δ98/95Mo values and Molybdenum Concentration Data for NIST SRM 610, 612 and 3134: Towards a Common Protocol for Reporting Mo Data

Molybdenum concentration and δ^98/95Mo values for NIST SRM 610 and 612 (solid glass), NIST SRM 3134 (lot 891307; liquid) and IAPSO seawater reference material are presented based on comparative measurements by MC‐ICP‐MS performed in laboratories at the Universities of Bern and Oxford. NIST SRM 3134 and NIST SRM 610 and 612 were found to have identical and homogeneous ⁹⁸Mo/⁹⁵Mo ratios at a test portion mass of 0.02 g. We suggest, therefore, that NIST SRM 3134 should be used as reference for the δ–Mo notation and to employ NIST SRM 610 or 612 as solid silicate secondary measurement standards, in the absence of an isotopically homogeneous solid geological reference material for Mo. The δ^98/95Mo_{JMC Bern} composition (Johnson Matthey ICP standard solution, lot 602332B as reference) of NIST SRM 3134 was 0.25 ± 0.09‰ (2s). Based on five new values, we determined more precisely the mean open ocean δ^98/95Mo_{SRM 3134} value of 2.09 ± 0.07‰, which equals the value of δ^98/95Mo_{JMC Bern} of 2.34 ± 0.07‰. We also refined the Mo concentration data for NIST SRM 610 to 412 ± 9 μg g^?1 (2s) and NIST SRM 612 to 6.4 ± 0.7 μg g^?1 by isotope dilution. We propose these concentration data as new working values, which allow for more accurate in situ Mo determination using laser ablation ICP‐MS or SIMS.     

GGR Biennial Critical Review: Analytical Developments Since 2010

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 thermal ionisation mass spectrometry, accelerator‐based methods and vibrational spectroscopy, are also presented in detail.     

Correlation and characterisation of individual glass shards from tephra deposits using trace element laser ablation ICP‐MS analyses: current status and future potential

Laser ablation inductively coupled plasma mass spectrometry (LA‐ICP‐MS) is a high spatial resolution analytical method which has been applied to the analysis of silicic tephras. With current instrumentation, around 30 trace elements can be determined from single glass shards as small as ～ 40 µm, separated from tephra deposits. As a result of element fractionation during the ablation process using a 266 nm laser, a relatively complex calibration strategy is required. Nonetheless, such a strategy gives analyses which are accurate (typically within ±5%) and have an analytical precision which varies from ～ ±2% at 100 ppm, to ～ ±15% at 1 ppm. Detection limits for elements used in correlation and discrimination studies are well below 1 ppm. Examples of the application of trace element analysis by LA‐ICP‐MS in tephra studies are presented from the USA, New Zealand and the Mediterranean. Improvements in instrumental sensitivity in recent years have the potential to lower detection limits and improve analytical precision, thus allowing the analysis of smaller glass shards from more distal tephras. Laser systems operating at shorter wavelengths (e.g. 193 nm) are now more widely available, and produce a much more controllable ablation in glasses than 266 nm lasers. Crater sizes of <10 µm are easily achieved, and at 193 nm many of the elemental fractionation issues which mar longer wavelengths are overcome. By coupling a short wavelength laser to a modern ICP‐MS it should be possible to determine the trace element composition of glass shards as small as 20 µm and, providing sample preparation issues can be overcome, the determination of the more abundant trace elements in glass shards as small as 10 µm is within instrumental capabilities. This will make it possible to chemically fingerprint tephra deposits which are far from their sources, and will greatly extend the range over which geochemical correlation of tephras can be undertaken. Copyright © 2007 John Wiley & Sons, Ltd.     

激光扫描深度数据配准方法的研究

在对最近对应点迭代方法研究的基础上,提出了数据格网化重组织策略和基于ICP的多级配准方案,在效率和精度上均取得了好的结果。     

激光扫描数据的多站配准方法

介绍了激光扫描数据多站配准的目的,详细阐述了固定球公共点转换法、ICP算法和测量设备绝对定位法的原理以及实现方法,并分析了3种方法的优缺点。对激光扫描仪数据处理以及逆向工程、曲面质量检测和虚拟现实等领域的相关问题具有一定参考。     

长江口沉积物全量硼的测定初探

利用ICP－AES测试方法准确测定长江口水下沉积物中的全量硼，对三种不同的样品消化方法进行了初步探索，我们认为HF－HCIO4－HNO3-H3PO4消化方法是可靠的理想的样品消化方法。     

基于八叉树与KD树索引的点云配准方法

针对点云配准算法中KD树多维查询效率较低的问题,提出一种基于八叉树和KD树多层索引结构的点云配准方法。首先为模型点云数据建立八叉树全局索引,然后在八叉树叶子结点构建局部数据的KD树索引。对传统的ICP点云配准算法进行改进,通过叶子结点的全局索引值快速定位局部点云数据块,利用局部KD树索引加快最近点的搜索,计算最近点时利用欧氏距离阈值、点对距离差值和法向量阈值剔除部分噪声点。实验表明,改进算法提高了点云配准的效率和精度。     

南秦岭枣木栏岩体LA-ICP-MS锆石U-Pb年龄、岩石地球化学特征及其地质意义

南秦岭地区印支期花岗质岩浆侵入活动频繁,出现了不同类型的花岗岩,高锶低钇花岗岩就是其中的一种,前人对其进行了广泛的研究,但仍有不同的认识。枣木栏岩体位于南秦岭光头山岩体群北部,为典型的印支期高锶低钇花岗岩,前人对其缺乏研究。本文在对其详细野外地质调查的基础上,进行了较系统的岩石学、岩石地球化学、LA-ICP-MS锆石U-Pb年代学研究,认为其主体为石英闪长岩,岩石中发育大量的暗色包体,低SiO_2(53.72%~62.21%),高镁(MgO:3.84%~7.19%),高Mg~#(65~70),属于准铝质高钾钙碱性岩石。岩石具有高Sr(402×10~(-6)~811×10~(-6))、低Y(5.91×10~(-6)~12.7×10~(-6),18×10~(-6))和重稀土,Yb含量为0.58×10~(-6)~1.22×10~(-6),1.8×10~(-6)),高Sr/Y比值(35~94)的高锶低钇中酸性岩(Adakite)的典型地球化学特征。LA-ICP-MS锆石U-Pb年龄为199±3Ma(MSWD=4.3),限定枣木栏岩体的形成时代为晚三叠世晚期—早侏罗世早期。结合区域地质资料,认为其应该是主碰撞造山后期,地壳加厚背景下形成的具有高锶低钇属性的壳幔混合花岗岩。同时表明南秦岭地区在200Ma左右,仍为后碰撞构造环境,为区域构造演化提供了信息。     

Metal Distribution in Different Size Fractions of Natural Organic Matter

In this paper, size‐exclusion chromatography (SEC) was used to determine the metal concentration in different size fractions of a bog lake water. Two methods were applied: (a) preparative SEC with off‐line metal concentration analysis and (b) direct coupling of an analytical SEC system on‐line with an inductively‐coupled plasma mass spectrometer (ICP‐MS). In the preparative SEC measurements, maximum concentrations were found for different metal ions in different size fractions of the natural organic matter (NOM). Normalization of metal concentrations to dissolved organic carbon concentration (DOC) yielded two maxima in the high and in the very low molecular‐weight fractions. Whereas good recoveries were found for Al, Fe, and Ni, only 40% were obtained for Pb. This indicates that Pb formed labile complexes with NOM, and hence could strongly interact with the column material. In the experiments with the analytical SEC‐ICP‐MS system, the same trends were observed, but with even lower recoveries than in the preparative system. Sample preconcentration and storage were also investigated with respect to decrease in metal concentration. During the ultrafiltration preconcentration step Al and Fe were removed only to a small extent, whereas about half of the initial Pb was lost. This indicates that Al and Fe were mainly bound to high molecular‐weight fractions of NOM. In contrast to that, Al and in particular Fe were removed from solution more than proportionally with respect to DOC because of aggregation of the NOM during storage, whereas Pb and Ni were concentrated relative to the DOC.     

Assessment of Dissolution of Silicate Rock Reference Materials with Ammonium Bifluoride and Nitric Acid in a Microwave Oven

The complete dissolution of representative test portions of powdered rock samples for the determination of the mass fractions of trace elements by ICP‐MS relies either on aggressive and time‐consuming acid digestions or fusion/sintering with appropriate fluxes. Here, we evaluate a microwave oven dissolution method that employs a solution of NH₄HF₂ and HNO₃. The entire procedure occurs in a closed vessel system and takes up to 4 h. In hundreds of digestions, the precipitation of fluorides was never observed. Replicate decomposition of 100 mg of twenty‐one international reference materials (RMs) of igneous rocks, and also one of a shale presented mostly satisfactory recoveries of forty‐one trace elements. Important exceptions were Zr and Hf in G‐2 and GSP‐2 (mean recoveries of ca. 70%), although for four other felsic rock RMs, the digestion was complete. For ultramafic rock RMs, we present Cr results that indicate quantitative dissolution of Cr‐bearing phases. We discuss the findings and conclude that advances in sample preparation of geological materials for instrumental analysis would benefit from a better understanding of how specific characteristics, such as composition and crystallinity of certain minerals, may affect their reactivity.