Geological reference materials (RMs) with variable compositions and NIST SRM 612 were analysed by isotope dilution mass spectrometry for bulk rock concentrations of chalcogen elements (sulfur, selenium and tellurium), rhenium and platinum‐group elements (PGEs: Ru, Pd, Os, Ir and Pt), including the isotope amount ratios of 187Os/188Os. All concentrations were obtained from the same aliquot after HCl‐HNO3 digestion in a high pressure asher at 320 °C. Concentrations were determined after chemical separation by negative TIMS, ICP‐MS and hydride generation ICP‐MS (Se, Te). As in previous studies, concentrations of the PGEs in most RMs were found to be highly variable, which may be ascribed to sample heterogeneity at the < 1 g level. In contrast, S, Se and Te displayed good precision (RSD < 5%) in most RMs, suggesting that part of the PGE budget is controlled by different phases, compared with the chalcogen budget. The method may minimise losses of volatile chalcogens during the closed‐system digestion and indicates the different extent of heterogeneity of chalcogens, Re and PGEs in the same sample aliquot. OKUM, SCo‐1, MRG‐1, DR‐N and MAG‐1 are useful RMs for the chalcogens. NIST SRM 612 displays homogenous distribution of S, Se, Te, Pt and Pd in 30 mg aliquots, in contrast with micro‐scale heterogeneity of Se, Pd and Pt. 相似文献
Mineral inclusions recovered from 100 diamonds from the A154 South kimberlite (Diavik Diamond Mines, Central Slave Craton, Canada) indicate largely peridotitic diamond sources (83%), with a minor (12%) eclogitic component. Inclusions of ferropericlase (4%) and diamond in diamond (1%) represent “undetermined” parageneses.
Compared to inclusions in diamonds from the Kaapvaal Craton, overall higher CaO contents (2.6 to 6.0 wt.%) of harzburgitic garnets and lower Mg-numbers (90.6 to 93.6) of olivines indicate diamond formation in a chemically less depleted environment. Peridotitic diamonds at A154 South formed in an exceptionally Zn-rich environment, with olivine inclusions containing more than twice the value (of 52 ppm) established for normal mantle olivine. Harzburgitic garnet inclusions generally have sinusoidal rare earth element (REEN) patterns, enriched in LREE and depleted in HREE. A single analyzed lherzolitic garnet is re-enriched in middle to heavy REE resulting in a “normal” REEN pattern. Two of the harzburgitic garnets have “transitional” REEN patterns, broadly similar to that of the lherzolitic garnet. Eclogitic garnet inclusions have normal REEN patterns similar to eclogitic garnets worldwide but at lower REE concentrations.
Carbon isotopic values (δ13C) range from − 10.5‰ to + 0.7‰, with 94% of diamonds falling between − 6.3‰ and − 4.0‰. Nitrogen concentrations range from below detection (< 10 ppm) to 3800 ppm and aggregation states cover the entire spectrum from poorly aggregated (Type IaA) to fully aggregated (Type IaB). Diamonds without evidence of previous plastic deformation (which may have accelerated nitrogen aggregation) typically have < 25% of their nitrogen in the fully aggregated B-centres. Assuming diamond formation beneath the Central Slave to have occurred in the Archean [Westerlund, K.J., Shirey, S.B., Richardson, S.H., Gurney, J.J., Harris, J.W., 2003b. Re–Os systematics of diamond inclusion sulfides from the Panda kimberlite, Slave craton. VIIIth International Kimberlite Conference, Victoria, Canada, Extended Abstracts, 5p.], such low aggregation states indicate mantle residence at fairly low temperatures (< 1100 °C). Geothermometry based on non-touching inclusion pairs, however, indicates diamond formation at temperatures around 1200 °C. To reconcile inclusion and nitrogen based temperature estimates, cooling by about 100–200 °C shortly after diamond formation is required. 相似文献
Ice core from Greenland was melted, filtered, homogenised, loaded into glass ampoules, sealed, autoclaved to eliminate biological activity, and calibrated by dual‐inlet isotope‐ratio mass spectrometry. This isotopic reference material (RM), USGS46, is intended as one of two secondary isotopic reference waters for daily normalisation of stable hydrogen (δ2H) and stable oxygen (δ18O) isotopic analysis of water with a mass spectrometer or a laser absorption spectrometer. The measured δ2H and δ18O values of this reference water were ?235.8 ± 0.7‰ and ?29.80 ± 0.03‰, respectively, relative to VSMOW on scales normalised such that the δ2H and δ18O values of SLAP reference water are, respectively, ?428 and ?55.5‰. Each uncertainty is an estimated expanded uncertainty (U =2uc) about the reference value that provides an interval that has about a 95‐percent probability of encompassing the true value. This reference water is available in cases containing 144 glass ampoules that are filled with either 4 ml or 5 ml of water per ampoule. 相似文献
The interest in variations of barium (Ba) stable isotope amount ratios in low and high temperature environments has increased over the past several years. Characterisation of Ba isotope ratios of widely available reference materials is now required to validate analytical procedures and to allow comparison of data obtained by different laboratories. We present new Ba isotope amount ratio data for twelve geological reference materials with silicate (AGV‐1, G‐2, BHVO‐1, QLO‐1, BIR‐1, JG‐1a, JB‐1a, JR‐1 and JA‐1), carbonate (IAEA‐CO‐9) and sulfate matrices (IAEA‐SO‐5 and IAEA‐SO‐6) relative to NIST SRM 3104a. In addition, two artificially fractionated in‐house reference materials BaBe12 and BaBe27 (δ137/134Ba = ?1.161 ± 0.049‰ and ?0.616 ± 0.050‰, respectively) are used as quality control solutions for the negative δ‐range. Accuracy of our data was assessed by interlaboratory comparison between the University of Bern and the United States Geological Survey (USGS). Data were measured by MC‐ICP‐MS (Bern) and TIMS (USGS) using two different double spikes for mass bias correction (130Ba–135Ba and 132Ba–136Ba, respectively). MC‐ICP‐MS measurements were further tested for isobaric and non‐spectral matrix effects by a number of common matrix elements. The results are in excellent agreement and suggest data accuracy. 相似文献
The calcium isotopic composition of NIST SRM 915b and 1486 provided by the National Institute of Standards and Technology was analysed. The δ44/40Ca values of the two reference materials relative to NIST SRM 915a were: NIST SRM 915b =+0.72 ± 0.04‰ and NIST SRM 1486 =?1.01 ± 0.02‰. NIST SRM 1486 did not require any chemical separation prior to measurement. 相似文献
Fluid inclusions represent a unique opportunity for a straightforward determination of the chemical and isotopic composition of fluids that composed the hydrosphere and atmosphere over Earth’s history. The production of reference materials in the laboratory is needed to monitor and to validate the determination of hydrogen and oxygen isotope compositions of water inclusions. We propose a protocol leading to the experimental synthesis of halite crystals that contain water inclusions whose δD and δ18O values can be related to those of surrounding evaporating waters where the crystals grew. Corrections to isotopic measurements were performed by applying an orthogonal projection of the raw data to the water evaporation trajectory line whose slope can be predicted by taking into account the parameters developed in the linear resistance model of Craig and Gordon (1965). Several hundreds of grams of halite reference material can be produced rapidly (within 2 d) at a low cost and can be stored within a vacuum desiccator at ambient temperature over several months or years. The described method is especially useful for the analysis of anhydrous salts and the interpretation of isotopic fractionations that operate within the surficial water cycle. 相似文献