鲤(Cyprinus carpio)仔鱼耳石锶(Sr)标记及其时滞特征的研究

本研究以确认鱼类早期个体规模化耳石锶(Sr)标记的可行性及其时滞特征为目的,选择鲤(Cyprinuscarpio)仔鱼为实验对象,开展了六水氯化锶(SrCl2.6H2O)溶液2d的活体浸泡标记研究。结果显示,该浸泡标记过程对鲤存活、生长无显著影响。利用X射线电子探针微区分析(EPMA)技术进行分析:定量线分析结果显示对照组Sr/Ca比值(3.0左右)趋于稳定,标记组却均出现了明显的标记峰值(远3.0);面分布分析结果表明在标记组鲤耳石上均呈现出一圈明显、清晰可见的红色"高Sr标记环"。此外,对比对照组和标记组微化学结果发现,"高Sr标记环"在恢复续养250d后的鲤耳石仍然可见,说明Sr标记可长期存在。观察鲤仔鱼耳石微结构,发现Sr在耳石上存在明显的时滞效应。首次得出在开始浸泡后的第3天,耳石上才开始出现Sr标记,在浸泡结束后的第6天,耳石Sr标记区才会完全消失的结论。本研究首次揭示出,外源Sr标记的方法在鲤仔鱼种群大规模增殖放流标记和评价中将具有很强的稳定性、可靠性、可行性和应用潜力。     

Single Particle Analysis of Aerosols, Observed in the Marine Boundary Layer during the Monterey Area Ship Tracks Experiment (MAST), with Respect to Cloud Droplet Formation

The chemical composition of individual particles >0.2 m sampled duringthe MAST-experiment wereanalysed by SEM-EDX, in combination with multivariatetechniques. The objective of this experiment was toidentify the mechanisms responsible for themodification of marine stratocumulus clouds byemissions from ships and in a wider sense to provideinformation on the global processes involved inatmospheric modification of cloud albedo. Aerosolswere examined under different MBL pollution levels(clean, intermediately polluted and moderatelypolluted) in five different reservoirs: backgroundbelow-cloud and above-cloud aerosol; background clouddroplet residual particles; below-cloud ship plumeaerosol and ship track cloud droplet residualparticles.In this study a relation was provided between theaerosol emitted from the ship's stack to an effect incloud. Additionally, a large fraction of the ambientaerosol was found to be composed of organic materialor other compounds, consisting of low Z-elements,associated with chlorine. Their number fraction waslargest in clean marine boundary layers, and decreasedwith increasing pollution levels. The fraction of`transformed sea salt' (Na, Cl, S), on the other hand,increased with the pollution level in the MBL. Only20% of the particles fell within the detectable rangeof the analysis.     

汉诺坝辉石岩包体中单斜辉石的微区微量元素组成特征及其地球动力学意义

本文对来自汉诺坝玄武岩中的三类辉石岩包体的单斜辉石（Cpx）利用LA—ICP—MS进行了原位微区微量元素分析研究。金云母单斜辉石岩中的单斜辉石具有低Cr,Co和Ni，高CaO、Zr、Hf、Ta和LREE特征，并且具有较低的Mg^#，反映金云母单斜辉石岩可能是经受了后期交代作用的地慢岩浆堆晶产物尖晶石二辉橄榄岩中的石榴辉石岩脉体中的Cpx具有高Na2O低CaO特征，其Ti、Zr、Hf、Y含量明显高于其它石榴辉石岩Cpx中的含量，反映了石榴辉石岩脉体可能是富Na硅酸盐熔体与地幔尖晶石二辉橄榄岩反应的成因，部分石榴辉石岩包体的Cpx具有特征的La富集或微量元素（如Zr、Hf、Ta、Li、P、REE等）环状对称分布特征，暗示华北克拉通北缘可能存在多期次地幔交代富集作用．通过对同一Cpx颗粒中的流体包裹体密集区和干净区域的对比研究，发现Cpx中的流体包襄体不仅富集LILE和LREE，而且HFSE中的Nb、Ta、Zr和P也具有明显的富集特征，LREE和HFSE未发生明显分异，这可能暗示地幔交代流体中含有少量的络阴离子（如F^-和Cl^-等）．     

硫化物矿物中痕量元素的激光剥蚀-电感耦合等离子体质谱微区分析进展

第一行过渡金属元素及痕量贵金属元素高度富集在硫化物矿物中,常形成具有工业意义的矿床,使得硫化物具有重大的经济价值。对天然硫化物矿物中的这些痕量金属元素丰度及其分布的研究,在矿石成因学、经济地质学、环境地球化学等领域具有重要的应用价值。激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)微区分析技术是一种强大的痕量元素分析工具,非常适合直接分析硫化物矿物中痕量元素的浓度及其空间分布。由于硫化物的激光剥蚀特性与硅酸盐及氧化物不同,分析校准用的标准物质又极度缺乏,严重阻碍了这一技术在硫化物矿物微区分析中的应用。本文评述了硫化物简介、硫化物中痕量金属元素分析的意义、LA-ICP-MS微区分析技术在硫化物矿物痕量元素分析中的优势及近年来的应用进展、硫化物分析中的干扰与校准、包含铂族元素及金的硫化物标准物质的研制进展及合成硫化物标准物质最有应用前景的方法。     

The sum of component concentrations as a quality indicator in X-ray electron probe microanalysis of minerals

X-ray electron probe microanalysis is a complete mineral analysis technique. Therefore, the sum of obtained concentrations can be used as an indicator of the quality of analysis. There are two kinds of errors of the sum of concentrations. The first is related to the deviation of the sum from the basic value and can be called a difference error. The second is the scattering of results around the mean value and can be called an averaging error. The difference error characterizes the reproducibility of the measurements and equals 0.41% at the current precision level. The averaging error characterizes the repeatability of the measurements and equals 0.23%. The difference error can be used as a quality indicator directly during analysis, while the averaging error can be used after analysis of a batch of specimens. According to the modified three-sigma rule, the acceptable sum values of separate analyses are in the range 98.8-100.8%. This range is obviously valid only for an ideal model with a basic sum value of 100%. In real analyses, the basic value deviates from 100% because of the presence of elements which are not detected in the analysis and elements with a variable valence. According to the three-sigma rule, the acceptable scattering of the sum of concentrations around the average value is ± 0.7%.     

BAM‐S005 Type A and B: New Silicate Reference Glasses for Microanalysis

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.     

激光剥蚀电感耦合等离子体质谱微区分析 进展评述

激光剥蚀电感耦合(LA-ICP-MS)等离子体以其高空间分辨率、高灵敏度、多元素同时测定并可提供同位素比值信息的检测能力在原位微区分析中已得到广泛应用。现从仪器的发展、基础研究等方面评述了近年来LA-ICP-MS微区分析的进展,重点介绍了与等离子体质谱(ICP-MS)联用的激光器(纳秒和飞秒激光器)的发展、校正方法、分馏效应及其在地球科学微量元素、同位素、包裹体分析中的应用。并简要地阐述了LA-ICP-MS分析技术存在的局限和发展趋势。     

磁铁矿中微量元素的激光剥蚀-电感耦合等离子体质谱分析方法探讨

微区原位分析提供了固体物质的元素及同位素组成的空间分布信息,有利于解决不同的地质问题、环境问题和工业方面的问题。磁铁矿中微量元素地球化学组成有助于研究成矿时的物理化学条件和示踪新的矿床。本文建立了利用激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)分析磁铁矿中微量元素的方法,探讨了选择必要的分析元素,选择合适的内标、外标,选择恰当的束斑大小等方法。以LA-ICP-MS分析澳大利亚Ernest Henry IOCG矿床磁铁矿中微量元素的方法为例,采用NIST SRM 610作为外标,Fe作为内标较为合理;正常情况下采用32~60 μm的激光束,但对于个别样品中磁铁矿颗粒较小,可以考虑使用较小的激光束(24 μm或16 μm);为消除质谱干扰,Ti选择测量⁴⁹Ti,Cu选择测量⁶⁵Cu,Sn选择测量¹¹⁸Sn。     

牙形石SHRIMP微区原位氧同位素分析方法

氧同位素温度计已被用于古温度变化研究多年。生物化石磷酸盐中的氧同位素组成对古气候环境变化响应灵敏,牙形石在古生代到中生代的古海洋地层中广泛存在,并具有较为重要的地层学意义,是研究古温度变化的最佳样品之一。SHRIMP具备高分辨、高灵敏、高精度和微量及原位微区分析的特点,可以进行20μm范围内的原位(in-situ)同位素分析。本文介绍了作者利用SHRIMP IIe-MC建立的牙形石微区原位氧同位素分析方法,这是国内关于该方法的首次报导。本文对磷灰石标准样Durango进行了测定,连续七昼夜获得的253次测定结果,平均值为δ18 Oapatite=9.78‰±0.29‰,与该标准参考值δ18 Oapatite=9.81‰±0.25‰(Williams,未刊资料)一致。作者并以二叠系—三叠系界线上下海水温度变化研究为示范,对采自西藏文布当桑二叠系—三叠系剖面上的49个层位中的237件牙形石样品进行了914个氧同位素分析,为研究二叠系—三叠系界线上发生的生物灭绝事件前后的海水温度变化提供了可靠详实的数据。     

铁氧化物型铜金矿中磁铁矿微量元素含量对结构参数影响的初步研究

磁铁矿是一种重要的铁氧化物,广泛分布于自然界的三大类岩石和各种不同类型的矿床中.采用激光剥蚀电感耦合等离子质谱仪,分析了澳大利亚Ernest Henry铁氧化物型铜金矿床中磁铁矿的微量元素含量,并用X衍射测定微量元素含量最高和最低时磁铁矿相应的晶胞参数,从而评价微量元素变化对磁铁矿结构参数的影响.结果表明,磁铁矿中存在着阳离子替代关系;微量元素含量高的磁铁矿晶胞参数a0值小于标准磁铁矿的a0值,含微量元素低的磁铁矿晶胞参数a0值则大于标准磁铁矿的a0值;磁铁矿中所含微量元素不同,其对应的晶胞参数a0值亦有明显变化.