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.     

太阳系形成及演化研究方法

通过对陨石的研究,说明太阳系的形成与演化历史,包括太阳星云的凝聚过程、高温加热熔融事件和低温蚀变过程,陨石母体的热变质作用、熔融分异作用以及冲击变质作用等。对太阳星云的化学组成和同位素组成不均一性、前太阳物质的存在及其意义、太阳系形成和演化的同位素绝对年龄、间隔年龄以及宇宙射线暴露年龄等进行了讨论。结合太阳系形成和演化的研究,特别对电子探针、离子探针、透射电子显微镜以及拉曼光谱等微束分析技术在该领域的应用和相关问题进行了讨论。     

关于研制X射线荧光微分析标准物质的探讨

将经过高温处理的土壤样品进行反复研磨后，用于X射线荧光微分析标准物质的研制，当99％的粉末粒径≤30μm时，用仪器中子活化和同步辐射X射线荧光进行元素分布均匀性和最少取样量分析，结果表明24个元素的最少取样量可以降到约1mg。     

X射线荧光光谱微区分析在铜矿物类质同象鉴定中的应用

铜矿物种类繁多,赋存状态各异,成分复杂,由于共生矿物和伴生矿物的存在,增加了传统岩矿鉴定工作的难度。特别是铜矿物间存在的类质同象现象(黝铜矿和砷黝铜矿)和铜矿物与其他矿物间(磁黄铁矿和方黄铜矿)存在镜下光学特征相似的现象,应用偏光或反光显微镜难以给铜矿物准确定名。本文应用具有微区分析功能的X射线荧光光谱仪扫描铜矿物标本谱图,通过选择测量条件、测量方式和干扰校正模型(谱线重叠和基体效应)建立了类质同象物相的鉴定方法。该方法具有较高的精密度和准确度,对黄铜矿标本进行12次测定,S、Fe、Cu的相对标准偏差(RSD)分别为0.74%、0.86%、0.18%;对铜矿物标准样品进行单次测定,待测元素的测量结果与推荐值的相对误差均小于6%。该方法可准确甄别出黝铜矿与含银砷黝铜矿、磁黄铁矿与方黄铜矿;测量效率高,能够提供主量元素和主要伴生元素的二维或三维图像,直观地呈现矿物的分布情况,为铜矿物的准确定名和矿物的综合利用提供了有价值的信息。     

碎屑重矿物分析对内蒙古西乌旗早二叠世寿山沟组的物源指示及构造意义

碎屑重矿物由于相对比较稳定,蕴含重要的成因信息,对其进行电子探针成分分析,能够还原岩石形成的物源区和盆地构造背景。内蒙古西乌旗早二叠世寿山沟组一段主要由砂岩夹砾岩等组成,二段主要由粉砂岩、泥岩等组成。重矿物分析表明,寿山沟组一段和二段砂岩重矿物主要有锆石、尖晶石和石榴子石等,指示其物源区为岩浆岩和变质岩。重矿物电子探针成分分析结果显示,电气石成分指示其具贫锂花岗岩和变沉积岩物源,尖晶石成分指示其具岛弧和洋中脊玄武岩类物源,石榴子石成分指示其具高级变质基性岩源区。综合物源分析显示,寿山沟组主要来源于迪彦庙蛇绿岩、锡林浩特杂岩和本巴图组玄武岩等。结合区域地质对比,认为寿山沟组形成于弧后盆地,古亚洲洋在早二叠世时期尚未闭合。     

Provenance of iron,bauxite and clay deposits of the Carboniferous Benxi Formation in southern margin of North China Craton: An example from Da'an bauxite and clay deposit of Sanmenxia area,Henan Province

During the Middle Ordovician to Late Carboniferous period,the North China Craton(NCC)was exposed and experienced prolonged weathering that resulted in the formation of large-scale iron,clay and bauxite deposits. The source of ore-forming material has always been a research focus,in particular,whether the sources of the iron ore and the Fe-bearing clay at the bottom of Benxi Formation are the same as the upper bauxite and clay deposit is still unclear. In this study,the Da'an bauxite and clay deposit at the southern margin of the NCC was chosen to carry out a detailed analysis of the micro-region mineral composition and elemental geochemical characteristics for further exploring the sources of iron,bauxite and clay deposits. The composition of the ore-bearing rocks in the Da'an bauxite deposit from the bottom to top includes Fe-bearing clay(locally iron ore),bauxite,and bauxitic clay;locally,in karstic uplift,bauxitic clay layer is directly overlying on the Fe-bearing clay. The Fe-bearing clay is dominated by siderite,pyrite,and illite in the karstic depression,and hematite,illite,and kaolinite in the uplift. Bauxite is mainly composed of diaspore,illite,and anatase,while bauxitic clay is mainly composed of illite. Mineral microanalysis revealed the development of large amounts of moissanite and small amounts of natural silica,silicalite,and chromite at the bottom of bauxitic clay layer. Regional comparison and correlation reveal that the ophiolite in the Shangdan suture zone and Erlangping Group in the North Qinling orogenic belt(NQOB)likely provides source materials for bauxite and clay deposits. The obvious differences in immobile element ratios (e.g., Zr/TiO₂,Hf/TiO₂,Nb/TiO₂,Ta/TiO₂)between the bottom Fe-bearing clay layer and the upper bauxite and clay layer in Da'an deposit,revealing that they are from different sources. The bottom Fe-bearing clay and iron ore layers are the products of in-situ weathering of underlying carbonates,while the top bauxite and clay are allochthonous. The regional uplift of the NQOB during the Late Carboniferous period provided important ore-forming materials for the formation of the NCC bauxite and clay deposits.     

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%.     

Suitability of Mn‐ and Fe‐Rich Reference Materials for Microanalytical Research

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.     

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。