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Determination of zeolite-group mineral compositions by electron probe microanalysis

Published online by Cambridge University Press:  02 January 2018

L. S. Campbell ,
J. Charnock ,
A. Dyer ,
S. Hillier ,
S. Chenery ,
F. Stoppa ,
C. M. B. Henderson ,
R. Walcott  and
M. Rumsey
L. S. Campbell*
Affiliation:
School of Earth, Atmospheric and Environmental Sciences, University of Manchester, Williamson Building, Oxford Road, Manchester M13 9PL, UK
J. Charnock
Affiliation:
School of Earth, Atmospheric and Environmental Sciences, University of Manchester, Williamson Building, Oxford Road, Manchester M13 9PL, UK
A. Dyer
Affiliation:
Materials and Physics Research Centre, University of Salford M5 4WT, UK
S. Hillier
Affiliation:
James Hutton Institute, Craigiebuckler, Aberdeen AB15 8QH, UK Swedish University of Agricultural Sciences, SLU, Department of Soil & Environment, SE-75007 Uppsala, Sweden
S. Chenery
Affiliation:
British Geological Survey, Keyworth, Nottingham NG12 5GG, UK
F. Stoppa
Affiliation:
Department of Psychological, Humanistic and Territory Sciences of G.d’Annunzio University Chieti-Pescara, 66100 Chieti, Italy
C. M. B. Henderson
Affiliation:
School of Earth, Atmospheric and Environmental Sciences, University of Manchester, Williamson Building, Oxford Road, Manchester M13 9PL, UK
R. Walcott
Affiliation:
Department of Natural Sciences, National Museums Scotland, Chambers Street, Edinburgh EH1 1JF, UK
M. Rumsey
Affiliation:
Department of Mineralogy, The Natural History Museum, Cromwell Road, London SW7 5BD, UK
*
E-mail: [email protected]
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Abstract

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A new protocol for the quantitative determination of zeolite-group mineral compositions by electron probe microanalysis (wavelength-dispersive spectrometry) under ambient conditions, is presented. The method overcomes the most serious challenges for this mineral group, including new confidence in the fundamentally important Si-Al ratio. Development tests were undertaken on a set of natural zeolite candidate reference samples, representing the compositional extremes of Na, K, Cs, Mg, Ca, Sr and Ba zeolites, to demonstrate and assess the extent of beam interaction effects on each oxide component for each mineral. These tests highlight the variability and impact of component mobility due to beam interaction, and show that it can be minimized with recommended operating conditions of 15 kV, 2 nA, a defocused, 20 μm spot size, and element prioritizing with the spectrometer configuration. The protocol represents a pragmatic solution that works, but provides scope for additional optimization where required. Vital to the determination of high-quality results is the attention to careful preparations and the employment of strict criteria for data reduction and quality control, including the monitoring and removal of non-zeolitic contaminants from the data (mainly Fe and clay phases). Essential quality criteria include the zeolite-specific parameters of R value (Si/(Si + Al + Fe3+), the 'E%' charge-balance calculation, and the weight percent of non-hydrous total oxides. When these criteria are applied in conjunction with the recommended analytical operating conditions, excellent inter-batch reproducibility is demonstrated. Application of the method to zeolites with complex solid-solution compositions is effective, enabling more precise geochemical discrimination for occurrence-composition studies. Phase validation for the reference set was conducted satisfactorily with the use of X-ray diffraction and laser-ablation inductively-coupled plasma mass spectroscopy.

Keywords

natural zeoliteelectron microprobeanalytical protocolmineral compositionssolid solution
Type
Research Article
Information
Mineralogical Magazine , Volume 80 , Issue 5 , August 2016 , pp. 781 - 807
Creative Commons
Creative Common License - CCCreative Common License - BY
Copyright © The Mineralogical Society of Great Britain and Ireland 2016 This is an Open Access article, distributed under the terms of the Creative Commons Attribution license. (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted re-use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2016

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