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Volume 33 / No. 1-4 / 2012 The Journal of Gemmology2012 / Volume 33 / Nos. 1/4 The Gemmological Association of Great Britain The Journal of Gemmology / 2012 / Volume 33 / No. 1–4 The Gemmological Association of Great Britain 27 Greville Street, London EC1N 8TN, UK T: +44 (0)20 7404 3334 F: +44 (0)20 7404 8843 E: [email protected] W: www.gem-a.com Registered Charity No. 1109555 Registered office: Palladium House, 1–4 Argyll Street, London W1F 7LD President: H. Levy Vice-Presidents: D. J. Callaghan, A. T. Collins, N. W. Deeks, E. A. Jobbins, M. J. O’Donoghue Honorary Life Members: A. J. Allnutt, H. Bank, T. M. J. Davidson, P. R. Dwyer-Hickey, G. M. Green, R. R. Harding, J. S. Harris, J. A. W. Hodgkinson, J. I. Koivula, C. M. Ou Yang, E. Stern, I. Thomson, V. P. Watson, C. H. Winter Chief Executive Officer: J. H. Riley Council: C. J. E. Oldershaw – Chairman, M. A. Burland, S. J. C. Collins, P. F. Greer, N. B. Israel, B. Jackson, A. H. Rankin, R. M. Slater, M. E. J. Wells, S. Whittaker, J. F. Williams Branch Chairmen: Midlands – P. Phillips, North East – M. Houghton, South East – V. Wetten, South West – R. M. Slater The Journal of Gemmology Acting Editor: Dr R. R. Harding Assistant Editor: M. J. O’Donoghue Associate Editors: Dr A. J. Allnutt (Chislehurst), Dr C. E. S. Arps (Leiden), Prof. A. T. Collins (London), J. Finlayson (Stoke-on-Trent), Dr J. W. Harris (Glasgow), E. A. Jobbins (Caterham), Dr J. M. Ogden (London), Prof. A. H. Rankin (Kingston upon Thames), Dr K. Schmetzer (Petershausen), Dr J. E. Shigley (Carlsbad), Prof. D. C. Smith (Paris), E. Stern (London), Prof. I. Sunagawa (Tokyo), Dr M. Superchi (Milan) Production Editor: M. A Burland The Editor is glad to consider original articles shedding new light on subjects of gemmological interest for publication in The Journal of Gemmology. A guide to the preparation of typescripts for publication in The Journal is given on our website, or contact the Production Editor at the Gemmological Association of Great Britain. Any opinions expressed in The Journal of Gemmology are understood to be the views of the contributors and not necessarily of the publishers. ©2012 The Gemmological Association of Great Britain The Journal of Gemmology / 2012 / Volume 33 / No. 1–4 Determining the geographical origins of natural emeralds through nondestructive chemical fingerprinting D.P. Cronin and A.M. Rendle Abstract: Analytical methods capable of differentiating trace elements in natural emerald may enable their geographical point of origin (GPO) to be elucidated. Emeralds were sampled from six distinct GPOs and the elemental composition of each sample was obtained nondestructively using energy dispersive X-ray spectroscopy (EDX). EDX results were chemometrically assessed for compositional differences and the results reveal that emeralds from the six GPOs possess a chemical identity that is statistically heterogeneous between GPOs, with the chromophores V, Ni and Mg being the most important trace elements for elucidating GPOs. Keywords: chemometrics, chromophore, emerald, energy dispersive X-ray spectroscopy, precipitation model Introduction mining operations — elucidating the from mining locations separated by only Evidenced from the earliest remnants point of origin of any gem material from a few kilometres (e.g. the Muzo and of human civilization, minerals have qualitative analyses alone would be Cosquez mining localities of Colombia) always been important natural resources irresponsible. The pursuit of scientific are distinctively different. Hence, even intimately linked to distinct cultural certainty relevant to mineral origin has within one basic precipitation model attributes such as personal adornment, greatly advanced in the past decade and for fluid processes culminating within a religious and secular customs, wealth continues to take monumental strides single geological formation there exist a and trade, and the arts. Determining towards a unified body of science. range of even more subtle precipitation the geographical point of origin of This research began towards mechanisms and fluid dynamics leading to minerals and other gems from antiquity identifying and relating trace elemental chemical heterogeneity between emerald required little more than a qualitative differences in emeralds from the Cordillera points of origin. understanding of cultural anthropology, Oriental in Colombia, differences which The initial data that emerged changed geographically specific artisanship, had arisen as a result of interstitial fluid the course of the research when it was traditional trade routes, and/or mining migration prior to precipitation. Although recognized that within-site chemical regions consistent with the age-specific the more subtle processes that link homogeneity and between-sites chemical attributes of the artefact. But with geochemical interactions to the precise heterogeneity was contingent on the advances in geophysical surveying and incorporation of trace elements remains chromophore concentrations in the increased global trade throughout the past poorly understood, this research revealed crystal structure. This unanticipated century — coupled with a combination that the chemical composition of emeralds result during the course of investigating of corporatized, indigenous and illegal — particularly the chromophores — the chemistry of interstitial fluids during ©2012 The Gemmological Association of Great Britain Page 1 The Journal of Gemmology / 2012 / Volume 33 / No. 1–4 Determining the geographical origins of natural emeralds through nondestructive chemical fingerprinting Hutton, 1978), it has since been suggested a b that Cr3+ in a coupled substitution with a monovalent cation may occupy tetravalent sites normally containing the framework silicon ion (Si4+) (Parikh et al., 2003). Whereas the primary chromophore(s) d e in the chemical framework give emeralds their distinctive green colour, it is the incorporation of secondary chromophores 2+ 3+ 2+ c (i.e. Fe , Fe , Ni ) that alter the chroma g of emeralds and lead to their wide- range of visible chromaticity. Much of the chromaticity dynamics results from f secondary chromophores competing for the Cr3+ and V3+ sites, thereby depleting concentrations of Cr3+ and V3+ (Platonov, Taran and Balitsky, 1984). More importantly, secondary chromophores are polyvalent ions that act as electron withdrawing groups. Their incorporation Figure 1: Each of the 36 emerald samples was mounted on an aluminium stud with silver into the crystal structure imparts an effect conductive paint for SEM-EDX analysis. The studs were etched with numbered pie-shaped sectors for on the visible spectrum that shifts the identification during SEM-EDX analysis and each stud was drilled for use with a positioning and Cr3+ and V3+ absorption bands towards removal tool to prevent contamination. (a) CZC, (b) MZC, (c) CVC, (d) ZAM, (e) ZAM, (f) GOB and longer wavelengths. For example, Al3+ (g) CFB. Photo by D. P. Cronin. can be substituted with ferric iron (Fe3+) tectonic precipitation dynamics in transmits the distinctive green hue or with magnesium (Mg2+), the latter the Cordillera Oriental quickly led to and treasured chroma that defines the requiring a coupled substitution with a this research evolving to determine if emerald variety. Because beryllium and monovalent cation (Acharya et al., 2000; chemical heterogeneity between emerald the primary chromophores necessary Parikh et al., 2003), leading to red-shifting mining localities was chemometrically for emerald precipitation, chromium in the absorption bands. With a lack of unique and statistically significant based and vanadium, are not normally in close d-electrons and no electronic transitions on chromophore constituents alone. association in Nature, the rarity of this in the visible region, Mg2+ would normally To test this assertion, three additional geochemical concurrence is the reason not be considered to be a secondary sites (two in Brazil and one in Zambia) for the scarcity of emerald occurrences chromophore, but its presence can shift were sampled and assessed for their worldwide (Schwarz and Giuliani, 2001). absorption bands and alter the colour architectural chemistries and chromophore The selective substitution of metal of an emerald. In addition to Fe3+ and constituents. cations in the beryl crystal structure, Mg2+ placement into Al3+ sites, Fe3+, Mg2+ such as the incorporation of chromium and divalent ferrous iron (Fe2+) ions can Natural emeralds ions (Cr3+) in octahedral sites that would each occupy the divalent beryllium (Be2+) Emerald is the richly coloured green otherwise host the framework aluminium tetrahedral sites (Braga et al., 2002); again, variety of the mineral species beryl. ion (Al3+) (Hasan, Keany and Manson, red-shifting the chromium and vanadium As an allochromatic mineral species 1986; Parikh et al., 2003; Acharya et al., absorption bands and changing the hue that is colourless and transparent in its 2000; Kim et al., 2000; Nassau, 1978), and chroma of emerald. purest state (var. goshenite), beryl does produces the defining hue of emerald In addition to the primary and not meet the defined characteristics of (Kleiðmantas and Skridlaitë, 2004). secondary chromophore elements, emerald unless the requisite chromophore Emeralds with characteristically low emeralds also contain other trace elements are properly incorporated chromium content often contain the elements that reflect the localized into the six-member cyclosilicate crystal trivalent primary chromophore vanadium geology and fluid-rock interaction
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