U–Pb ages of several apatite reference materials, acquired by LA-ICP-MS over a 3.5 year period using the Otter Lake apatite as a primary standard, show systematic offsets (up to 3%) from reference ages obtained by isotope dilution mass spectrometry. The offsets are well outside known analytical errors from counting statistics, uncertainty in common Pb corrections or excess 206Pb in high-Th/U materials. The age offsets also do not correlate strongly with the concentrations of F, Cl, REE, Th and U, with accumulated radiation dose or with the depth of ablation pits. We suggest that the observed age offsets are related to elemental fractionation at the ablation site, but their direction and magnitude cannot at present be predicted from compositional differences in different apatite samples. Our results further suggest that Otter Lake apatite is too heterogeneous for use as a calibration standard. Two other apatite samples, OD306 (1596.7 ± 7.1 Ma) and the 401 apatite (530.3 ± 1.5 Ma) are introduced as potential U–Pb reference materials.
30 April 2019 in Geostandards and Geoanalytical Research
A new olivine reference material – MongOL Sh11‐2 – for in situ analysis has been prepared from the central portion of a large (20 × 20 × 10 cm) mantle peridotite xenolith from a ~ 0.5 My old basaltic breccia at Shavaryn‐Tsaram, Tariat region, central Mongolia. The xenolith is a fertile mantle lherzolite with minimal signs of alteration. Approximately 10 g of 0.5–2 mm gem quality olivine fragments were separated under binocular microscope and analysed by EPMA, LA‐ICP‐MS, SIMS and bulk analytical methods (ID‐ICP‐MS for Mg and Fe, XRF, ICP‐MS) for major, minor and trace elements at six institutions world‐wide. The results show that the olivine fragments are sufficiently homogeneous with respect to major (Mg, Fe, Si), minor and trace elements. Significant inhomogeneity was revealed only for phosphorus (homogeneity index of 12.4), whereas Li, Na, Al, Sc, Ti and Cr show minor inhomogeneity (homogeneity index of 1–2). The presence of some mineral and fluid‐melt micro‐inclusions may be responsible for the inconsistency in mass fractions obtained by in situ and bulk analytical methods for Al, Cu, Sr, Zr, Ga, Dy and Ho. Here we report reference and information values for twenty‐seven major, minor and trace elements.
Strontium titanate SrTiO3(100), (110), and (111) single crystals, undoped or donor doped with up to 1 at% La, were isothermally equilibrated at temperatures between 1523 and 1773 K in synthetic air followed by two different methods of Sr tracer deposition: ion implantation of 87Sr and chemical solution deposition of a thin 86SrTiO3 layer. Subsequently, the samples were diffusion annealed under the same conditions as before. The initial and final depth profiles were measured by SIMS. For strong La-doping both tracer deposition methods yield similar Sr diffusion coefficients, whereas for weak doping the tracer seems to be immobile in the case of ion implantation. The Sr diffusivity does not depend on the crystal orientation, but shows strong dependency on the dopant concentration supporting the defect chemical model that under oxidizing conditions the donor is compensated by Sr vacancies. A comparison with literature data on Sr vacancy, Ti, and La diffusion in this system confirms the concept that all cations move via Sr vacancies. Cation diffusion is several orders of magnitude slower than oxygen diffusion.