Determination of Carbon,Hydrogen, Nitrogen and Sulfur in Geological Materials Using Elemental Analysers

This article describes a series of methods developed for the determination of total carbon (C_Total), organic carbon (C_org), hydrogen, nitrogen and sulfur. The following elemental analysers were used: LECO model RC‐412 for the determination of organic carbon, total carbon and hydrogen; LECO model CS‐200 for the determination of total carbon and sulfur; LECO model TN‐400 for the determination of nitrogen; and LECO model TruSpec CHNS for the determination of organic carbon, total carbon, hydrogen, nitrogen and sulfur. Uncertainty and limits of detection and quantification were calculated for each method, as well as the running costs to define the most effective instrument for each material and each analyte. Accuracy was checked by the application of the Sutarno–Steger test. Finally, a compilation of the results obtained in the determination of C_Total, C_org, H, N and S in forty‐nine reference materials is presented.     

Neodymium and Strontium Isotope Data for USGS Reference Materials BCR-1, BCR-2, BHVO-1, BHVO-2, AGV-1, AGV-2, GSP-1, GSP-2 and Eight MPI-DING Reference Glasses

We have measured ⁸⁷Sr/⁸⁶Sr and ¹⁴³ Nd/¹⁴⁴ Nd isotope ratios in different batches and aliquots of the new US Geological Survey (USGS) reference materials (RMs) BCR-2, BHVO-2, AGV-2 and GSP-2 and the original USGS RMs BCR-1, BHVO-1, AGV-1 and GSP-1 by thermal ionisation mass spectrometry. In addition, we also analysed the eight Max-Planck-Institut-Dingwell (MPI-DING) reference glasses. Nearly all isotope ratios obtained in the different aliquots and batches agree within uncertainty limits indicating excellent homogeneity of the USGS powders and the MPI-DING glasses. With the exception of GSP-2, the new USGS RMs are also indistinguishable from the ratios found in the original USGS RMs (⁸⁷Sr/⁸⁶Sr: 0.704960, 0.704958 (BCR-1, -2), 0.703436, 0.703435 (BHVO-1, -2), 0.703931, 0.703931 (AGV-1, -2); ¹⁴³ Nd/¹⁴⁴ Nd: 0.512629, 0.512633 (BCR-1, -2), 0.512957, 0.512957 (BHVO-1, -2); 0.512758, 0.512755 (AGV-1, -2)). This means that for normalisation purposes in Sr and Nd isotope geochemistry BCR-2, BHVO-2 and AGV-2 can well replace BCR-1, BHVO-1 and AGV-1 respectively.     

武汉老浦片工程逆作法钢格构柱施工技术

建筑逆作法施工中,钢格构柱的精确定位及垂直度控制是基础施工中的难点。武汉老浦片商业及住宅项目工程,设计制作出钢格构柱的导向架、定位架,方便快捷地完成钢格构柱的垂直度、定位调节。通过开挖后检测数据分析,采用本文所述方法施工,钢格构柱垂直度、定位均能满足设计要求,可有效降低施工成本。     

International Association of Geoanalysts'Protocol for the Certification of Geological and Environmental Reference Materials

This protocol has been developed by the International Association of Geoanalysts to demonstrate procedures for the certification of geological and environmental reference materials to comply to the fullest extent possible with recommendations of the International Organisation for Standardisation (ISO Guide 35). A practical approach is described on the assumption that certifications will be normally be based on collaborative analysis programmes in which participating laboratories are preselected on the basis of performance in a proficiency testing programme or on the basis of other criteria of merit.     

非预应力格构锚固机制与优化设计研究

非预应力格构锚固是集坡面生态防护、浅表层与深层加固于一体的新型边坡加固技术,但目前无论就其加固力学机制,还是工程设计计算方法而言,学术界尚未达成共识。在分析边坡开挖失稳破坏力学过程与稳定性工况的基础上,依据应力扩散原理与Mohr-Coulomb强度理论,探讨了非预应力全长黏结格构锚固通过自主调动稳定区岩土体的力学强度来有效改善不稳定区边坡的受力状态和主动约束边坡不稳定变形持续发展的综合加固机制,包括双向挤密效应、锚拉效应、销钉效应、框箍效应与土拱效应;依照优化设计的基本原理与有关规范,构建了格构框架的优化设计数学模型与相关约束方程;利用Matlab7.0编写了该结构优化模型的自动寻优程序;通过在三峡库区某边坡治理工程中的应用,详细地介绍了其优化设计的计算过程;与基于工程类比法的原设计相比,可达到节省工程造价和优化设计结果的目的。     

The Preparation and Preliminary Characterisation of Three Synthetic Andesite Reference Glass Materials (ARM‐1, ARM‐2, ARM‐3) for In Situ Microanalysis

Three synthetic reference glasses were prepared by directly fusing and stirring 3.8 kg of high‐purity oxide powders to provide reference materials for microanalytical work. These glasses have andesitic major compositions and are doped with fifty‐four trace elements in nearly identical abundance (500, 50, 5 µg g^?1) using oxide powders or element solutions, and are named ARM‐1, 2 and 3, respectively. We further document that sector‐field (SF) ICP‐MS (Element 2 or Element XR) is capable of sweeping seventy‐seven isotopes (from ⁷Li to ²³⁸U, a total of sixty‐eight elements) in 1 s and, thus, is able to quantify up to sixty‐eight elements by laser sampling. Micro‐ and bulk analyses indicate that the glasses are homogeneous with respect to major and trace elements. This paper provides preliminary data for the ARM glasses using a variety of analytical techniques (EPMA, XRF, ICP‐OES, ICP‐MS, LA‐Q‐ICP‐MS and LA‐SF‐ICP‐MS) performed in ten laboratories. Discrepancies in the data of V, Cr, Ni and Tl exist, mainly caused by analytical limitations. Preliminary reference and information values for fifty‐six elements were calculated with uncertainties [2 relative standard error (RSE)] estimated in the range of 1–20%.     

低质量数元素同位素在线连续流同位素比值质谱分析的质量控制和数据标准化

同位素比值质谱分析方法是准确测量各种同位素相对丰度的标准方法。连续流同位素质谱的出现不仅提高运行效率,也降低了样品用量并提高灵敏度。但是,要使这种方法获得更好准确度和精度的同位素数据,并做到所获得数据可与其他实验室结果进行类比,从而得到可靠的同位素数据,这就需要好的分析策略和运行方案,还需要对仪器日常性能和数据质量进行严密的监视管控,而且还取决于原始数据如何进一步标准化到国际同位素尺度上。因此,同位素比值质谱结合元素分析仪(或热转换元素分析仪)连续流方法要实现可靠的稳定同位素分析需要:①设备安装和环境控制、测试准备、样品制备和称量、标准物质选择及序列等规范化质量控制措施;②严格校准仪器系统(包括调节灵敏度和线性,背景值监测,稳定性检测,H+3系数校正等);③可靠的数据处理。目前不同的实验室,采用标准物质来标定系统、对测量的同位素数据进行标准化,以及利用控制曲线来监测系统稳定性并对不确定度的计算,这些策略往往都不同。因此,统一的数据处理方案是被高度期待的。目前最好的执行方案是基于线性回归的两点或多点标准化方法。如果每一批样品中测量两个不同的标准物质四次,或者测量四个标准物质两次,那么不确定度会降低50%。当前同位素比值质谱能够测定同位素比值的不确定度一般要好于0.02‰。但是,标准物质的使用既要考虑样品的性质,同时要涵盖它们未知同位素组成的范围,尤其氢同位素在现阶段缺乏标准物质和测量的仪器精度较差(比碳、氮、氧等要低一个数量级)的情况下,这显然是稳定同位素分析者的一个重大挑战。本文概括了同位素比值质谱结合元素分析仪(或热转换元素分析仪)的基本操作原理和分析实践,将数据处理运用到同位素比值分析之中,获得连续流同位素比值质谱分析结果的合理准确度和精度。     

苯乙烯型大孔树脂对海水中微量有机磷农药的吸附性能研究

为获得不含农药的当地海水在利用酶传感器监测海水有机磷农药时作为对照溶液使用,选用苯乙烯型大孔吸附树脂ASD5作为吸附剂,对含马拉硫磷和甲基对硫磷的海水样品进行动态吸附研究。发现该树脂较适合去除海水中的微量马拉硫磷,在温度10℃,流速0.5mL.min-1的条件下,10g树脂制成的吸附柱处理含500μg.L-1马拉硫磷的海水样品(乙酰胆碱酯酶活性抑制率为30.0%),出水的乙酰胆碱酯酶(AChE)活性抑制率仅为0.4%,而对海水自身的性质没有显著影响。结果表明:苯乙烯型大孔吸附树脂ASD5适合去除海水中的微量马拉硫磷,在海水有机磷农药的酶传感器监测中有很好的应用前景。     

关于2000中国大地坐标系的建议

简述了建议的我国新一代大地坐标系——2000中国大地坐标系的定义和实现,给出了参考椭球的定义常数和导出常数的计算公式及其常数值,以及椭球面及其外部的正常重力公式。     

重晶石矿石成分分析标准物质研制

研制了7个重晶石矿石成分分析标准物质。其中,GSO-1为铁矿型重晶石,GSO-2、GSO-3为萤石型重晶石,GSO-4、GSO-5为石英型重晶石,GSO-6为硫化物型重晶石,GSO-7为黏土型重晶石。样品采用陶瓷衬里的球磨机加工,加工后样品粒度达到-0.074 mm。采用X射线荧光光谱法检验了钡、铜、铅、锌、锆、铝、硅、铁和钙共9种元素的均匀性,并进行振动试验。8个实验室参加定值工作,提供了硫酸钡、氧化钡、三氧化硫和锶的7个标准值,全三氧化二铁的2个标准值,氟化钙的1个标准值及铜、铅、锌和水溶盐等标准值或参考值。2009年4月,7个样品已被国家质量监督检验检疫总局批准为国家一级标准物质,编号为GBW 07811~GBW 07817。