Using SIMS to diagnose color changes in heat treated gem sapphires

Novak, Steven W.; Magee, C. W.; Moses, Tom; Wang, Wuyi

doi:10.1016/j.apsusc.2004.03.171

Applied Surface Science

2004

DOI: 10.1016/j.apsusc.2004.03.171

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Using SIMS to diagnose color changes in heat treated gem sapphires

Steven W. Novak

C. W. Magee

Tom Moses

et al.

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Cited by 6 publications

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“…[5,6] Many significant efforts were quickly launched to try to identify the cause of yellow and brown colouration in Be-treated sapphires. [5,7,8] They endeavored to point out that this colour alteration would have been caused by the diffusion of beryllium from an external source. However, primary analysis provided by the Gemological Institute of America (GIA) laboratories using x-ray electron probe microscopy analysis (EPMA) and laser ablation inductively coupledplasma-mass spectrometry (LA-ICP-MS) was unable to detect any physical differences between the core and the rim parts of Be-treated sapphires.…”

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“…However, primary analysis provided by the Gemological Institute of America (GIA) laboratories using x-ray electron probe microscopy analysis (EPMA) and laser ablation inductively coupledplasma-mass spectrometry (LA-ICP-MS) was unable to detect any physical differences between the core and the rim parts of Be-treated sapphires. [7] These treated sapphires were subsequently acquired by Novak et al [8] for secondary ion mass spectroscopy (SIMS) analysis at Evans East. They presented the mass spectral analysis of the cores and rims of these stones using SIMS and detected a higher Be content in the coloured rims.…”

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confidence: 99%

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Revelation of Causes of Colour Change in Beryllium-Treated Sapphires

Limsuwan¹,

Meejoo²,

Somdee³

et al. 2008

Chinese Phys. Lett.

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Blue sapphires are treated with Be in oxidizing atmosphere to change the blue colour into yellow. Untreated and Be-treated samples are examined using laser ablation inductively coupled-plasma-mass spectrometry (LA-ICP-MS), electron spin resonance (ESR) and ultraviolet–visible (UV–vis) spectroscopy. The results show that the yellow colouration in Be-heated blue sapphires is not due to Be diffusion from the surface of sapphire. Be behaves as a sole catalyst in this process. We find that the charge transfer between the ferrous (Fe2+) and ferric (Fe3+) is the reason of the colour change. The above conclusions are confirmed by ESR measurements to determine the connections between the Fe3+ ions before and after Be-treated heat treatments.

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mentioning

confidence: 99%

mentioning

confidence: 99%

Revelation of Causes of Colour Change in Beryllium-Treated Sapphires

Limsuwan¹,

Meejoo²,

Somdee³

et al. 2008

Chinese Phys. Lett.

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Towards the differentiation of non-treated and treated corundum minerals by ion-beam-induced luminescence and other complementary techniques

et al. 2009

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Differentiation of treated and non-treated gemstones is a chief concern for major jewellery import companies. Low-quality corundum specimens coming from Asia appear to be often treated with heat, BeO or flux in order to enhance their properties as precious minerals. A set of corundum samples, rubies and sapphires from different origins, both treated and non-treated has been analysed at the Centre Européen d'Archéométrie, with ion-beam-induced luminescence (IBIL) and other complementary techniques such as Raman, proton-induced X-ray emission (PIXE), and proton-induced gamma-ray emission (PIGE). IBIL, also known as ionoluminescence, has been used before to detect impurities or defects inside synthetic materials and natural minerals; its use for the discrimination of gemstone simulants or synthetic analogues has been elsewhere discussed (Cavenago-Bignami Moneta, Gemología, Tomo I Piedras preciosas, perlas, corales, marfil. Ediciones Omega, Barcelona, 1991). PIXE has been frequently applied in the archaeometric field for material characterisation and provenance studies of minerals (Hughes, Ruby & sapphire. RWH Publishing, Fallbrook, 1997; Calvo del Castillo et al., Anal Bioanal Chem 387:869-878, 2007; Calligaro et al., NIM-B 189:320-327, 2002) and PIGE complements the elemental analysis by detecting light elements in these materials such as-and lighter than-sodium that cannot be identified with the PIXE technique (Sanchez et al., NIM-B 130:682-686, 1997; Emmett et al., Gems Gemology 39:84-135, 2003). The micro-Raman technique has also been used complementarily to ion beam analysis techniques for mineral characterisation (Novak et al., Appl Surf Sci 231-232:917-920, 2004). The aim of this study is to provide new means for systematic analysis of corundum gemstone-quality mineral, alternative to the traditional gemmologic methods; for this purpose, a Spanish jewellery import company supplied us with a number of natural corundum samples coming from different places (part of them treated as explained above). The PIXE elemental concentrations of the samples showed large quantities of calcium and lead in some cases that can be linked to treatment with fluxes or lead oxide. The plot of the chromium and iron concentration grouped the samples in various aggregates that corresponded to the different types of corundum analysed. Micro-Raman complemented the PIXE analysis corroborating the presence of lead oxides but the use of the PIGE technique was not successful for the detection of beryllium due to the low cross section of the nuclear reaction chosen for its identification. IBIL was capable of distinguishing between treated and non-treated samples of the same type based on the luminescent features of the materials.

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XPS and ToF-SIMS analysis of natural rubies and sapphires heated in an inert (N 2 ) atmosphere

Achiwawanich

James

Liesegang

2007

Applied Surface Science

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Using SIMS to diagnose color changes in heat treated gem sapphires

Cited by 6 publications

References 2 publications

Revelation of Causes of Colour Change in Beryllium-Treated Sapphires

Revelation of Causes of Colour Change in Beryllium-Treated Sapphires

Towards the differentiation of non-treated and treated corundum minerals by ion-beam-induced luminescence and other complementary techniques

XPS and ToF-SIMS analysis of natural rubies and sapphires heated in an inert (N 2 ) atmosphere

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