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黑色页岩铁同位素标准物质的研制 总被引：1，自引：0，他引：1
本文选择宜昌三峡地区九龙湾剖面采集的黑色页岩作为黑色页岩Fe同位素备选标准物质, 命名为CAGS-BS。使用单因素方差分析法对CAGS-BS进行均匀性检验; 使用t检验对其在24个月中四次分析的数据进行长期稳定性的检验, 结果显示均匀性和稳定性良好, 满足标准物质的要求。黑色页岩Fe同位素标准物质采用多家实验室协作定值的方法确定特征量值。协作定值的单位包括: 中国地质科学院地质研究所, 中国科学技术大学, 中国地质大学(北京), 天津大学和中国科学院广州地球化学研究所。剔除了可疑值之后的数据符合正态分布, 可以采用算术平均法进行标准物质的定值。标准物质不确定度由协作测定的不确定度分量(uchar)、批内瓶间差异引起的不均匀性不确定度分量(ubb’)和实验室保存引起的长期不稳定性不确定度分量(ults)共同确定, 总不确定度为扩展不确定度, 包含因子(k)等于2。得到CAGS-BS的特征值及不确定度为: δ56FeIRMM-014/‰ = 0.10 ± 0.04。该标准物质可用于黑色页岩样品的化学流程评价和验证、质谱仪的校正及整个过程的分析质量控制。 相似文献
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贵州遵义和湖南张家界黑色岩系中的矿物组合非常复杂,用X射线衍射仪分析并结合前人的研究成果,显示其中的硫化物矿物、粘土矿物和有机质含量较高;经破碎和分选流程对样品进行处理后,用ICP-MS方法测定了黑色页岩和分选后样品中的铂族元素含量,对贵州遵义和湖南张家界黑色岩系中的铂族元素赋存特征进行研究,结果表明:贵州遵义和湖南张家界的黑色页岩系中赋存高含量的铂族元素,且含量表现较高的稳定性;低温氧化条件下,铂族元素的化学活动性足以使之以相当规模活化、迁移并在还原条件下沉淀富集;经强风化淋滤作用,富含碳硫钼矿黑色页岩中铂族各元素含量都有不同程度的降低;绝大部分的铂族元素富集于黑色页岩的有机质和黄铁矿中;铂族元素的分布模式具规律性,铂族元素的明显分异说明此黑色页岩的分布模式不具有地外物质的特征。 相似文献
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铌钽精矿标准物质研制 总被引：2，自引：2，他引：0
铌钽精矿标准物质在监控选冶样品分析的过程起到重要作用,在选厂及冶金系统有很大的需求,国内外的文献检索均未发现铌钽精矿标准物质的报道;而铌钽矿物的性质决定了铌钽精矿的粉碎粒度及均匀性对铌钽精矿标准物质的研制提出了更高的要求。本文阐述了4个铌钽精矿标准物质的研制过程,铌钽精矿采集于宜春及尼日利亚铌钽选厂,样品经气流粉碎和高铝球磨两次细碎及机械混匀后,随机抽取包装好的样品进行均匀性和稳定性检验及定值。采用电感耦合等离子体发射光谱法与质谱法(ICP-OES/MS)进行均匀性和稳定性检验,结果表明样品的均匀性和稳定性良好。采用多个实验室协同测试的定值方式,利用不同原理的分析方法对此样品的铌钽等12个元素进行定值,给出了各定值元素的认定值和不确定度。4个铌钽精矿标准物质Ta(Nb)_2O_5的含量为9. 89%、20. 55%、40. 79%、53. 69%,形成一个从粗精矿到精矿较为完整的含量体系,可以满足选冶试验各阶段流程样品分析对标准物质的需求。 相似文献
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铂族元素地球化学标准物质的研制 总被引：12，自引：3，他引：9
ＧＰｔ＿１～７系列标准物质由土壤、水系沉积物、富镁超基性岩、富铁超基性岩、含铜镍贫铂矿石及铬铁矿等不同类型７个样品组成。铂族元素的含量范围从土壤和岩石的背景含量到矿石达４～５个数量级。经方差检验样品均匀度良好。标准物质的定值分析采用了不同类型的试金和湿化学法分离富集,以原子吸收、催化比色、催化极谱、等离子体质谱、发射光谱和中子活化等方法进行测定。定值的元素为Ｐｔ、Ｐｄ、Ｏｓ、Ｒｕ、Ｉｒ、Ｒｈ６个铂族元素及Ａｕ。该系列标准物质主要适于作铂族元素地球化学勘查和铂矿勘查中铂族元素分析的量值标准与测试的质量监控。 相似文献
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用于铂族元素分析的中外地质标准物质 总被引：2，自引：2，他引：0
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。 相似文献
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中国与世界铂族元素地球化学标准物质评介 总被引：4，自引：0，他引：4
铂族元素分析一直是地质材料分析中最棘手的任务之一,是铂族金属矿产资源勘查、评价和相关研究工作的瓶颈。铂族元素标准物质作为铂族元素分析的计量标准,在分析质量监控、分析仪器校准、分析方法评价和仲裁分析中发挥着重要作用。笔者等评介了我国研制的超基性岩和铬铁矿铂族元素标准物质、铂族元素地球化学标准物质、铂族元素矿石标准物质和海山富钴结壳铂族元素标准物质共4个系列21个标准物质,也给出了其他地球化学标准物质中铂族元素的定值数据;并与南非、加拿大、俄罗斯和岩石矿物分析标准国际工作组(GIT-IWG)研制的13个铂族元素标准物质及其他国际地球化学标准物质中铂族元素的数据进行了对比。这些标准物质的研制与应用将大大提高铂族元素分析数据的可靠性,为我国和世界铂族金属矿产资源勘查、评价及研究提供了有力的技术支撑。 相似文献
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长江三角洲沉积物标准物质研制 总被引：3，自引：3，他引：0
美国、加拿大等国家先后研制了10余个海湾和河口沉积物标准物质,但定值成分较少,大多侧重于有机污染物和放射性核素值。我国于2007年研制了3个黄河三角洲沉积物标准物质,为进一步满足近海地球化学调查及资源勘探的需要,本文按照ISO导则35和国家一级标准物质技术规范,研制了2个长江三角洲沉积物标准物质。按照不同粒径采集两个候选物样品,样品经干燥、球磨至200目,采用电感耦合等离子体质谱和发射光谱法进行均匀性检验,结果表明F实测值小于列表临界值F0.05(24,25)=1.96,样品均匀性良好。在两年时间内采用X射线荧光光谱法进行了4次稳定性检验,未发现统计学意义上的明显变化,样品稳定性良好。由12家有技术权威的实验室共采用13种准确、可靠的分析方法进行协作定值,最终定值元素53项,涵盖了主量、微量及全部稀土元素,其中主量成分含量呈梯度分布,如Al2O3的含量分别为16.42%、11.48%。该系列标准物质定值元素种类多,定值方法准确,能够为河口三角洲地区地质及环境调查的分析测试工作提供可靠的质量保证。 相似文献
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Jean S. Kane Bombor Batjargal Dorj Erdenetsetseg 《Geostandards and Geoanalytical Research》2009,33(3):295-308
A report is presented on the recertification of two certified reference materials (CRMs) initially prepared and certified by the Central Geological Laboratory of Mongolia (CGL), namely serpentinite GAS and alkaline granite OShBO. Subsequent work done in collaboration with the International Association of Geoanalysts (IAG) followed the International Organisation for Standardisation (ISO) guidelines for certification (ISO Guide 35, 2006) more closely than had been possible originally. The certification protocol followed was that of the International Association of Geoanalysts (IAG). The recertification added to the number of elements that were certified for OShBO (from 21 to 30), but not for GAS (decreased from 15 to 12) because of the greater analytical difficulties posed by that sample matrix in meeting the more stringent metrological requirements for recertification. Further, the uncertainties for these values were established in accordance with the Guide to Measurement Uncertainty ; individual contributions of heterogeneity and bias are reported as appropriate for each of the certified constituents. Traceability of the certified values was demonstrated to the greatest possible extent, based on concurrent analyses of the matrix-matched existing CRMs, SW and GM, by all participating laboratories. The materials are now available from the CGL for use by laboratories in controlling data quality when analysing materials of similar matrices. 相似文献
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Jean S. Kane 《Geostandards and Geoanalytical Research》2004,28(1):53-80
The International Association of Geoanalysts (IAG) has certified a slate sample, OU-6, for twelve major and minor constituents, as well as thirty-five trace elements through an interlaboratory programme conducted in close compliance with the International Organization for Standardization (ISO) Guide 35 (1989). Laboratories were qualified for participation in the certification programme, based on their performance in the prior analysis of OU-6 as a proficiency test material. Thirty laboratories provided data for the certification, though not for each constituent that was certified. Certification criteria included a means of establishing traceability for the certification data, generally through concurrent analysis of the existing Geological Survey of Japan reference material JSl-1, agreement of results between laboratories and methods, and a minimum of data rejection (4% rejection rate for OU-6 data and 6% for JSl-1 data), preferably for well-understood technical reasons only. Information values are provided for an additional eight constituents where certification criteria were not met. Uncertainties developed in accordance with the "Guide on Uncertainty in Measurement" (Eurachem 2000) and representing the 95% confidence interval of the certified and information values are reported for all fifty five constituents. The material is currently available in 40 g units for distribution by the IAG. Supply is anticipated to last about ten years. 相似文献
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在分析地质标准物质标准值不确定度来源的基础上,提出了在多个实验室协作研制地质标准物质时,协作单位除提供重现性检测数据外,还应分别提供各项目检测数据的合成不确定度。分析方法或实验室之间的平均值的合成不确定度按不等精度方法处理。标准物质标准值的不确定度由分析方法、检测实验室、样品均匀性和样品稳定性的不确定度合成后乘以扩展不确定度置信水平下的包含因子而得。 相似文献
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Developments at ISO/REMCO and its Impact on the Production and Use of Geological Reference Materials
Angelique Botha 《Geostandards and Geoanalytical Research》2010,34(3):237-244
During the past decade the work of ISO/REMCO, the International Organization for Standardization’s Technical Committee on Reference Materials, was dedicated to achieving global harmonisation, and true involvement of the member countries. The first major accomplishment was the clarification of the terminology in the definitions for reference material and certified reference material, which were published as an amendment to ISO Guide 30 in 2008. The next milestone was the recognition that ISO Guide 34 (‘General requirements for the competence of reference material producers’) be used in conjunction with ISO/IEC 17025 for the accreditation of reference material producers. The third edition of ISO Guide 34 published in November 2009, clarifies the acceptable procedures for the certification of reference materials. This paper will discuss the role of ISO/REMCO in formalising the procedures for the accreditation of reference material producers and the evolution of the terms reference material and certified reference material. The paper will conclude with a case study, where a primary method in a single laboratory – one of the recognised acceptable metrologically valid procedures according to ISO Guide 34 – was used for the certification of reference materials. The reference materials are South African Reference Material SARM 2 (Syenite), SARM 3 (Lujavrite) and SARM 4 (Norite) from the suite of six NIMROCs that were originally certified by the Council for Mineral Technology (MINTEK) in South Africa in the 1970s. 相似文献
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Preparation and Certification of Re-Os Dating Reference Materials: Molybdenites HLP and JDC 总被引：27，自引：1，他引：27
Andao Du Shuqi Wu Dezhong Sun Shuxian Wang Wenjun Qu Richard Markey Holly Stain John Morgan Dmitry Malinovskiy 《Geostandards and Geoanalytical Research》2004,28(1):41-52
Two Re-Os dating reference material molybdenites were prepared. Molybdenite JDC and molybdenite HLP are from a carbonate vein-type molybdenum-(lead)-uranium deposit in the Jinduicheng-Huanglongpu area of Shaanxi province, China. The samples proved to be homogeneous, based on the coefficient of variation of analytical results and an analysis of variance test. The sampling weight was 0.1 g for JDC and 0.025 g for HLP. An isotope dilution method was used for the determination of Re and Os. Sample decomposition and pre-concentration of Re and Os prior to measurement were accomplished using a variety of methods: acid digestion, alkali fusion, ion exchange and solvent extraction. Negative thermal ionisation mass spectrometry and inductively coupled plasma-mass spectrometry were used for the determination of Re and 187 Os concentration and isotope ratios. The certified values include the contents of Re and Os and the model ages. For HLP, the Re content was 283.8 ± 6.2 μg g−1 , 187 Os was 659 ± 14 ng g−1 and the Re-Os model age was 221.4 ± 5.6 Ma. For JDC, the Re content was 17.39 ± 0.32 μg g−1 , 187 Os was 25.46 ± 0.60 ng g−1 and the Re-Os model age was 139.6 ± 3.8 Ma. Uncertainties for both certified reference materials are stated at the 95% level of confidence. Three laboratories (from three countries: PR. China, USA, Sweden) joined in the certification programme. These certified reference materials are primarily useful for Re-Os dating of molybdenite, sulfides, black shale, etc. 相似文献
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Reference materials (RM) are essential to achieve traceability of measurements. Specific uses of RM in analytical laboratories are the validation of methods, the calibration of instruments, the quality control and the demonstration of proficiency. This paper describes the certification of a new geochemical reference material, named BRP-1 (Basalt Ribeirão Preto), and acts as the certificate of analysis for this RM. The rock sample was crushed and pulverised at the USGS (Denver, USA), homogenised and split into 1920 bottles, with 55 g each. BRP-1 was transported back to Brazil and the homogeneity between and within bottles was assessed to demonstrate sufficient homogeneity for certification. The chemical characterisation was performed by twenty-five laboratories. Each laboratory received two bottles of BRP-1 and one of BCR-2 (Basalt Columbia River) used for quality control (QC). Reference values and uncertainties were calculated for forty-four constituents of BRP-1, following ISO Guide 35 recommendations and the IAG Protocol. The calculation of each reference value included data of proven traceability from at least ten laboratories using two or more analytical techniques and the uncertainties combines the characterisation and between bottle homogeneity contributions. 相似文献
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The International Organisation for Standardisation (ISO) has published many guides, or technical standards, of great value to analytical geochemists. Two of particular importance are Guide 33 (Uses of Certified Reference Materials) and Guide 35 (Certification of Reference Materials). Both were first developed in the 1980s and undergo regular review and updating by the Reference Materials Committee (REMCO) that operates within ISO. Recent revisions have focused on adding statistical rigour to both guides. Although this offers significant advantages for use by professional metrologists, there are consequent issues of comprehension by the analytical chemists who in fact have the greatest need of them. A major focus of Guide 35 is the development of reference material uncertainties that are in full compliance with the Guide on Measurement Uncertainty (GUM), jointly issued by ISO, IUPAC and others. Guide 35 details handling of uncertainty due to (1) degradation on the shelf and in transport, (2) sample heterogeneity and (3) inter‐method and inter‐laboratory bias, as well as within‐laboratory repeatability. The International Association of Geoanalysts has developed a protocol for reference material certification that applies Guide 35 to the specific needs of the geoanalytical community. The approach being taken by the IAG in developing GUM‐compliant uncertainties for its certified values is presented. Recommendations made in Guide 33 for how a laboratory should compare its own results with certified values in assessing laboratory accuracy are outlined. Additionally, the subject of misusing reference materials is discussed. The apparent misuse occurs because so few CRMs exist that meet critical measurement needs of geoanalytical laboratories and that also meet the rigorous metrological demands of the latest editions of the ISO Guides. All of the focus of the IAG certification programme has been to undertake certifications that would fill gaps in CRM availability and thus serve to limit this misuse. 相似文献
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Lev L. Petrov Yuri N. Kornakov Irina la. Korotaeva Elena A. Anchutina Luidmila A. Persikova Vera E. Susloparova Irina N. Fedorova Viktor A. Shibanov 《Geostandards and Geoanalytical Research》2004,28(1):89-102
This paper describes the creation of two new reference samples of black shale, SCHS-1 and SLg-1, collected in the Bodaibo Region of Irkutsk District (Siberia, Russia). These samples have been developed as State Standard Samples to meet the requirements of Russia's Normative Documents, so that they can be recognised by the Russian State Certification Agency and included on the State Register of certified reference materials. SCHS-1 was produced from shale of the Khomolkho suite; SLg-1 represents the average composition of the Sukhoy Log gold deposit (within Au mineralisation). The homogeneity was assessed by applying the concept of potential inhomogeneity, and the inhomogeneity uncertainties (σinhom ) for the indicator elements that were estimated experimentally by silicate XRF analysis. It was found that a majority of the indicator elements was characterised by σinhom /Δp < 1/8 (Δp is the permissible certification uncertainty), and so σinhom was neglected for the indicator elements and all other elements that were included in their respective group. The value of σinhom calculated for Fe (σinhom,Fe /Δp > 1 /8) was taken into consideration for the noble metals and their associated elements (e.g., Ag, As, Au, etc.). More than fifty laboratories (thirty-seven from Russia) were involved in the interlaboratory experiment (ILE) to analyse these reference samples. The data obtained from the ILE allowed SCHS-1 and SLg-1 to be certified for, fifty-one and forty-three elements, respectively, as State Standard Samples. 相似文献