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Kathryn A. Matthews Michael T. Murrell Steven J. Goldstein Andrew J. Nunn Deborah E. Norman 《Geostandards and Geoanalytical Research》2011,35(2):227-234
Here we report uranium and thorium isotopic ratios and elemental concentrations measured in solid reference materials from the USGS (BHVO‐2G, BCR‐2G, NKT‐1G), as well as those from the MPI‐DING series (T1‐G, ATHO‐G). Specifically created for microanalysis, these naturally‐sourced glasses were fused from rock powders. They cover a range of compositions, elemental concentrations and expected isotopic ratios. The U‐Th isotopic ratios of two powdered source materials (BCR‐2, BHVO‐2) were also characterised. These new measurements via multi‐collector thermal ionisation mass spectrometry and multi‐collector inductively coupled plasma‐mass spectrometry can now be used to assess the relative performance of techniques and facilitate comparison of U‐Th data amongst laboratories in the geoscience community for in situ and bulk analyses. 相似文献
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Klaus Peter Jochum Steven A. Wilson Wafa Abouchami Marghaleray Amini Jérome Chmeleff Anton Eisenhauer Ernst Hegner Linda M. Iaccheri Bruno Kieffer Joachim Krause William F. McDonough Regina Mertz‐Kraus Ingrid Raczek Roberta L. Rudnick Denis Scholz Grit Steinhoefel Brigitte Stoll Andreas Stracke Sonia Tonarini Dominique Weis Ulrike Weis Jon D. Woodhead 《Geostandards and Geoanalytical Research》2011,35(2):193-226
This paper contains the results of an extensive isotopic study of United States Geological Survey GSD‐1G and MPI‐DING reference glasses. Thirteen different laboratories were involved using high‐precision bulk (TIMS, MC‐ICP‐MS) and microanalytical (LA‐MC‐ICP‐MS, LA‐ICP‐MS) techniques. Detailed studies were performed to demonstrate the large‐scale and small‐scale homogeneity of the reference glasses. Together with previously published isotopic data from ten other laboratories, preliminary reference and information values as well as their uncertainties at the 95% confidence level were determined for H, O, Li, B, Si, Ca, Sr, Nd, Hf, Pb, Th and U isotopes using the recommendations of the International Association of Geoanalysts for certification of reference materials. Our results indicate that GSD‐1G and the MPI‐DING glasses are suitable reference materials for microanalytical and bulk analytical purposes. 相似文献
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Klaus Peter Jochum Ulrike Weis Brigitte Stoll Dmitry Kuzmin Qichao Yang Ingrid Raczek Dorrit E. Jacob Andreas Stracke Karin Birbaum Daniel A. Frick Detlef Günther Jacinta Enzweiler 《Geostandards and Geoanalytical Research》2011,35(4):397-429
We present new reference values for the NIST SRM 610–617 glasses following ISO guidelines and the International Association of Geoanalysts’ protocol. Uncertainties at the 95% confidence level (CL) have been determined for bulk‐ and micro‐analytical purposes. In contrast to former compilation procedures, this approach delivers data that consider present‐day requirements of data quality. New analytical data and the nearly complete data set of the GeoReM database were used for this study. Data quality was checked by the application of the Horwitz function and by a careful investigation of analytical procedures. We have determined quantitatively possible element inhomogeneities using different test portion masses of 1, 0.1 and 0.02 μg. Although avoiding the rim region of the glass wafers, we found moderate inhomogeneities of several chalcophile/siderophile elements and gross inhomogeneities of Ni, Se, Pd and Pt at small test portion masses. The extent of inhomogeneity was included in the determination of uncertainties. While the new reference values agree with the NIST certified values with the one exception of Mn in SRM 610, they typically differ by as much as 10% from the Pearce et al. (1997) values in current use. In a few cases (P, S, Cl, Ta, Re) the discrepancies are even higher. 相似文献
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Qi‐Chao Yang Klaus Peter Jochum Brigitte Stoll Ulrike Weis Dmitry Kuzmin Michael Wiedenbeck Heike Traub Meinrat O. Andreae 《Geostandards and Geoanalytical Research》2012,36(3):301-313
To test whether the silicate reference glasses BAM‐S005‐A and BAM‐S005‐B from BAM (The Federal Institute for Materials Research and Testing, Germany) are suitable materials for microanalysis, we investigated the homogeneity of these reference glasses using the microanalytical techniques EPMA, LA‐ICP‐MS and SIMS. Our study indicated that all major and most trace elements are homogeneously distributed at micrometre sampling scale in both types of glass. However, some trace elements (e.g., Cs, Cl, Cr, Mo and Ni) seem to be inhomogeneously distributed. We also determined the composition of BAM‐S005‐A and BAM‐S005‐B. The EPMA data of major elements confirmed the information values specified by the certificate. With the exception of Sr, Ba, Ce and Pb, our trace element data by LA‐ICP‐MS were also in agreement with the certified values within the stated uncertainty limits. The reasons for the discrepancy in these four elements are still unclear. In addition, we report new data for twenty‐two further trace elements, for which the concentrations were not certified. Based on our investigation, we suggest that both of these materials are suitable for many microanalytical applications. 相似文献
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Dorothea S. Macholdt Klaus Peter Jochum Stephen A. Wilson Laura M. Otter Brigitte Stoll Ulrike Weis Meinrat O. Andreae 《Geostandards and Geoanalytical Research》2016,40(4):493-504
Manganese‐ and iron‐rich materials are of major geoscientific and economic interest, many of which contain microscopic features that provide valuable information. To obtain accurate results, a homogeneous microanalytical reference material for calibration is needed. Several researchers have used the Mn‐ and Fe‐rich RMs, JMn‐1, NOD‐A‐1, NOD‐P‐1 and FeMn‐1, for this purpose; therefore, they were tested in this study to determine their suitability for microanalysis. Their homogeneity was investigated by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) with two different types of lasers (nano‐ and femtosecond), with spot and line scan analyses and with different operating parameters, such as spot size, pulse repetition rate and fluence. As the established manganese nodule RMs revealed inhomogeneities for picogram to microgram test portions, we also investigated the new synthetic Fe‐ and Mn‐rich RM, FeMnOx‐1. FeMnOx‐1 was found to be homogeneous for large (ø 40 μm: 2% RSD repeatability) and small (ø 8–10 μm: 10% RSD repeatability) spot sizes. This homogeneity is in the range of the homogeneous NIST SRM 610 and GSE‐1G reference glasses. Furthermore, FeMnOx‐1 revealed a large‐scale homogeneity within uncertainties of a few per cent, using test portions in the ng range, when measuring four individual mounts of this material. 相似文献
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Peter Sjövall Volker Thiel Sandra Siljeström Christine Heim Tomas Hode Jukka Lausmaa 《Geostandards and Geoanalytical Research》2008,32(3):267-277
Time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) is a powerful method for the chemical analysis of solid surfaces. In this paper, the capabilities and limitations of this technique and the potential for its use in geochemical research are outlined. Using ToF‐SIMS, the chemical composition of sample structures down to 10–100 μm can be determined, without the need for pre‐selection or labelling of the analysed substances. In addition, the lateral distribution of organic and inorganic compounds can be mapped in geochemical samples at a resolution in the micrometre range. The capabilities of the technique in geochemistry are illustrated by two examples. In the first example, it is shown that ToF‐SIMS can be used to detect biomarkers in oil samples, making it a promising method for the analysis of biomarkers in fluid inclusions. In the second example, a number of specific lipid biomarkers were identified and mapped on the surface of a microbial mat cryosection surface. Post‐measurement optical microscopy correlated the localisation of the lipids with the presence of methanotrophic archaea in the microbial mat. 相似文献
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Magne Ødegård 《Geostandards and Geoanalytical Research》1999,23(2):173-186
This paper describes a technique for the preparation of synthetic calibration materials for use in laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) and other microtechniques for mineral analysis. The method is based on direct fusion in high-purity graphite electrodes, and the requisite temperatures for melting are obtained by resistance heating using a welding rectifier as the power source. The technique has been tested on quartz (SiO2) and rutile (TiO2) for a relatively large range of elements, including all the rare earth elements. Different starting materials for preparation of calibration materials were studied, and it is shown that many natural materials form separate phases during fusion, resulting in unusable calibration materials for microanalysis. However, calibration materials prepared fully synthetically from oxides and/or element nitrates in solution were found to be of good homogeneity, and this preparation technique was used throughout in this work. The quality of the calibration materials for quartz and rutile was assessed by LA-ICP-MS, using Si and Ti as internal standard elements respectively. The NIST SRM 612 and 614 glass standards were used to assess the accuracy of the calibration materials for quartz. Calibration curves based on two independently prepared sets of calibration materials and the two NIST glasses are shown for a number of elements, demonstrating excellent agreement between the NIST glasses and the synthetically prepared quartz glasses. Vesicles are shown to form in the SiO2 glasses, but this does not influence their value as calibration materials, provided that a reference element is used as an internal standard. The advantages of fusion in high-purity graphite electrodes are emphasised, particularly the very high sublimation point of graphite, its very high state of purity, the very short melting and quench time, the speed and simplicity of the method, and the low risk of introducing impurities. Extension of the method to other minerals and applications is discussed. 相似文献
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