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The Use of Lithium Heteropolytungstate As an Alternative to Bromoform For The use of lithium heteropolytungstate as an alternative to bromoform for heavy media separations Mineralogy, Petrology and Biostratigraphy Facility Internal Report IR/11/049 BRITISH GEOLOGICAL SURVEY MINERALOGY, PETROLOGY & BIOSTRATIGRAPHY FACILITY INTERNAL REPORT IR/11/049 The use of lithium heteropolytungstate as an alternative to bromoform for heavy media separations The National Grid and other Ordnance Survey data are used with the permission of the Controller of Her Majesty’s I Mounteney Stationery Office. Licence No: 100017897/2010. Keywords bromoform, lithium heteropolytungstate, heavy media separation. Front cover Heavy media separation apparatus. Bibliographical reference MOUNTENEY, I 2011. The use of lithium heteropolytungstate as an alternative to bromoform for heavy media separations. British Geological Survey Internal Report, IR/11/049. 12pp. Copyright in materials derived from the British Geological Survey’s work is owned by the Natural Environment Research Council (NERC) and/or the authority that commissioned the work. You may not copy or adapt this publication without first obtaining permission. Contact the BGS Intellectual Property Rights Section, British Geological Survey, Keyworth, e-mail [email protected]. You may quote extracts of a reasonable length without prior permission, provided a full acknowledgement is given of the source of the extract. Maps and diagrams in this book use topography based on Ordnance Survey mapping. © NERC 2011. All rights reserved Keyworth, Nottingham British Geological Survey 2011 BRITISH GEOLOGICAL SURVEY The full range of Survey publications is available from the BGS British Geological Survey offices Sales Desks at Nottingham, Edinburgh and London; see contact details below or shop online at www.geologyshop.com Keyworth, Nottingham NG12 5GG The London Information Office also maintains a reference 0115-936 3241 Fax 0115-936 3488 collection of BGS publications including maps for consultation. e-mail: [email protected] The Survey publishes an annual catalogue of its maps and other www.bgs.ac.uk publications; this catalogue is available from any of the BGS Sales Shop online at: www.geologyshop.com Desks. Murchison House, West Mains Road, Edinburgh EH9 3LA The British Geological Survey carries out the geological survey of Great Britain and Northern Ireland (the latter as an agency 0131-667 1000 Fax 0131-668 2683 service for the government of Northern Ireland), and of the e-mail: [email protected] surrounding continental shelf, as well as its basic research projects. It also undertakes programmes of British technical aid in London Information Office at the Natural History Museum geology in developing countries as arranged by the Department (Earth Galleries), Exhibition Road, South Kensington, London for International Development and other agencies. SW7 2DE 020-7589 4090 Fax 020-7584 8270 The British Geological Survey is a component body of the Natural 020-7942 5344/45 email: [email protected] Environment Research Council. Forde House, Park Five Business Centre, Harrier Way, Sowton, Exeter, Devon EX2 7HU 01392-445271 Fax 01392-445371 Geological Survey of Northern Ireland, Colby House, Stranmillis Court, Belfast BT9 5BF 028-9038 8462 Fax 028-9038 8461 Maclean Building, Crowmarsh Gifford, Wallingford, Oxfordshire OX10 8BB 01491-838800 Fax 01491-692345 Columbus House, Greenmeadow Springs, Tongwynlais, Cardiff, CF15 7NE 029–2052 1962 Fax 029–2052 1963 Parent Body Natural Environment Research Council, Polaris House, North Star Avenue, Swindon, Wiltshire SN2 1EU 01793-411500 Fax 01793-411501 www.nerc.ac.uk IR/11/049; Version 3 Last modified: 2011/09/27 15:19 Foreword This report is the published product of a study by the British Geological Survey (BGS) and was produced under the Science Facilities’ Maintenance and Development of Capability (MaDCap) project. This report aims to provide a procedural guide for heavy media separations using non toxic lithium heteropolytungstate (LST) in place of the more toxic bromoform and methylene iodide previously used for this purpose. Acknowledgements I would like to thank to Gren Turner for his assistance with SEM imaging, Mark Ingham and his team for producing the XRFS data and Simon Kemp for helping to draft this report. i IR/11/049; Version 3 Last modified: 2011/09/27 15:19 Contents Foreword ......................................................................................................................................... i Acknowledgements ......................................................................................................................... i Contents .......................................................................................................................................... ii Summary ....................................................................................................................................... iv 1 Introduction ............................................................................................................................ 1 1.1 Halogenated organic solvents ......................................................................................... 1 1.2 Polytungstates ................................................................................................................. 2 2 Materials and Methodology .................................................................................................. 3 2.1 Sample preparation ......................................................................................................... 3 2.2 Heavy media separation .................................................................................................. 3 2.3 Recovery procedure ........................................................................................................ 4 3 Results ..................................................................................................................................... 5 4 Discussion ................................................................................................................................ 6 5 Conclusion and recommendations ........................................................................................ 6 Appendix 1 Heteropoly blues ................................................................................................. 8 Scanning Electron Microscopy ................................................................................................ 9 Inductively coupled plasma-atomic emission spectroscopy (ICP-AES) ............................... 10 X-ray fluorescence spectrometry (XRFS) .............................................................................. 11 6 References ............................................................................................................................. 12 ii IR/11/049; Version 3 Last modified: 2011/09/27 15:19 FIGURES Figure 1. Density as a function of viscosity adapted from http://www.heavyliquids.com . .......... 2 Figure 2. Simplified heavy media separation method.. c.100 ml LST added to separating funnel followed by c.50g sample and a further c.150ml LST, Particle dispersion following dispersion with a glass rod, Separation and division of minerals (c.20 minutes), Heavy mineral concentrate tapped off and recovered on filter paper. ................................. 4 Figure 3 Separation times for SPT (left) and LST (right): A. 0 Minutes, B. 5 Minutes, C. 10 Minutes and D. 20 Minutes. ..................................................................................................... 5 Figure 4 Left, Sample of beach sand. Right, heavy and light fractions, separated using LST. ...... 5 Figure 5. Example of heteropoly blues during LST testwork. ....................................................... 6 Figure 6. Optical photomicrograph showing heteropoly blues due to disc mill contamination. ... 8 Figure 7. Disc mill swarf with imbedded quartz. Note the iron oxide, a bi-product of wet sieving. ...................................................................................................................................... 8 Figure 8. BSEM photomicrograph of a disc mill swarf (un-milled) and associated EDXA spectra. .................................................................................................................................................. 9 Figure 9. BSEM photomicrograph of disc mill swarf (milled) engulfed with platy tungsten precipitates and associated EDXA spectra. ............................................................................ 10 Figure 10. ICP-AES data comparing clean LST with LST contaminated with ‘heteropoly blues’. ................................................................................................................................................ 10 TABLES Table 1. Common heavy liquids used for heavy media separations. ............................................. 1 Table 2. XRFS data. ..................................................................................................................... 11 Table 3. Percentage contamination from disc milling. ................................................................. 11 iii IR/11/049; Version 3 Last modified: 2011/09/27 15:19 Summary This report describes a suggested new procedure for heavy media separation using non-toxic lithium heteropolytungstate as a replacement for bromoform and other halogenated organic solvents. This work was carried out as part of the Science Facilities’ Maintenance and Development
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