issue aims to publish papers with appropriate examples that confirm the important role of the XRF technique in the characterisation of mineral and glass samples. Papers showing how the XRF technique can be developed to give improved analytical results are also welcome.

Dr. Anthony Bell
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Minerals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • X-Ray Fluorescence
  • minerals
  • glass samples
  • nuclear waste materials
  • technique development

Published Papers (3 papers)

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Research

25 pages, 6161 KiB  
Article
Possible Pitfalls in the Analysis of Minerals and Loose Materials by Portable XRF, and How to Overcome Them
by Valérie Laperche and Bruno Lemière
Minerals 2021, 11(1), 33; https://doi.org/10.3390/min11010033 - 29 Dec 2020
Cited by 20 | Viewed by 7678
Abstract
Portable X-ray fluorescence spectroscopy is now widely used in almost any field of geoscience. Handheld XRF analysers are easy to use, and results are available in almost real time anywhere. However, the results do not always match laboratory analyses, and this may deter [...] Read more.
Portable X-ray fluorescence spectroscopy is now widely used in almost any field of geoscience. Handheld XRF analysers are easy to use, and results are available in almost real time anywhere. However, the results do not always match laboratory analyses, and this may deter users. Rather than analytical issues, the bias often results from sample preparation differences. Instrument setup and analysis conditions need to be fully understood to avoid reporting erroneous results. The technique’s limitations must be kept in mind. We describe a number of issues and potential pitfalls observed from our experience and described in the literature. This includes the analytical mode and parameters; protective films; sample geometry and density, especially for light elements; analytical interferences between elements; physical effects of the matrix and sample condition, and more. Nevertheless, portable X-ray fluorescence spectroscopy (pXRF) results gathered with sufficient care by experienced users are both precise and reliable, if not fully accurate, and they can constitute robust data sets. Rather than being a substitute for laboratory analyses, pXRF measurements are a valuable complement to those. pXRF improves the quality and relevance of laboratory data sets. Full article
(This article belongs to the Special Issue X-ray Fluorescence Spectrometry in Mineral and Glass Analysis)
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21 pages, 11531 KiB  
Article
Identification of Economic Activity in a Bronze Age Settlement in Central Russia Based on the Results of XRF Analysis of Samples of the Cultural Layer
by Konstantin Voronin
Minerals 2020, 10(7), 607; https://doi.org/10.3390/min10070607 - 06 Jul 2020
Cited by 1 | Viewed by 2442
Abstract
In central Russia, the examination of characteristics of economic activity of Bronze Age settlements and the determination of functional zones that existed in their territories in the first half of the second millennium BC based on the results of XRF (X-ray Fluorescence) analysis [...] Read more.
In central Russia, the examination of characteristics of economic activity of Bronze Age settlements and the determination of functional zones that existed in their territories in the first half of the second millennium BC based on the results of XRF (X-ray Fluorescence) analysis of samples of the cultural layer have never been done before. The data from elemental analysis of the samples of the cultural layer of the Bronze Age settlement Pesochnoe 1 from an excavation area of 126 m2 obtained via the XRF method showed significant content of copper (Cu), zinc (Zn), calcium (Ca) and phosphorus (P), several times exceeding the content of the same chemical elements in the surrounding soils. The discovered Cu can be associated with metalworking, Zn are likely from ash and the biomass of the aquatic environment, and Ca and P can be found in bone remnants. Analysis of the spatial distribution of archaeological objects with quantitative indicators of Cu, Zn, Ca, P made it possible to distinguish two functional areas in the excavation of the Bronze Age settlement. A very high concentration of Cu, Zn, Ca, P recorded in the first functional zone, in the center of which was a hearth, indicates diverse activity that took place in this territory, including the use of different organic materials (plants, bones) as fuel and melting of metal. The second functional area with high concentrations of Zn, Ca and especially P suggests it was a place where biomaterials of animal origin might have been used. Full article
(This article belongs to the Special Issue X-ray Fluorescence Spectrometry in Mineral and Glass Analysis)
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17 pages, 1686 KiB  
Article
X-ray Fluorescence Analysis of Feldspars and Silicate Glass: Effects of Melting Time on Fused Bead Consistency and Volatilisation
by Anthony M. T. Bell, Daniel J. Backhouse, Wei Deng, James D. Eales, Erhan Kilinc, Katrina Love, Prince Rautiyal, Jessica C. Rigby, Alex H. Stone, Shuchi Vaishnav, Gloria Wie-Addo and Paul A. Bingham
Minerals 2020, 10(5), 442; https://doi.org/10.3390/min10050442 - 15 May 2020
Cited by 11 | Viewed by 4981
Abstract
Reproducible preparation of lithium tetraborate fused beads for XRF analysis of glass and mineral samples is of paramount importance for analytical repeatability. However, as with all glass melting processes, losses due to volatilisation must be taken into account and their effects are not [...] Read more.
Reproducible preparation of lithium tetraborate fused beads for XRF analysis of glass and mineral samples is of paramount importance for analytical repeatability. However, as with all glass melting processes, losses due to volatilisation must be taken into account and their effects are not negligible. Here the effects of fused bead melting time have been studied for four Certified Reference Materials (CRM’s: three feldspars, one silicate glass), in terms of their effects on analytical variability and volatilisation losses arising from fused bead preparation. At melting temperatures of 1065 °C, and for feldspar samples, fused bead melting times shorter than approximately 25 min generally gave rise to a greater deviation of the XRF-analysed composition from the certified composition. This variation might be due to incomplete fusion and/or fused bead inhomogeneity but further research is needed. In contrast, the shortest fused bead melting time for the silicate glass CRM gave an XRF-analysed composition closer to the certified values than longer melting times. This may suggest a faster rate of glass-in-glass dissolution and homogenization during fused bead preparation. For all samples, longer melting times gave rise to greater volatilisation losses (including sulphates and halides) during fusion. This was demonstrated by a linear relationship between SO3 mass loss and time1/2, as predicted by a simple diffusion-based model. Iodine volatilisation displays a more complex relationship, suggestive of diffusion plus additional mechanisms. This conclusion may have implications for vitrification of iodine-bearing radioactive wastes. Our research demonstrates that the nature of the sample material impacts on the most appropriate fusion times. For feldspars no less than ~25 min and no more than ~60 min of fusion at 1065 °C, using Li2B4O7 as the fusion medium and in the context of feldspar samples and the automatic fusion equipment used here, strikes an acceptable (albeit non-ideal) balance between the competing factors of fused bead quality, analytical consistency and mitigating volatilisation losses. Conversely, for the silicate glass sample, shorter fusion times of less than ~30 min under the same conditions provided more accurate analyses whilst limiting volatile losses. Full article
(This article belongs to the Special Issue X-ray Fluorescence Spectrometry in Mineral and Glass Analysis)
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