analytical methods were used to obtain a large spectrum of major and trace element data, in particular, EPMA, SIMS, LA-ICPMS, and isotope dilution by TIMS and ICPMS. Altogether, more than 60 qualified geochemical laboratories worldwide contributed to the analyses, allowing us to present new reference and information values and their uncertainties (at 95% confidence level) for up to 74 elements. We complied with the recommendations for the certification of geological reference materials by the International Association of Geoanalysts (IAG). The reference values were derived from the results of 16 independent techniques, including definitive (isotope dilution) and comparative bulk (e.g., INAA, ICPMS, SSMS) and microanalytical (e.g., LA-ICPMS, SIMS, EPMA) methods. Agreement between two or more independent methods and the use of definitive methods provided traceability to the fullest extent possible. We also present new and recently published data for the isotopic compositions of H, B, Li, O, Ca, Sr, Nd, Hf, and Pb. The results were mainly obtained by high-precision bulk techniques, such as TIMS and MC-ICPMS. In addition, LA-ICPMS and SIMS isotope data of B, Li, and Pb are presented.
This paper reports the results from a second characterisation of the 91500 zircon, including data from electron probe microanalysis, laser ablation inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS), secondary ion mass spectrometry (SIMS) and laser fluorination analyses. The focus of this initiative was to establish the suitability of this large single zircon crystal for calibrating in situ analyses of the rare earth elements and oxygen isotopes, as well as to provide working values for key geochemical systems. In addition to extensive testing of the chemical and structural homogeneity of this sample, the occurrence of banding in 91500 in both backscattered electron and cathodoluminescence images is described in detail. Blind intercomparison data reported by both LA‐ICP‐MS and SIMS laboratories indicate that only small systematic differences exist between the data sets provided by these two techniques. Furthermore, the use of NIST SRM 610 glass as the calibrant for SIMS analyses was found to introduce little or no systematic error into the results for zircon. Based on both laser fluorination and SIMS data, zircon 91500 seems to be very well suited for calibrating in situ oxygen isotopic analyses.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS ) is a versatile technique for trace element analysis with respect to depth in solid samples. The high sensitivity of ICP-MS makes it possible to determine most elements in the periodic table at trace levels (<1 mg g−1). Recent trends in the development of instrumentation have led to the possibility of analysing craters of smaller diameter with variable depth. However, a major limitation to this approach for depth profiling, preventing accurate and precise analysis, is element-selective, non-reproducible ablation. The ability for representative sampling during depth analysis is tested in this study by ablating into homogeneous silica-based glass materials. Elemental relative response deviations of up to 300% are observed for selected elements during progressive ablation into the glass target. The geometry of the ablation crater controls the accuracy of sampling of the material at depth. Elemental fractionation becomes significant for some elements (e.g., Zn, Pb) when the depth/diameter ratio of the ablation crater is >6, corresponding to a 50% reduction in analyte response. Large diameter craters, if ablated with sufficient laser power density, reduce elemental fractionation and give a larger signal for a longer period of time, providing more suitable conditions for representative analysis. LA-ICP-MS can be a powerful technique for depth profiling provided that optimum analytical conditions are selected.
We applied laser-ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) as a new and precise technique for measuring trace elements in benthic foraminifera (Hoeglundina elegans). With this technique, trace element concentrations were accurately measured without the elaborate cleaning required in standard methods. Contaminated coatings are easily excluded during spatially resolved analysis. Application of this new technique allowed us to calibrate the trace elements incorporated in single tests of living (when sampled) benthic foraminifera to ambient seawater temperature (Mg and Sr) and redox conditions (Mn) for the first time. Incorporation of Ba showed a more complex pattern that cannot be explained by a direct correlation to water column concentration.
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