ALBERT

Description: Advances in the chemical, crystallographic and isotopic characterisation of geological and environmental materials can often be ascribed to technological improvements in analytical hardware or to innovative approaches to data acquisition and/or its interpretation. This biennial review addresses key laboratory methods that form much of the foundation for analytical geochemistry; again this contribution is presented as a compendium of laboratory techniques. We highlight advances that have appeared since January 2012 and that are of particular significance for the chemical and isotopic characterisation of geomaterials. Prominent scientists from the selected analytical fields present publications they judge to be particular noteworthy, providing background information about the method and assessing where further opportunities might be anticipated. In addition to well established technologies such as thermal ionisation mass spectrometry and plasma emission spectroscopy, this publication also presents new or rapidly growing methods such as electron backscattered diffraction analysis and atom probe tomography – a very sensitive method providing atomic scale information. This article is protected by copyright. All rights reserved.

Description: Key Points Homogeneous (x, y and z) geochemical references materials can be produced by multi‐energy ion implantation. First quantification results are promising. ’Box‐profile’ implants are suitable for use as reference materials for SIMS measurements. The multi‐energy ion implantation technique has the potential to produce EPMA‐suitable reference materials. Although electron probe microanalysis and secondary ion mass spectrometry are widely used analytical techniques for geochemical and mineralogical applications, metrologically rigorous quantification remains a major challenge for these methods. Secondary ion mass spectrometry (SIMS) in particular is a matrix‐sensitive method, and the use of matrix‐matched reference materials (RMs) is essential to avoid significant analytical bias. A major problem is that the number of available RMs for SIMS is extremely small compared with the needs of analysts. One approach for the production of matrix‐specific RMs is the use of high‐energy ion implantation that introduces a known amount of a selected isotope into a material. We chose the more elaborate way of implanting a so‐called ‘box‐profile’ to generate a quasi‐homogeneous concentration of the implanted isotope in three dimensions, which allows RMs not only to be used for ion beam analysis but also makes them suitable for EPMA. For proof of concept, we used the thoroughly studied mineralogically and chemically ‘simple’ SiO2 system. We implanted either 47Ti or 48Ti into synthetic, ultra‐high‐purity silica glass. Several ‘box‐profiles’ with mass fractions between 10 and 1000 μg g−1 Ti and maximum depths of homogeneous Ti distribution between 200 nm and 3 μm were produced at the Institute of Ion Beam Physics and Materials Research of Helmholtz‐Zentrum Dresden‐Rossendorf. Multiple implantation steps using varying ion energies and ion doses were simulated with Stopping and Range of Ions in Matter (SRIM) software, optimising for the target concentrations, implantation depths and technical limits of the implanter. We characterised several implant test samples having different concentrations and maximum implantation depths by means of SIMS and other analytical techniques. The results show that the implant samples are suitable for use as reference materials for SIMS measurements. The multi‐energy ion implantation technique also appears to be a promising procedure for the production of EPMA‐suitable reference materials.

Description: Advances in the chemical and isotopic characterisation of geological and environmental materials can often be ascribed to technological improvements in analytical hardware. Equally, the creation of novel methods of data acquisition and interpretation, including access to better reference materials, can also be crucial components enabling important breakthroughs. This biennial review highlights key advances in either instrumentation or data acquisition and treatment which have appeared since January 2010. This review is based on the assessments by scientists prominent in each of the given analytical fields; it is not intended as an exhaustive summary, but rather provides insight from experts of the most significant advances and trends in their given field of expertise. In contrast to earlier reviews, this presentation has been formulated into a unified work, providing a single source covering a broad spectrum of geoanalytical techniques. Additionally, some themes that were not previously emphasised, in particular TIMS, accelerator-based methods and vibrational spectroscopy, are also presented in detail. © 2012 The Authors. Geostandards and Geoanalytical Research © 2012 International Association of Geoanalysts

Description: 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. Afin de tester si les verres silicatés de référence BAM-S005-A et BAM-S005-B provenant du BAM (Institut fédéral de recherche et d’essais sur les matériaux, Allemagne) sont des matériaux appropriés pour la microanalyse, nous avons étudié l’homogénéité de ces verres de référence en utilisant les techniques de microanalyse EPMA, LA-ICP-MS et SIMS. Notre étude a révélé que tous les éléments majeurs et la plupart des éléments traces sont répartis de façon homogène dans les deux types de verre à l’échelle micrométrique d’échantillonnage. Toutefois, certains éléments traces (par exemple, Cs, Cl, Cr, Mo et Ni) semblent être distribués de façon inhomogène. Nous avons également déterminé les compositions de BAM-S005-A et BAM-S005-B. Les données EPMA des éléments majeurs ont confirmé les valeurs spécifiées par le certificat. À l’exception du Sr, Ba, Ce et Pb, nos données d’éléments traces par LA-ICP-MS sont également en accord avec les valeurs certifiées dans les limites d’incertitude indiquées. Les raisons des écarts observés pour ces quatre éléments sont encore mal connues. En outre, nous présentons de nouvelles données pour vingt-deux éléments traces supplémentaires, pour lesquels les concentrations n’ont pas été certifiées. Sur la base de notre étude, nous suggérons que ces deux matériaux sont adaptés pour de nombreuses applications de microanalyse.

Description: Secondary ion mass spectrometry (SIMS or ion microprobe) remains one of the most powerful techniques in the analytical geochemist’s toolkit. The key strength of SIMS is its capacity to provide trace element and isotope data at sampling sizes which are not approached by other methods. As compared with the main competing technique of laser ablation-ICP-MS, SIMS commonly provides a total sampling mass some 10 to 500 times smaller; this feature can be the deciding factor as to whether an analytical objective is technically achievable. Additional strengths of SIMS lie in the areas of depth profiling and trace element imaging. Though perhaps not as commonly used in the geosciences, these two operational modes represent unique capabilities of SIMS.

Description: This collection of articles represents the fourth in a series of reviews in which authors have aimed at capturing the key advances in a range of analytical fields ( Hergt et al. 2005, 2006, 2008 ). The publication period under review is 2008–2009 and the intention here is to provide readers with a summary of the most influential developments published during this period, across a broad range of topics appropriate to the Earth and environmental sciences. Most authors comment on the ways in which the emphases of research in their specific fields of examination have changed over time. All note an increase in rigour and focus on data quality. Whether advances have taken place in instrumentation, sample manipulation or data deconvolution, there are a large number of dedicated scientists out there contributing to the high quality of geochemical data employed in geological and environmental research.

Description: Abstract Although electron probe microanalysis and secondary ion mass spectrometry are widely used analytical techniques for geochemical and mineralogical applications, metrologically rigorous quantification remains a major challenge for these methods. SIMS in particular is a matrix‐sensitive method; for SIMS the use of matrix‐matched reference materials (RMs) is essential in order to avoid significant analytical bias. A major problem is that the number of available RMs for SIMS is extremely small compared with the needs of the analyst. One approach for the production of matrix‐specific RMs is the use of high‐energy ion implantation that introduces a known amount of a selected isotope into a material. We chose the more elaborate way of implanting a so‐called ‘box profile’ to generate a quasi‐homogeneous concentration of the implanted isotope in three dimensions, which allows RMs not only to be used for ion beam analysis but also makes them suitable for EPMA. For proof of concept, we used the thoroughly studied mineralogically and chemically ‘simple’ SiO2 system. We implanted either 47Ti or 48Ti into synthetic, ultra‐high purity silica glass. Several ‘box profiles’ with concentrations between 10 and 1000 μg g−1 Ti and maximum depths of homogeneous Ti distribution between 200 nm and 3 μm were produced at the Institute of Ion Beam Physics and Materials Research of Helmholtz‐Zentrum Dresden‐Rossendorf (HZDR). Multiple implantation steps using varying ion energies and ion doses were simulated with the SRIM (Stopping and Range of Ions in Matter) software (Ziegler et al. 2008), optimising for the target concentrations, implantation‐depths and technical limits of the implanter. We characterised several implant test‐samples having different concentrations and maximum implantation depths by means of SIMS and other analytical techniques. The results show that the implant samples are suitable for use as reference materials for SIMS measurements. The multi‐energy ion implantation technique also looks to be very promising procedure for the production of EPMA‐suitable reference materials. This article is protected by copyright. All rights reserved.

Description: We systematically measured oxygen self-diffusion coefficients ( D O ) in forsterite along b - crystallographic axis at a pressure of 8 GPa and temperatures of 1600 – 1800 K, over a wide range of water content ( C H2O ) from 〈1 up to ~800 wt. ppm. The experimental results suggest that D O ∝ ( C H2O ) 0.05±0.06  ≈ ( C H2O ) 0 . Thus, water has no significant effect on oxygen self-diffusion rate in forsterite. Since the C H2O dependence of silicon self-diffusion rate is also very small [ Fei et al ., 2013], the effect of water on olivine rheology is not significant by assuming the diffusion controlled creep mechanism.

Description: Here we document a detailed analytical characterisation of zircon M127, a homogeneous 12.7 carat gemstone from Ratnapura, Sri Lanka. Zircon M127 has TIMS-determined mean U-Pb radiogenic isotopic ratios of 0.084743 ± 0.000027 for 206 Pb/ 238 U and 0.67676 ± 0.00023 for 207 Pb/ 235 U (weighted means, 2 s uncertainties). Its 206 Pb/ 238 U age of 524.36 ± 0.16 Ma (95% confidence uncertainty) is concordant within the uncertainties of decay constants. The δ 18 O value (determined by laser fluorination) is 8.26 ± 0.06‰ VSMOW (2 s ), and the mean 176 Hf/ 177 Hf ratio (determined by solution ICP-MS) is 0.282396 ± 0.000004 (2 s ). The SIMS-determined δ 7 Li value is -0.6 ± 0.9‰ (2 s ), with a mean mass fraction of 1.0 ± 0.1 μg g −1 Li (2 s ). Zircon M127 contains ~ 923 μg g −1 U. The moderate degree of radiation damage corresponds well with the time-integrated self-irradiation dose of 1.82 × 10 18 alpha events per gram. This observation, and the (U-Th)/He age of 426 ± 7 Ma (2 s ), which is typical of unheated Sri Lankan zircon, enable us to exclude any thermal treatment. Zircon M127 is proposed as a reference material for the determination of zircon U-Pb ages by means of SIMS analysis in combination with hafnium and stable-isotope (oxygen and potentially also lithium) analysis. This article is protected by copyright. All rights reserved.

Description: Minerals, Vol. 8, Pages 175: The Hydrothermal Breccia of Berglia-Glassberget, Trøndelag, Norway: Snapshot of a Triassic Earthquake Minerals doi: 10.3390/min8050175 Authors: Axel Müller Morgan Ganerød Michael Wiedenbeck Skule Svendsen Spjelkavik Rune Selbekk The quartz-K-feldspar-cemented breccia of Berglia-Glassberget in the Lierne municipality in central Norway forms an ellipsoid structure 250 m × 500 m in size. The hydrothermal breccia is barren in terms of economic commodities but famous among mineral collectors for being a large and rich site of crystal quartz of various colours and habits. Despite being a famous collector site, the mineralization is rather unique in respect to its geological setting. It occurs within Late Palaeoproterozoic metarhyolites of the Lower Allochthon of the Norwegian Caledonides regionally isolated from any other contemporaneous hydrothermal or magmatic event. In order to understand better the formation of the Berglia-Glassberget breccia, the chemistry, fluid inclusion petrography and age of the breccia cement were determined. Structural features indicate that the Berglia-Glassberget is a fault-related, fluid-assisted, hydraulic breccia which formed by single pulse stress released by a seismic event. 40Ar-39Ar dating of K-feldspar cement revealed a middle Triassic age (240.3 ± 0.4 Ma) for this event. The influx into the fault zone of an aqueous CO2-bearing fluid triggered the sudden fault movement. The high percentage of open space in the breccia fractures with cavities up 3 m × 3 m × 4 m in size, fluid inclusion microthermometry, and trace element chemistry of quartz suggests that the breccia was formed at depths between 4 and 0.5 km (1.1 to 0.1 kbar). The origin of the breccia-cementing, CO2-bearing Na-HCO3-SO4 fluid may have been predominantly of metamorphic origin due to decarbonation reactions (T > 200 °C) of limestones of the underlying Olden Nappe. The decarbonation reactions were initiated by deeply derived, hot fluids channelled to sub-surface levels by a major fault zone, implying that the breccia is situated on a deep-seated structure. Regionally, the Berglia-Glassberget occurs at a supposed triple junction of long-lived fault zones belonging to the Møre-Trøndelag, Lærdal-Gjende and the Kollstraumen fault complexes. These fault systems and the associated Berglia-Glassberget earthquake are the expression of rifting and faulting in northern Europe during the middle/late Triassic.