泛滥平原沉积物标准物质研制

泛滥平原沉积物能代表流域内元素的平均分布规律并具有普遍的适用性,是地球化学填图工作的重要介质。目前国际上尚无泛滥平原沉积物标准物质,国外相似标准物质的研制注重于环境方面,定值成分较少;我国同类的土壤和水系沉积物标准物质受限于不同工作需要,研制目的各不相同,且多数标准物质不足。为满足需求,本文研制了长江流域、赣江流域、汉水流域、淮河流域、黄河流域、海河流域、黑龙江流域共7个泛滥平原沉积物国家一级标准物质(编号为GBW07385～GBW07391)。此系列标准物质采用X射线荧光光谱压片法测试了26种成分,主量成分的RSD小于1%,微量元素的RSD约为2%,所有成分的RSD均小于7%,方差检验的F值均小于临界值F0. 05(24,25)=1. 96,表明样品的均匀性良好。在23个月的考察期内,检验的24种成分未发现统计学意义的明显变化,证明样品的稳定性良好。由全国13家实验室采用不同原理的、可靠的多种分析方法共同完成了73种元素和化合物共511个特性成分的定值测试,除GBW07386和GBW07388的CO2未能赋值外,其余494个特性成分给出了认定值与不确定度,15个特性成分给出了参考值,是我国同类标准物质定值最为齐全的一个系列。该系列标准物质代表了各自流域元素的背景含量,适用于多目标地球化学调查、土地质量地球化学调查等样品的分析质量监控,亦可用作环境、农业等领域相关样品测试的量值和质量监控标准。     

用于铂族元素分析的中外地质标准物质

标准物质作为地质分析的计量标准,在分析质量监控、仪器校准、方法评价和仲裁分析中发挥着重要作用。铂族元素分析一直是地质材料分析中最棘手的任务之一,铂族元素标准物质研制困难,数量少,严重影响了对铂族元素分析方法的评价和分析数据的质量监控,成为铂族金属矿产资源勘查、评价和相关研究工作的瓶颈。收集了中国及国际上现有的34个铂族元素标准物质和52个其他地球化学标准物质中的101个铂族元素定值数据。为便于使用也收集了这些标准物质中其他元素的含量信息,给出了铂族各元素按含量大小排列的信息简表以方便选择。充分利用这些标准物质对促进铂族元素分析方法研究,保证铂族元素分析数据质量,提高中国和世界铂族金属矿产资源勘查、评价及研究水平具有重要意义。     

鄂尔多斯盆地北缘地球化学大数据样本优选分析

众所周知,地球化学数据携带有众多地质噪音,这些噪音严重影响地球化学数据信息的客观性与可靠性;对于地球化学大数据融合分析而言,确定样品的有效性及变量优选是滤除地质噪音、建立最优样本集合的必要性工作,因而在地球化学大数据处理分析前需首先进行大样本优选,从而更加客观、真实的揭示地球化学大数据信息及相关地质意义。本文以鄂尔多斯盆地北缘1∶20万地球化学土壤测量数据为例,考虑元素之间的地球化学亲和力与组合匹配关系,建立非线性大样本优选模型。具体做法是基于优选后的样品矩阵,将39个元素变量分解成若干独立因子向量,将最优独立因子向量作为元素组合,其向量各分量作为元素变量的权重,依权重大小进行变量优选;优选后的样本集合可以作为该区地球化学数据分析与信息识别的有效地学信息集合,运用这种集合可以有效开展鄂尔多斯盆地外围铀地球化学分析,并为盆地铀资源预测奠定基础。     

我国主要覆盖区土壤地球化学标准物质的研制

覆盖区1∶25万多目标地球化学调查作为我国新一轮地质大调查的重要组成部分正在全国逐步展开.研制的覆盖区7个土壤系列地球化学标准物质,主要用作该地球化学调查样品分析的量值和质量监控标准.由全国14个水平较高的研究院所和中心实验室参加测试,采用16种不同原理的方法分析,共取得了5200多个平均值数据,定值了72种元素和成分,定为标准值的计65种元素和成分.多数元素定值的相对不确定度<5%.     

从数据统计学处理谈标样的组织与管理

研制天然物质化学成分的标准样品是现代地球化学工作的重要内容之一。据1984年K.Govindaraju报导,目前国际上已有170多种岩石和矿物标准样品,其中有我国的8个水系沉积物和2个超基性岩标样。这些标准样品在验证大量地质样品分析数据的可靠性,仪器校正、考核新技术新方法以及为进行实验室间以至国际间的地质样品数据对比等方面,起着十分重要的作用。     

关注地质分析文献,了解分析技术发展——地质分析技术应用类评述论文评介

地质分析技术产生的数据是进行地质科学研究和矿产资源、地质环境评价的重要基础,是发展国土资源地质调查事业和地球科学的重要技术支撑。中国地质事业已经得到了空前的发展,地质分析文献迅速增加,迫切需要对文献进行整理、加工、综合、评价。为了解当前中国地质分析技术在各领域的应用状况和获得的成果,对国内科研人员20年来发表的地质分析应用类评述性论文作一评介,内容联系当今全球地质分析技术发展的新趋势,主要包括标准物质与标准方法,岩石矿物分析,地球化学调查（区域地球化学、多目标地球化学和生态地球化学调查）、地球化学填图样品分析,海洋地质样品分析,现场分析,贵金属分析,化学物相与元素形态分析,水分析,能源矿产和环境样品分析,稳定同位素和同位素地质年代学技术与应用10项分析技术领域取得的研究成果。阐述了国内地质分析技术新应用领域的进展、动态和发展前景。     

地球化学标准物质标准不确定度估算探讨

在用高精度分析方法经检验证明样品均匀知识性和稳定性良好的条件下，可以以定值测试的不确定度表示标准物质标准值的不确定度。在较全面分析了地球化学标准物质定值测试的误差后，提出以测试结果平均值的标准偏差算得A类不确定度、以定值方法间的偏倚估计B类不确定度，以两者的合成值作为地理化学标准物质不确定度的估计值，并用其试算了部分已有地球化学标准物质有代表性元素的不确定度，结果表明提出的不确定度估算方法是可信的。     

多接收电感耦合等离子体质谱法测定岩石和土壤等国家标准物质的硅同位素组成

随着分析方法的进步和分析精度的提高，硅(Si)同位素被越来越多地应用于地球化学、宇宙化学和环境化学研究中，可以用于示踪壳幔物质循环、俯冲流体的来源，以及制约月球和地外天体的起源与演化等。为确保不同类型样品中硅同位素测量的准确性和不同实验室间数据可以进行对比，需标定一系列标准物质的硅同位素组成。前人工作中已经标定一系列来自美国地质调查局(USGS)的标准物质的硅同位素，为硅同位素的研究奠定了坚实的基础。但由于这些标准物质已经售罄，今后继续开展硅同位素研究面临无标样可用的境况。为了能持续性地用高精度硅同位素数据对相关领域研究提供支持，急需对新的标准物质进行高精度的硅同位素的测量。本文采用氢氧化钠碱熔法消解样品，经化学纯化后，利用多接收电感耦合等离子体质谱法精确测量了30个国家标准物质的硅同位素组成，δ³⁰Si值测试精度优于0.08‰。这些标准物质包括11个火成岩、2个变质岩、2个沉积岩、6个河流和海洋沉积物以及9个土壤，SiO₂含量范围为32.69%～90.36%,覆盖了大部分自然样品的变化范围。在这些标准物质中，河流沉积物GBW07310具有最...     

区域地球化学异常分析GIS系统及其应用

在区域矿产资源评价中,地球化学找矿信息为成矿分析提供了成矿作用的直接信息.GIS为化探数据分析提供了非常好的数据库管理功能、提供了化探数据处理的数字化产品及制图功能及提供了数据挖掘的形象化图示可视化功能.GGCAS(GIS-Based Regional Geochemical Data Processing System)将GIS功能无缝地与化探数据处理结合起来的地球化学异常信息分析系统.它包括地球化学异常确定的基本方法、多变量异常相关分析、地球化学异常空间趋势结构地质统计分析,也包括面金属量、累乘组合异常的计算.系统实现了所算及所得,使得地球化学科学计算、GIS数据库管理、图形可视一体化.运用该系对全国环境地球化学数据进行分析.     

基于网络的地球化学样品分析管理和质量监控系统

目前地球化学样品分析管理和质量监控系统多为单机版程序。文章介绍基于.net framework 3.5、以Microsoft Visual Studio 2005为开发工具、以Microsoft SQL server 2005为数据库服务器、采用ADO数据库访问技术的地球化学样品分析管理和质量监控系统。系统包括基于C/S体系结构的地球化学样品分析管理与质量监控子系统和基于B/S体系结构的分析任务下载与分析结果上传Web子系统,在网络上实现从样品接收、重新编号、分配任务、数据上传到质量监控的所有功能。系统的核心功能是管理地球化学样品分析过程中的任务和数据,进行质量监控。程序调试的结果表明,数据传输和处理准确无误,各功能模块均达到设计要求。     

GGR Biennial Review: Reference Materials in Geoanalytical and Environmental Research – Review for 2008 and 2009

This review gives an overview of the literature on reference materials of geochemical and environmental interest for the two-year period 2008–2009. Reference materials play an increasingly important role in all fields of geoanalytical research. This is demonstrated by the large number of publications containing data on reference materials. Although many reference materials exist, there is still a great need for certified samples, so-called delta zero materials for stable isotopic work and homogeneous microanalytical reference materials. This review focuses on six topics: developments of certification processes of reference materials mainly postulated in ISO guidelines and the IAG protocol, new developments of the GeoReM database, investigations of powdered rock reference materials, Chinese reference materials published in Chinese journals, microanalytical reference materials and isotopic reference materials.     

GeoReM: A New Geochemical Database for Reference Materials and Isotopic Standards

We have developed a new database named GeoReM ( http://georem.mpch-mainz.gwdg.de ) for reference materials and isotopic standards of geochemical and mineralogical interest. Reference samples include rock powders originating from the USGS, GSJ, GIT-IWG, synthetic and natural reference glasses originating from NIST, USGS, MPI-DING, as well as mineral (e.g., 91500 zircon), isotopic (e.g., La Jolla, E&A, NIST SRM 981), river water and seawater reference materials. GeoReM is a relational database, which strongly follows the concept of the three EARTHCHEM databases. It contains published analytical and compilation values (major and trace element concentrations, radiogenic and stable isotope ratios), important metadata about the analytical values, such as uncertainty, uncertainty type, method and laboratory. Sample information and references are also included. Three different ways of interrogating the database are possible: (1) sample names or material types, (2) chemical criteria and (3) bibliography. Some typical applications are described. GeoReM currently (October 2005) contains more than 750 geological reference materials, 6000 individual sets of results and references to 650 publications.     

Reference Values Following ISO Guidelines for Frequently Requested Rock Reference Materials

We present new reference values for nineteen USGS, GSJ and GIT‐IWG rock reference materials that belong to the most accessed samples of the GeoReM database. The determination of the reference values and their uncertainties at the 95% confidence level follows as closely as possible ISO guidelines and the Certification Protocol of the International Association of Geoanalysts. We used analytical data obtained by the state‐of‐the‐art techniques published mainly in the last 20 years and available in GeoReM. The data are grouped into four categories of different levels of metrological confidence, starting with isotope dilution mass spectrometry as a primary method. Data quality was checked by careful investigation of analytical procedures and by the application of the Horwitz function. As a result, we assign a new and more reliable set of reference values and respective uncertainties for major, minor and a large group of trace elements of the nineteen investigated rock reference materials.     

An Automated Iridium-Strip Heater for LA-ICP-MS Bulk Analysis of Geological Samples

In this paper we describe a flux‐free fusion technique for the highly precise LA‐ICP‐MS bulk analysis of geological samples. For this purpose we have developed an automated iridium‐strip heater with temperature and melt time control. To optimise the homogeneity of the fused glasses and to reduce possible depletion of volatile elements during melting, we undertook experiments with basaltic rock and glass powders using different melting temperatures (1300–1700 °C) and melting times (5‐80 s). Major and trace element microanalysis was performed using EPMA and LA‐ICP‐MS. Homogeneous glasses were obtained for temperatures ≥ 1500 °C and melting times ≥ 10 s. High loss (20‐90%) of highly volatile elements (e.g., Cs, Ge, Sn, Pb) was observed for high melting temperatures (≥ 1600 °C) and long melting times (80 s). Standard melting conditions (1600 °C, 10 s) represent a compromise, as the glasses were homogeneous with respect to major and trace elements and, at the same time, were not depleted in elements with condensation temperatures (at a pressure of 10^?4 bar) higher than about 900 K (e.g., Zr, Hf, Ba, Sr, REE, U, Mo, Ni, Rb, Ga). Several international geological reference materials with SiO₂ ranging between 47% m/m and 59% m/m were prepared using our standard melting conditions (1600 °C, 10 s) and subsequently analysed by LA‐ICP‐MS. These samples also include the new Brazilian basaltic reference material BRP‐1. Matrix‐matched calibration of the LA‐ICP‐MS data was performed using the basaltic reference glasses KL2‐G, ML3B‐G, BCR‐2G and BHVO‐2G. Most analytical data agreed within uncertainty at the 95% confidence level with the GeoReM preferred values published in the GeoReM database for reference materials of geological and environmental interest. To demonstrate routine bulk LA‐ICP‐MS analyses of geochemical and cosmochemical samples using the whole rock fusion technique, we also present trace element data for ocean island basalts from Lanai (Hawaii) and of Martian meteorites.     

地球化学数据库及其应用概况

地学数据库已得到广泛应用。在整个地学数据库中,地球化学数据库占据着重要的地位。地球化学数据库可概括为固体矿产地球化学数据库、油气地球化学数据库、同位素地球化学数据库、农业生态环境地球化学数据库、地球化学分析数据库和标准物质数据库等6大类。分析论述了地球化学数据库的现状和应用情况,并指出了发展趋势。     

GEOCHEMICAL STANDARD REFERENCE SAMPLES GSD 9–12, GSS 1–8 AND GSR 1–6

The 18 Chinese geochemical standard reference samples GSD 9-12 (stream sediments), GSS 1-8 (soils) and GSR 1-6 (rocks) were prepared after GSD 1-8 (stream sediments) for even wider and increasing needs of geology, exploration geochemistry and geochemical analysis. Usable values of 41 trace, minor and major elements of the 18 samples were published in 1984. In the following two years, efforts were concentrated on the determination of other elements, most of which are more difficult to determine accurately and hence not many data were available in the literature. At the same time, additional data on the 41 elements already evaluated were also submitted. In all, 155 234 results were available along with the 35 284 analytical data submitted. The processing of samples, the examination of sample homogeneity, the plan of collaborative analysis of the samples, and the criteria for defining the recommended values are described. The recommended or reference values of the 72 constituents, to-gether with the 35 284 analytical data of the 18 samples are published in this paper.     

Determination of Reference Values for NIST SRM 610–617 Glasses Following ISO Guidelines

We present new reference values for the NIST SRM 610–617 glasses following ISO guidelines and the International Association of Geoanalysts’ protocol. Uncertainties at the 95% confidence level (CL) have been determined for bulk‐ and micro‐analytical purposes. In contrast to former compilation procedures, this approach delivers data that consider present‐day requirements of data quality. New analytical data and the nearly complete data set of the GeoReM database were used for this study. Data quality was checked by the application of the Horwitz function and by a careful investigation of analytical procedures. We have determined quantitatively possible element inhomogeneities using different test portion masses of 1, 0.1 and 0.02 μg. Although avoiding the rim region of the glass wafers, we found moderate inhomogeneities of several chalcophile/siderophile elements and gross inhomogeneities of Ni, Se, Pd and Pt at small test portion masses. The extent of inhomogeneity was included in the determination of uncertainties. While the new reference values agree with the NIST certified values with the one exception of Mn in SRM 610, they typically differ by as much as 10% from the Pearce et al. (1997) values in current use. In a few cases (P, S, Cl, Ta, Re) the discrepancies are even higher.     

Preparation and Characterisation of Two Geochemical Reference Materials: DG‐H (Granite) and AM‐H (Amphibolite) from the Himalayan Orogenic Belt

Two geochemical reference materials of Himalayan origin named DG‐H (a granite) and AM‐H (an amphibolite) prepared by the Wadia Institute of Himalayan Geology Dehradun are described. Both samples were collected from the NW Himachal Himalaya in India. With the participation of analysts from more than forty international laboratories, element determination data collected during the past 10 years for characterisation of the samples was processed to assign working values using statistical procedures in use for this purpose. Earlier work published on these samples is incorporated in the present communication making it an updated document. The typical chemical and petrological characteristics of these two samples may prove useful for method validation and calibration of analytical instruments used for analysing similar rock types, and for widening the analytical range of several analytical methods used for geochemical analysis.     

Sequential Inductively Coupled Plasma Determination Of Some Rare-Earth Elements in Five French Geostandards

Experimental data for eleven rare-earth elements (REE) obtained by inductively coupled plasma spectrometry (ICP) in five French geochemical reference standards (BE-N, BR, DR-N, GS-N and FK-N)are presented. The method is based on acid digestion of the sample and cation-exchange separation from matrix elements.
Together with these new determinations an updated compilation of these reference materials are presented. Good agreement between the present results and previously preferred and published values obtained by various analytical techniques is observed. The values obtained in the present work corroborate the validity of the outlined method.