Comparison of Two Sample Preparation Methods for X‐Ray Fluorescence Spectrometry in the Determination of Ni and Cr     

Surendra P. Verma  Rosalinda González‐Ramírez  Rodolfo Rodríguez‐Ríos 《Geostandards and Geoanalytical Research》2011,35(2):183-192

Pressed powder pellets and fused beads or glass disks are routinely used in X‐ray fluorescence spectrometry for the determination of major and trace elements, respectively, in geological materials. In order to evaluate the performance of these two sample preparation methods, we determined Ni and Cr concentrations of fourteen RMs from Japan, France and South Africa, and eighty‐five igneous and three sedimentary rock samples from Mexico in both powder pellets and glass beads. We also computed new values of statistical parameters for RMs from an outlier‐based multiple‐test method and compared them with the literature mean and confidence limit values. The results showed that the multiple‐test method provided more reliable central tendency and dispersion parameters for RMs than those obtained previously from the two or three standard deviation method, or from robust methods. The powder pellet and fused bead sample preparation methods provided consistent results for Ni and Cr at concentration levels > 50 μg g^?1 in this application; for lower concentration levels, however, these methods showed somewhat greater differences. For quantitative comparisons, both ordinary and weighted least‐squares linear regression models were used to show that the two sample preparation methods provided generally unbiased results.  相似文献   

Precise Determination of Silicon Isotopes in Silicate Rock Reference Materials by MC‐ICP‐MS     

Thomas Zambardi  Franck Poitrasson 《Geostandards and Geoanalytical Research》2011,35(1):89-99

A HF‐free sample preparation method was used to purify silicon in twelve geological RMs. Silicon isotope compositions were determined using a Neptune instrument multi‐collector‐ICP‐MS in high‐resolution mode, which allowed separation of the silicon isotope plateaus from their interferences. A 1 μg g^‐1 Mg spike was added to each sample and standard solution for online mass bias drift correction. δ³⁰Si and δ²⁹Si values are expressed in per mil (‰), relative to the NIST SRM 8546 (NBS‐28) international isotopic RM. The total variation of δ³⁰Si in the geological reference samples analysed in this study ranged from ‐0.13‰ to ‐0.29‰. Comparison with δ²⁹Si values shows that these isotopic fractionations were mass dependent. IRMM‐17 yielded a δ³⁰Si value of ‐1.41 ± 0.07‰ (2s, n = 12) in agreement with previous data. The long‐term reproducibility for natural samples obtained on BHVO‐2 yielded δ³⁰Si = ‐0.27 ± 0.08‰ (2s, n = 42) on a 12 month time scale. An in‐house Si reference sample was produced to check for the long‐term reproducibility of a mono‐elemental sample solution; this yielded a comparable uncertainty of ± 0.07‰ (2s, n = 24) over 5 months.  相似文献   

Iron Isotopic Compositions of Geological Reference Materials and Chondrites   总被引：2，自引：0，他引：2  

Paul R. Craddock  Nicolas Dauphas 《Geostandards and Geoanalytical Research》2011,35(1):101-123

High‐precision iron isotopic compositions for Fe‐bearing geological reference materials and chondrites with a wide range of matrices (e.g., silicates, oxides, organic‐bearing materials) are reported. This comprehensive data set should serve as a reference for iron isotopic studies across a range of geological and biological disciplines for both quality assurance and inter‐laboratory calibration. Where comparison is available, the iron isotopic compositions of most geological reference materials measured in this study were in agreement with previously published data within quoted uncertainties. Recommendations for the reporting of future iron isotopic data and associated uncertainties are also presented. Long‐term repeat analyses of all samples indicate that highly reproducible iron isotopic measurements are now obtainable (± 0.03‰ and ± 0.05‰ for δ⁵⁶Fe and δ⁵⁷Fe, respectively).  相似文献   

Oracle 10g拓扑数据模型自动建立方法研究     

韦波 《测绘科学》2007,32(2):102-104,171

本文在分析了Oracle 10g拓扑数据模型数据特点和拓扑编辑包优点及缺点的基础上,针对使用SQL语句上载数据,特别是上载复杂的拓扑关系信息数据需要人为处理而导致低效且容易出错的缺点,提出了基于矢量图基础上的模型自动建立方法,实现了模型数据的自动上载及模型的一次性建立,具有高效、快速和准确的特点。方法具有通用性,可在多种GIS软件平台下开发实现。  相似文献   

云南光茅山地区斑岩体地质特征及构造环境分析——来自主量元素地球化学方面的证据     

徐恒  ;崔银亮  ;荣惠锋  ;张苗红  ;梁庭祥 《矿产与地质》2014,(4):479-486

对云南光茅山地区斑岩体的岩石学和主量元素地球化学特征进行分析,研究区斑岩体的SiO2、Al2O3、Na2O和K2O的平均质量百分数分别为67.84%、15.39%、3.40%和4.37%,里特曼指数平均为2.40,固结指数和分异指数平均值分别为11.14和82.95。主量元素特征表明:其属SiO2过饱、过铝质和富碱高钾的钙碱性系列的斑岩体,属于造山期后A型花岗岩;其形成于喜山期陆陆碰撞接壤处的地壳消减带构造环境。研究区斑岩体在主量元素地球化学特征和成岩构造环境方面,不同程度的表现出与马厂箐斑岩体的相似性,具有寻找与马厂箐斑岩型矿床相同模式的铜、钼(金)多金属矿床的前景。  相似文献   

西藏果芒错蛇绿混杂岩中硅质岩的地球化学特征及其形成环境     

徐梦婧  李才  吴彦旺  解超明 《中国区域地质》2014,(7):1061-1066

果芒错蛇绿混杂岩位于狮泉河—永珠—嘉黎蛇绿混杂岩带中段,是该带中保存较好的一套蛇绿混杂岩,其形成环境是确定狮泉河—永珠—嘉黎蛇绿混杂岩带构造属性的重要依据。对果芒错蛇绿混杂岩中的硅质岩进行了地球化学分析,为判断蛇绿混杂岩的形成环境提供新的约束条件。硅质岩通常呈几十厘米夹层产于玄武岩中,含有大量晚三叠世—白垩纪放射虫化石。硅质岩SiO2含量为71.38%～77.67%,Al2O3含量为8.62%～11.51%,MnO/TiO2值为0.28～0.35,（Ce/Ce＊）SN值为0.92～0.94,（La/Ce）SN值为1.13～1.17,反映了陆源物质的影响,而V、Ni、Cu和V/Y值高于大陆边缘硅质岩,与洋中脊和大洋盆地硅质岩相似,说明果芒错硅质岩可能形成于受陆源物质影响且与大陆边缘有一定距离的环境中。结合变质橄榄岩、镁铁质岩墙和玄武岩的地球化学特征,初步认为果芒错蛇绿混杂岩的形成环境为靠近大陆边缘的弧后盆地。  相似文献   

New Chinese National Reference Materials for Hydrogen and Oxygen Isotopes in Water     

Lin Zhang  Fuliang Liu  Yankun Jia  Xiangyang Zhang 《Geostandards and Geoanalytical Research》2013,37(2):189-195

The Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences recently prepared four certified reference materials for hydrogen and oxygen stable isotopes in water, which are called ‘China Standard Water' (CSW)‐HO1–HO4 (hereafter referred to as HO1–HO4). These reference materials are intended for calibration purposes and provide reference values of their relative difference in ²H/¹H and ¹⁸O/¹⁶O isotope‐amount ratios expressed in delta notation, normalised to the VSMOW–SLAP scale. The certified values of the reference materials were determined by an interlaboratory comparison of results from eleven participating laboratories. This paper describes in detail the production and certification procedure of the four reference materials. The first analytical data for the reference materials are also provided using a variety of analytical techniques, namely CO₂–H₂O equilibration and laser spectroscopy for δ¹⁸O and Cr reduction, as well as H₂–H₂O equilibration, laser spectroscopy, and high‐temperature conversion for δ²H. The reference values for materials HO1–HO4 and their associated uncertainties are assigned.  相似文献   

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

Maria F. Gazulla  Marta Rodrigo  Monica Orduña  Carmen M. Gómez 《Geostandards and Geoanalytical Research》2012,36(2):201-217

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.  相似文献   

Calibration of the New Certified Reference Materials ERM‐AE633 and ERM‐AE647 for Copper and IRMM‐3702 for Zinc Isotope Amount Ratio Determinations     

Kirsten Moeller  Ronny Schoenberg  Rolf‐Birger Pedersen  Dominik Weiss  Shuofei Dong 《Geostandards and Geoanalytical Research》2012,36(2):177-199

The commonly used, but no longer available, reference materials NIST SRM 976 (Cu) and ‘JMC Lyon’ (Zn) were calibrated against the new reference materials ERM^®‐AE633, ERM^®‐AE647 (Cu) and IRMM‐3702 (Zn), certified for isotope amount ratios. This cross‐calibration of new with old reference materials provides a continuous and reliable comparability of already published with future Cu and Zn isotope data. The Cu isotope amount ratio of NIST SRM 976 yielded δ^65/63Cu values of ?0.01 ± 0.05‰ and ?0.21 ± 0.05‰ relative to ERM^®‐AE633 and ERM^®‐AE647, respectively, and a δ^66/64Zn_IRMM‐3702 value of ?0.29 ± 0.05‰ was determined for ‘JMC Lyon’. Furthermore, we separated Cu and Zn from five geological reference materials (BCR‐2, BHVO‐2, BIR‐1, AGV‐1 and G‐2) using a two‐step ion‐exchange chromatographic procedure. Possible isotope fractionation of Cu during chromatographic purification and introduction of resin‐ and/or matrix‐induced interferences were assessed by enriched ⁶⁵Cu isotope addition. Instrumental mass bias correction for the isotope ratio determinations by MC‐ICP‐MS was performed using calibrator‐sample bracketing with internal Ni doping for Cu and a double spike approach for Zn. Our results for the five geological reference materials were in very good agreement with literature data, confirming the accuracy and applicability of our analytical protocol.  相似文献   

Chemical Characterisation of Natural Ilmenite: A Possible New Reference Material     

Patrick H. Donohue  Antonio Simonetti  Clive R. Neal 《Geostandards and Geoanalytical Research》2012,36(1):61-73

Seven ilmenite (FeTiO₃) megacrysts derived from alnöite pipes (Island of Malaita, Solomon Islands) were characterised for their major and trace element compositions in relation to their potential use as secondary reference materials for in situ microanalysis. Abundances of thirteen trace elements obtained by laser ablation ICP‐MS analyses (using the NIST SRM 610 glass reference material) were compared with those determined by solution‐mode ICP‐MS measurements, and these indicated good agreement for most elements. The accuracy of the LA‐ICP‐MS protocol employed here was also assessed by repeated analysis of MPI‐DING international glass reference materials ML3B‐G and KL2‐G. Several of the Malaitan ilmenite megacrysts exhibited discrepancies between laser ablation and solution‐mode ICP‐MS analyses, primarily attributed to the presence of a titano‐magnetite exsolution phase (at the grain boundaries), which were incorporated solely in the solution‐mode runs. Element abundances obtained by LA‐ICP‐MS for three of the ilmenite megacrysts (CRN63E, CRN63H and CRN63K) investigated here had RSD (2s) values of < 20% and therefore can be considered as working values for reference purposes during routine LA‐ICP‐MS analyses of ilmenite.  相似文献