二次离子质谱微区原位牙形石氧同位素分析及其在古海表水温记录中的应用

利用生物成因磷灰石的氧同位素信息能够重建古海水温度,尤其是牙形石,结合其在生物地层学上的研究,它的数据解释具有明确的古环境意义。牙形石微小的个体一直是其精确地球化学分析的限制因素。作为对牙形石微区原位氧同位素测试方法的探索研究,本文利用Cameca IMS--1280 型二次离子质谱仪对牙形石进行了微区原位氧同位素组成测试,通过分析得到可靠的古表层海水温度 ( SST) 记录,表明从晚二叠世到早三叠世SST 存在明显的上升过程。相比常规Ag3PO4 实验方法,牙形石微区原位氧同位素分析方法更加快速,而且能够有效避免牙形石易受到污染的部位,获得更为可靠的牙形石氧同位素组成的测定结果。     

紫金山金铜矿二元铜硫化物成分特点的初步研究

文章在电子显微成分分析的基础上,结合XRD、振动光谱等研究手段,对高硫型浅成热液形成的紫金山金铜矿床中铜硫化物的成分、物相特点进行了研究.首次在该区找到了久辉铜矿(Cu1.97S)、雅硫铜矿(Cu1.25S)等铜硫二元组分系列矿物,并发现了铜蓝被蓝辉铜矿明显交代的现象,进而推断它们基本上是同期形成的,但其所处的氧化-还...     

Microstructural characterization of firn

In this paper, we use a scanning electron microscope (SEM) coupled with X‐ray spectroscopy and electron back‐scattered diffraction patterns to examine firn in cores retrieved by the United States International Trans‐Antarctic Scientific Expedition. From grain boundary grooves we were able to see where the previously existing snow crystals were joined, and can determine grain sizes. From the SEM images, the porosity and the surface area per unit volume of the pores were measured. Finally, we have shown that we can determine the microchemistry of impurities in firn and demonstrated that we can determine the orientations of the firn crystals. Copyright © 2007 John Wiley & Sons, Ltd.     

Disproportionation of Fe<Superscript>2+</Superscript> in Al-free silicate perovskite in the laser heated diamond anvil cell as recorded by electron probe microanalysis of oxygen

Experimental evidence is reported for Fe²⁺ disproportionation in Al-free perovskite (Pv), when submitted to large temperature gradients (i.e., under off-equilibrium conditions) in a laser heated diamond anvil cell (LHDAC). To enable this effect, the experimental procedure was designed to produce large radial and axial temperature gradients. In the Pv and ferropericlase (Fp) assemblage synthesized after dissociation of natural olivine, the three chemical states of iron (i.e., Fe⁰, Fe²⁺ and Fe³⁺) could be evidenced by electron probe microanalysis (EPMA), through variations of oxygen contents attached to the Fe cations. Despite inherent difficulties for determination of O-contents and Fe³⁺/ΣFe ratios using EPMA, we recorded significant changes in iron oxidation state across the laser-heated strip. These changes are correlated with variations in composition for the major elements (Fe, Mg, and Si), which evidences that the Pv/Fp assemblage experienced large segregation under the strong temperature gradients. Grains of metallic iron were detected in parts of the laser-heated strip coexisting with a Pv phase with Fe/(Mg + Fe) = 6 at% and most of its iron as Fe³⁺. This Fe²⁺-disproportionation reaction involves insertion of Fe³⁺-defects in the Pv lattice. This Fe³⁺-bearing Pv phase is presumably unstable and decomposes into a mineral assemblage including magnesioferrite, which is detected at the border of the laser-heated strip.     

水体悬浮颗粒物的扫描电镜与X射线能谱显微分析

通过对湖州地区74个土壤样品多环芳烃含量的测定,分析了湖州市不同土地利用类型土壤中多环芳烃(PAHs)的含量特征及污染水平。结果表明,湖州地区PAHs各组分的含量均有检出,各种土地利用类型表层土壤均受到一定程度的PAHs污染,但均小于荷兰土壤修复标准;湖州市区耕地中PAHs的含量最高;从PAHs低环/高环比值小于1以及芘/苯并(a)芘比值小于2,反映了湖州地区土壤中PAHs主要是由燃煤和生活污染产生的。     

Preparation of a Synthetic Titanite Glass Calibration Material for In Situ Microanalysis by Direct Fusion in Graphite Electrodes: A Preliminary Characterisation by EPMA and LA-ICP-MS

This paper describes a technique for the preparation of a titanite (CaTiSiO₅) glass calibration material for use in in situ microanalysis of major, minor, and trace elements in geological materials. The starting composition was a titanite matrix doped with minor and trace elements at ∼ 200 μg g^-1. The elements Sc, Y, REEs, Th and U were added in the form of nitrates in solution, and the elements V, Cr, Mn, Fe, Co, Ni, Zr, Nb, Hf and W were added as solid oxides. The synthetic titanite glass was produced by direct fusion by resistance heating in graphite electrodes at 1600-1700 °C, and quenched in air. Backscattered electron images indicate good homogeneity, with no signs of separate phases or vesicles, and analysis of the major elements Ca, Ti and Si by electron microprobe showed relative standard deviations between 0.5 and 0.7%, based on six independent measurements. Deviations from nominal concentrations for Ca, Si and Ti were measured to -1.2, -3.3 and -0.8%, respectively. The homogeneity of the trace elements in the glass was assessed by LA-ICP-MS analyses, using NIST SRM 610, 612 and 616 as external calibrators, and Ca as the internal standard element. Determinations were made both with a quadrupole mass spectrometer and a sector field instrument, and both raster and spot modes of analysis were used. For the majority of doped elements, precision was better than 10%, and relative deviations from nominal values were, with few exceptions, between 5 and 10%.     

The Serra da Graciosa A-type Granites and Syenites, southern Brazil. Part 3: Magmatic evolution and post-magmatic breakdown of amphiboles of the alkaline association

Amphiboles are the main mafic minerals in most metaluminous to peralkaline alkali-feldspar granites and syenites, and they usually preserve an important record of the compositional evolution of the melts from which they crystallize. In the alkaline association of the Serra da Graciosa A-type Granites and Syenites (southern Brazil), amphibole compositions span a large range, including calcic, sodic–calcic, and sodic amphiboles. Calcic amphiboles are typically observed in the metaluminous rocks, while sodic amphiboles are characteristic of the more strongly peralkaline rocks; sodic–calcic amphiboles are found in intermediate varieties. Compositional variations record the differentiation trends within two petrographic series of the alkaline association. The overall evolution of amphibole compositions is similar in both: they reveal a progressive increase in Na and Fe³⁺ with differentiation (increase in alkalinity of the magmas), a characteristic shared by undersaturated peralkaline (or agpaitic) differentiation trends. In detail, however, the evolutions of the amphibole compositions in the two series are distinct. In Alkaline series 1, the cores of the crystals form a continuum from calcic to sodic compositions, with the exception of a small compositional gap within the sodic–calcic amphiboles. The rims, however, show compositions that diverge from this main trend; this divergence results from increasing amounts of the oxy-amphibole component, and reflects more oxidizing conditions at the final stages of magmatic crystallization. In Alkaline series 2, these oxidation trends are much more subtle and a reverse trend is observed in the sodic amphiboles. Sodic–calcic amphiboles are in several cases replaced by intergrowths of post-magmatic sodic amphibole and Al-poor (“tetrasilicic”) biotite.     

Combining CSD and isotopic microanalysis: Magma supply and mixing processes at Stromboli Volcano, Aeolian Islands, Italy

Integrating isotopic microanalysis with other analytical techniques creates powerful new methodologies for understanding the evolution of rock samples at the sub-grain scale. Here we present Crystal Size Distribution (CSD) data for a 26,000 year old sample from Stromboli Volcano and accompanying isotopic microanalysis of the phenocrysts. A technique, called the ICSD plot, is introduced which given stated assumptions allows the integration of both sets of data to generate timelines of isotopic evolution through the volcanic system. The combined approach is powerful, allowing investigation of the magma supply, mixing, crystallisation and contamination processes prior to eruption of a volcanic sample. For Stromboli Volcano, the combined analysis suggests that the change in magma type following a cone collapse took roughly five years to complete, similar to the timescale of changes seen in recent decades.     

Tephrological implications of beam size—sample‐size effects in electron microprobe analysis of glass shards

This paper concerns the potential consequences of varying procedures for the determination of tephra geochemistry by electron microprobe. Application of electron probe microanalysis to tephrostratigraphical methods has increasingly facilitated the resolution and refinement of Quaternary chronology associated with records of proxy‐environmental or proxy‐climatic change. The geographical range over which tephras are recovered has expanded significantly with the identification and analysis of crypto (or hidden) tephras in areas far removed from tephra sources. These tephras are dominated by glass shards, which, in many distal environments, may be either small in size (μm) or may be highly pumiceous with low glass:void ratios and thin (<10 μm) shard walls. We demonstrate that reducing the size of the electron beam used to analyse shard geochemistry cannot be used reliably to permit analysis of thin glass walls. This approach distorts the geochemical data, creating analytical differences that may generate inappropriate tephrogeochemical fingerprints. Additional distortion of the geochemical fingerprint in the form of hybrid analyses may be encountered in glass fragments containing micron‐sized crystalline phases such as feldspar. Copyright © 2001 John Wiley & Sons, Ltd.