A Revisited Purification of Li for ‘Na Breakthrough’ and its Isotopic Determination by MC‐ICP‐MS     

Lin Xu  Chongguang Luo  Hanjie Wen 《Geostandards and Geoanalytical Research》2020,44(1):201-214

The accurate and precise determination of Li isotopic composition by MC‐ICP‐MS suffers from the poor performance of traditional column chromatography. Previously established chromatographic processes cannot completely remove Na in complex geological samples, which is currently interpreted to be a result of Na breakthrough. In this study, Na breakthrough during single‐column purification was found to differ between simply artificial Na‐containing sample solutions, where a little Na residue was found, and silicate rocks, where a large amount of breakthrough occurred. A revised two‐step column purification for Li using 0.5 and 0.3 mol l^?1 HCl as eluents was designed to remove the Na. This modified method achieves high‐efficiency Li purification from Na and consequently avoiding high Na/Li ratio interference for subsequent MC‐ICP‐MS analyses. The proposed method was validated by the analysis of a series of reference materials, including Li₂CO₃ (IRMM‐016, ‐0.10‰), basalt (BCR‐2: 2.68‰; BHVO‐2: 4.39‰), andesite (AGV‐2: 6.46‰; RGM‐2: 2.59‰), granodiorite (GSP‐2: ?0.87‰) and seawater (CASS‐5, 30.88‰). This work reports early Na appearance prior to the elution curves in chromatography and emphasises its influence for subsequent Li isotope measurement. Based on the findings, the established two‐step method would be more secure than single‐column chemistry for Li purification.  相似文献   

一种由粗到精的地面激光点云多层级配准方法     

王英  张云生 《测绘与空间地理信息》2020,(2):156-159

提出了一种综合利用快速点特征直方图(FPFH)描述符和同名点引导ICP优化的地面激光扫描(TLS)点云配准方法。该方法包括3个步骤:1)点云金字塔构建;2)基于FPFH的粗配准;3)同名点引导的ICP精配准。首先使用体素网格滤波器构造点云的金字塔结构,在粗配准时,FPFH描述符用于金字塔顶层上点云的鲁棒匹配,在此基础上,再进行两层级同名点引导的ICP精配准优化,使用3组典型TLS点云对进行实验,结果表明本文方法可以高效地完成TLS点云的配准。  相似文献   

Copper Isotopic Analysis in Geological and Biological Reference Materials by MC‐ICP‐MS     

Kaj Sullivan  Daniel Layton‐Matthews  Matthew Leybourne  James Kidder  Zoltn Mester  Lu Yang 《Geostandards and Geoanalytical Research》2020,44(2):349-362

The characterisation of relative copper isotope amount ratios (δ⁶⁵Cu) helps constrain a variety of geochemical processes occurring in the geosphere, biosphere and hydrosphere. The accurate and precise determination of δ⁶⁵Cu in matrix reference materials is crucial in the effort to validate measurement methods. With the goal of expanding the number and variety of available geological and biological materials, we have characterised the δ⁶⁵Cu values of ten reference materials by MC‐ICP‐MS using C‐SSBIN model for mass bias correction. SGR‐1b (Green River shale), DOLT‐5 (dogfish liver), DORM‐4 (fish protein), TORT‐3 (lobster hepatopancreas), MESS‐4 (marine sediment) and PACS‐3 (marine sediment) have for the first time been characterised for δ⁶⁵Cu. Additionally, four reference materials (with published δ⁶⁵Cu values) have been characterised: BHVO‐1 (Hawaiian basalt), BIR‐1 (Icelandic basalt), W‐2a (diabase) and Seronorm? Trace Elements Serum L‐1 (human serum). The reference materials measured in this study possess complex and varied matrices with copper mass fractions ranging from 1.2 µg g^?1 to 497 µg g^?1 and δ⁶⁵Cu values ranging from ?0.20‰ to 0.52‰ with a mean expanded uncertainty of ± 0.07‰ (U, k = 2), covering much of the natural copper isotope variability observed in the environment.  相似文献   

Chemical Procedures for Rhenium Extraction from Geological Samples: Optimising the Anion Resin Bead Clean‐up Step     

Gang Yang  Aaron Zimmerman  Nicole C. Hurtig  Svetoslav V. Georgiev  Vineet Goswami  Judith L. Hannah  Holly J. Stein 《Geostandards and Geoanalytical Research》2020,44(2):231-242

Rhenium–osmium geochronometry for samples with low Re and complex matrices requires improved Re extraction methods. Here, we investigate plausible controls on efficiency and efficacy of Re extraction during our anion resin bead purification. Four different protocols are compared, each isolating a single variable to test. Rhenium concentrations for solutions at each step of each protocol document differences in chemical recovery/yield. The negative‐thermal ionisation mass spectrometry (N‐TIMS) signal intensity serves as a proxy for Re yield and purity. These data document correlations between the N‐TIMS signal intensity and (a) the duration of anion resin bead conditioning prior to loading with Re‐bearing solution, and (b) both duration and strength of nitric acid used during rinsing of the Re‐loaded anion resin bead. The optimal protocol improved Re signal intensity around fourteen times compared with our current Re extraction protocol, an aggregate of 2.4 times improvement in chemical recovery (yield) and 5.8 times improvement in emission efficiency (purity). Repeated N‐TIMS isotopic measurements on our in‐house Re standard solution (1407) verify that our optimal protocol‐3 does not fractionate Re isotopes. The improved anion resin bead method considerably lowers the Re detection limit and allows Re‐Os isotopic analysis of picogram‐level Re hosted in geological samples with complex matrices.  相似文献   

The δ60/58Ni Values of Twenty‐Six Selected Geological Reference Materials     

Weihan Li  Jian‐Ming Zhu  Decan Tan  Guilin Han  Zhouqiao Zhao  Guangliang Wu 《Geostandards and Geoanalytical Research》2020,44(3):523-535

The high‐precision δ^60/58Ni values of twenty‐six geological reference materials, including igneous rocks, sedimentary rocks, stream sediments, soils and plants are reported. The δ^60/58Ni values of all samples were determined by double‐spike MC‐ICP‐MS (Nu Plasma III). Isotope standard solution (NIST SRM 986) and geological reference materials (BHVO‐2, BCR‐2, JP‐1, PCC‐1, etc.) were used to evaluate the measurement bias and intermediate precision over a period of six months. Our results show that the intermediate precision of Ni isotope determination was 0.05‰ (2s, n = 69) for spiked NIST SRM 986 and typically 0.06‰ for actual samples, and the δ^60/58Ni _{NIST SRM 986} values were in excellent agreement with previous studies. Eighteen high‐precision Ni isotope ratios of geological reference materials are first reported here, and their δ^60/58Ni values varied from ?0.27‰ to 0.52‰, with a mean of 0.13 ± 0.34‰ (2s, n = 18). Additionally, SGR‐1b (0.56 ± 0.04‰, 2s), GSS‐1 (?0.27 ± 0.06‰, 2s), GSS‐7 (?0.11 ± 0.01‰, 2s), GSD‐10 (0.46 ± 0.06‰, 2s) and GSB‐12 (0.52 ± 0.06‰, 2s) could potentially serve as candidate reference materials for Ni isotope fractionation and comparison of Ni isotopic compositions among different laboratories.  相似文献   

不同测站点云数据的配准算法     

高益忠 《北京测绘》2020,(2):180-184

随着三维激光扫描技术的发展,利用三维激光扫描仪采集信息,构建三维模型成为了热门的课题。由于受到观测环境、观测方向等影响,无法一次性地获得物体的所有的点云数据。因此,不同视角下点云数据的配准成为了三维建模中的关键技术,直接影响了最终的重合结果以及模型精度。本文着重研究主方向贴合法和最近点迭代算法(ICP算法),基于matlab平台编写算法,并对算法进行研究,得出配准结果以及配准精度。  相似文献   

Effect of different registration methods on precision of orientation based on RTK registration/georeferencing mode     

Shengming Hu  Zhijian Chen  Chenghui Wan  Chun Tang  Wen Xiong 《Marine Georesources & Geotechnology》2020,38(4):385-392

Abstract

Compared with traditional methods, the three-dimensional laser-scanning (3D-LS) technique can efficiently acquire many high-quality geometric properties of rock discontinuities. In practice, engineers usually prefer to simplify the processing by using single-station point data and roughly orienting owing to the complexity of registration/georeferencing multi-station point data. However, prior published studies have paid little attention to the accuracy and reliability when determining discontinuity orientations using 3D-LS. We propose a reliable and accurate method with robust on-site applicability. As part of an ongoing effort, we are evaluating the precision of the commonly used coarse registration method and the fine registration method, and promoted the optimized coarse- and fine-registration methods and evaluated their precision. It is found that: (1) the common and the optimized registration method can meet our project’s engineering requirements, and the optimized registration method improved accuracy in the dip direction by approximately 1°; (2) fine registration using an iterative closest point (ICP) algorithm can correct both dip direction and dip angle; and (3) the orientation is of high precision with commonly used coarse and fine registration, whereas the optimization effect to correct the orientation is slightly limited.  相似文献   

Development and Re‐Evaluation of Tourmaline Reference Materials for In Situ Measurement of Boron δ Values by Secondary Ion Mass Spectrometry     

Katharina Marger  Matthieu Harlaux  Andrea Rielli  Lukas P. Baumgartner  Andrea Dini  Barbara L. Dutrow  Anne‐Sophie Bouvier 《Geostandards and Geoanalytical Research》2020,44(3):593-615

Six tourmaline samples were investigated as potential reference materials (RMs) for boron isotope measurement by secondary ion mass spectrometry (SIMS). The tourmaline samples are chemically homogeneous and cover a compositional range of tourmaline supergroup minerals (primarily Fe, Mg and Li end‐members). Additionally, they have homogeneous boron delta values with intermediate precision values during SIMS analyses of less than 0.6‰ (2s). These samples were compared with four established tourmaline RMs, that is, schorl IAEA‐B‐4 and three Harvard tourmalines (schorl HS#112566, dravite HS#108796 and elbaite HS#98144). They were re‐evaluated for their major element and boron delta values using the same measurement procedure as the new tourmaline samples investigated. A discrepancy of about 1.5‰ in δ¹¹B was found between the previously published reference values for established RMs and the values determined in this study. Significant instrumental mass fractionation (IMF) of up to 8‰ in δ¹¹B was observed for schorl–dravite–elbaite solid solutions during SIMS analysis. Using the new reference values determined in this study, the IMF of the ten tourmaline samples can be modelled by a linear combination of the chemical parameters FeO + MnO, SiO₂ and F. The new tourmaline RMs, together with the four established RMs, extend the boron isotope analysis of tourmaline towards the Mg‐ and Al‐rich compositional range. Consequently, the in situ boron isotope ratio of many natural tourmalines can now be determined with an uncertainty of less than 0.8‰ (2s).  相似文献   

Effect of the Dry Ashing Method on Cadmium Isotope Measurements in Soil and Plant Samples     

Wei‐Xin Lv  Hao‐Ming Yin  Meng‐Shu Liu  Fang Huang  Hui‐Min Yu 《Geostandards and Geoanalytical Research》2021,45(1):245-256

A dry ashing method is commonly used to remove organic material from samples prior to geochemical analysis. In the course of this study, the Cd isotope ratios of a series of soil and plant reference materials and samples were studied to evaluate the effect of the dry ashing method on measurement results of Cd isotope ratios. The samples were pre‐treated using the dry ashing method and high‐pressure bomb for comparison. The results show that the digestion using high‐pressure bombs did not lead to Cd loss, but using the dry ashing method would cause different proportions of Cd loss. The whole range of Cd isotope difference between two methods was from ?0.07‰ to 3.01‰. There was also an obvious difference in measured Cd isotope ratios from the same leaf sample pre‐treated independently by the dry ashing method, indicating that the amount of Cd loss and the effect on Cd isotope measurement during dry ashing is related to the properties of the samples. Therefore, dry ashing may not be appropriate for the removal of organic material in Cd isotope ratio measurement, especially for samples with high organic contents. The δ^114/110Cd values of reference materials NIST SRM 1573a and GSD‐30 are reported for the first time in this study.  相似文献   

应用电感耦合等离子体质谱/光谱法研究上扬子区新华磷块岩稀土元素特征及沉积学意义   总被引：2，自引：2，他引：0  

段凯波  王登红  何汉江  郑国栋  熊先孝  袁建国  贺宝宝  屈云燕 《岩矿测试》2015,34(2):261-267

新华磷矿床是我国重要的富集稀土元素的沉积型含稀土磷块岩矿床,本文利用电感耦合等离子体质谱/光谱法(ICP-MS/AES),辅以岩矿鉴定等分析技术,结合沉积学理论研究了新华磷块岩稀土元素地球化学特征及相关问题。结果表明,新华磷块岩稀土总量(∑REEs)较高,集中值介于800×10-6~1200×10-6,其组成属轻稀土+钇型,稀土元素主要以类质同象形式存在于胶磷矿中;新华磷块岩和昆阳磷块岩具相似的REEs配分曲线和明显铈负异常,δCe介于0.28~0.36,表明上扬子区南缘成磷环境为氧化条件,且为稳定的滨浅海被动大陆边缘沉积环境;但新华磷块岩与其上覆黑色岩系REEs配分曲线迥异,后者表现出不明显的铈、铕异常,说明黑色岩系主要形成于深海-半深海静水还原环境,从梅树村期早期至晚期经历了海平面升高的过程,地层层序整体显示向上变深的沉积相变,磷块岩和黑色岩系之间的接触面可能为三级层序甚至更小层序级别的界面。这些沉积学的认识揭示了上扬子区下寒武统层序地层学意义和海相沉积环境特征,对华南早寒武世生命大爆发和层序地层学深入研究提供了证据。  相似文献