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1.
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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Albina I. Kuznetsova Olga V. Zarubina Olga A. Sklyarova 《Geostandards and Geoanalytical Research》2007,31(3):251-259
Reference samples of soils from the Institute of Applied Physics, Irkutsk (RIAP), the Institute of Geochemistry, Irkutsk (IGI) and the United States Geological Survey, Reston (USGS) were analysed with the aim of determining Ag, B, Ge, Mo, Sn, Tl and W abundances by an atomic emission method with air-stabilised D.C. arc excitation. Two series of reference samples of soils and bottom sediments, GSS-1-8 and GSD-1-12 (IGGE), were used to ensure the traceability link for the analytical results. Traceability was also demonstrated through the comparison of measured results by AES and ICP-MS methods. It is shown that the reference samples GSS-1-8 and GSD-1-12 satisfied the "fitness-for-purpose" criterion (uncertainty U of the certified value should be one-third to one-tenth the magnitude of routine laboratory data uncertainty S (S/U > 3-10)) and can be applied for calibrating AES techniques. 相似文献
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One or two gram aliquots of twelve reference materials with low platinum-group element (PGE) abundances (Ir concentrations ranging from 30 to 510 pg g-1 ) were analysed by isotope dilution ICP-MS using an on-line chromatographic matrix separation after acid digestion in a high pressure asher (HPA-S) to determine the concentrations of Ru, Pd, Re, Ir and Pt. Osmium concentrations were determined via ID-ICP-MS but as volatile OsO4 , whereas Rh concentrations were calculated by comparing the peak areas of the chromatographic peak with that of a standard solution. Validation of the method was performed and the concepts of traceability and measurement uncertainty were applied to assure comparability. The reference materials BCR-2, BHVO-1, BHVO-2, BIR-1, DNC-1, EN026 10D-3, MAG-1, RGM-1, SCo-1, SDO-1, TDB-1 and W-2 were investigated to test for their usefulness for certification. The use of TDB-1 is highly recommended because it is homogeneous at the two gram level and many values based on several different analytical procedures have been published. It is recommended that our efforts should focus on the certification of this reference material to reduce the uncertainties of its currently certified values (Pd and Pt only) and to assign certified values to the other PGE and Re. It is necessary to have at least one well-characterised RM for validation of methods applied to the analysis of PGE and Re in low abundance samples, although the matrix of TDB-1 might not completely match those of many samples. 相似文献
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(Institute of Rock Mineral Analysis Ministry of geology mineral Resources Beijing 《岩矿测试》1995,14(2):114-161
研制了霓霞正长岩，粗面岩，花岗闪长岩，辉长石，流纹岩及白云岩６种不同类型的岩石标准物质，对用Ｘ射线荧光光谱均匀性检验实际取样量进行了探讨，选择分析测试方法时，除采用了标准方法和长期应用的分析方法外，还采用了近年发展起来的新技术新方法，在定值中应用了多参数统计定值模式，给出了６９个元素的标准值和参考值，该批标准物质于１９９１年１月经国家技术监督局审核批准为国家一级标准物质，编号分别为ＧＢＷ０７１０９ 相似文献
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手持式X射线荧光光谱仪在富钴结壳资源勘查中的应用 总被引：1，自引：1，他引：0
便携式X射线荧光光谱仪具有快速、无损分析的特点,本文重点研究了手持式X射线荧光光谱仪在富钴结壳碎块和浅钻岩心野外现场原位分析中的应用能力。采用压片法制样,以富钴结壳国家标准物质(GBW 07337~GBW 07339)和多金属结核国家标准物质(GBW 07249、GBW 07295和GBW 07296)作为校准样品,建立了手持式X射线荧光光谱仪测定富钴结壳样品的校准曲线。方法经国家标准物质GBW 07339验证,元素Mn、Fe、Co、Ni和Cu的精密度(RSD)在0.3%~3.0%之间,满足富钴结壳样品现场分析的要求。在海上资源勘查现场,应用手持式X射线荧光光谱仪对富钴结壳碎块和浅钻岩心原样进行了现场原位分析。富钴结壳碎块原样烘干后直接测试分析数据与实验室压片制样XRF分析数据对比表明,Mn、Fe、Co、Ni和Cu元素的测定值一致性良好;浅钻岩心的原位分析数据与实验室人工分层分析数据对比表明,各层位Mn、Fe、Co、Ni和Cu元素直接测试数据与实验室压片制样XRF分析数据分布趋势基本一致。实际应用研究表明,手持式X射线荧光光谱仪适合于现场原位分析,满足野外富钴结壳资源快速评价的要求,同时原位分析能更真实地反映原始富钴结壳岩心不同层位中各元素的变化特征,为进一步研究富钴结壳成矿机制提供更丰富的数据资料。 相似文献
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便携式X射线荧光光谱仪具有快速、无损分析的特点,本文重点研究了手持式X射线荧光光谱仪在富钴结壳碎块和浅钻岩心野外现场原位分析中的应用能力。采用压片法制样,以富钴结壳国家标准物质（GBW 07337~GBW 07339）和多金属结核国家标准物质（GBW 07249、GBW 07295和GBW 07296）作为校准样品,建立了手持式X射线荧光光谱仪测定富钴结壳样品的校准曲线。方法经国家标准物质GBW 07339验证,元素Mn、Fe、Co、Ni和Cu的精密度（RSD）在0.3%~3.0%之间,满足富钴结壳样品现场分析的要求。在海上资源勘查现场,应用手持式X射线荧光光谱仪对富钴结壳碎块和浅钻岩心原样进行了现场原位分析。富钴结壳碎块原样烘干后直接测试分析数据与实验室压片制样XRF分析数据对比表明,Mn、Fe、Co、Ni和Cu元素的测定值一致性良好;浅钻岩心的原位分析数据与实验室人工分层分析数据对比表明,各层位Mn、Fe、Co、Ni和Cu元素直接测试数据与实验室压片制样XRF分析数据分布趋势基本一致。实际应用研究表明,手持式X射线荧光光谱仪适合于现场原位分析,满足野外富钴结壳资源快速评价的要求,同时原位分析能更真实地反映原始富钴结壳岩心不同层位中各元素的变化特征,为进一步研究富钴结壳成矿机制提供更丰富的数据资料。 相似文献
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A Properly Developed Consensus from a Proficiency Test is,for All Practical Purposes,Interchangeable with a Certified Value for a Matrix Reference Material Derived from an Interlaboratory Comparison 
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下载免费PDF全文 Michael Thompson 《Geostandards and Geoanalytical Research》2018,42(1):91-96
A properly developed consensus from a proficiency test is, for all practical purposes, interchangeable with a certified value derived from an interlaboratory comparison. But some scientists have doubts about the metrological status of such values. In particular, the materials are not regarded as equivalent to certified reference materials (CRM) because of a lack of traceability of the consensus value. However, the detailed considerations in this study show that such a distinction is without foundation. The following issues are addressed. (a) Misgivings about the traceability of an interlaboratory consensus are found to be insubstantial because chemical measurements are hardly ever fully traceable. (b) Reproducibility (i.e., interlaboratory) conditions account for all sources of variation in results other than long‐term stability, so lead to a valid estimate of uncertainty. (c) Certification of a reference material according to ISO procedures is homologous with a proficiency test and no more secure against bias in the characterised value and its standard error. In particular, residual (common) bias cannot be fully addressed in either approach. (d) A consensus in itself attests to a valid outcome. (e) Proficiency test providers have access to a powerful method of monitoring long‐term stability that is denied to CRM producers. 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 Canadian Certified Reference Materials Project announces recommended values for radium-226 activity in four reference materials previously certified for uranium. Thirteen laboratories participated in the interlaboratory program for DL-la, DH-la, BL-4a and BL-5. Four measurement techniques were applied. Procedural and instrument calibrations were performed with certified radium solutions from the National Bureau of Standards, thereby establishing traceability of the recommended values for radium-226 in DL-la, DH-la, BL-4a and BL-5. These reference ores are also shown to be close to, if not in, radioactive equilibrium. 相似文献
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金矿石化学物相分析标准物质的研制 总被引：10，自引：2，他引：10
介绍了金矿石化学物相分析标准物质的研制工艺及技术关键，列出了单体金、连生体金、硫化物包裹金、其他矿物包裹金及总金的原始数据和定值数据。经9个实验室共同分析协作，研制的5个标准物质已被国家质量监督检验检疫总局批准为国家一级标准物质。该系列标准物质主要用于金矿石化学物相分析质量监控、分析方法评价等。 相似文献
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随着我国对生态文明建设的重视,自然资源综合调查势在必行,对生物标准物质亦提出了新的需求。当前相关调研工作已经大面积开展,自然资源综合调查、农产品与食品安全评价都需要对生物样品元素组成进行准确测试,需要以生物标准物质作为生物成分测试量值比对和溯源的基础,因此对生物基体标准物质的需求量大幅增加。大米作为主要粮食之一,其食品安全日益受到重视,对大米中的化学成分进行准确的分析测试具有重要的现实意义,因而对大米标准物质的需求量尤为突出,但目前大米成分分析标准物质已供不应求。本文严格按照《标准物质定值的通用原则及统计学原理》（JJF 1343—2012）和《地质分析标准物质的研制》（JJF 1646—2017）等相关规范要求,开展了GBW10010a大米成分分析标准物质的复（研）制工作,包括样品采集、加工制备、均匀性检验、稳定性检验、多家实验室协作定值测试及不确定度评定等关键环节。结果表明：本次复（研）制的大米标准物质定值成分多样、量值准确可靠,符合国家一级标准物质的要求。GBW10010a共定值54项主微量元素,包括Ag、Al、As、B、Ba、Be、Bi、Ca、Cd、Ce、Co、Cr、Cs、Cu、Dy、Er、Eu、Fe、Gd、Ge、Hg、Ho、K、La、Li、Ho、Mg、Mn、Mo、N、Na、Nb、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Sc、Se、Si、Sm、Sr、Tb、Th、Tl、Tm、U、V、Y、Yb、Zn,其中的39项元素给出了标准值及不确定度,包括Ag、Al、As、B、Ba、Ca、Cd、Ce、Co、Cs、Cu、Dy、Er、Fe、Hg、K、Li、Mg、Mn、Mo、N、Na、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Se、Si、Sm、Sr、Tb、Tl、Y、Yb、Zn;15项元素提供参考值,包括Be、Bi、Cr、Eu、Gd、Ge、Ho、Ho、La、Nb、Sc、Th、Tm、U、V。与原有GBW10010大米标准物质相比较,GBW10010a中As、Cd、Co、Cr、Cu、Hg、Mn、Mo、Ni、Zn等重金属元素含量显著下降,其中Cd、Cu、Zn降幅较大,分别下降约39%、43%、38.7%,一定程度上反映了农田生态环境的改善。本批标准物质定值元素总数量增加了6项,新增定值元素Ag、Nb（Nb给出参考值）,并且各项元素不确定度范围整体上有所缩小,如Al、Cd、Cu、Fe、K、Mg、Mo、Na、P、Pb、Se、Zn等对生物易有影响的重要元素,表明了地质分析测试方法技术的进步及定值水平的提高。本批标准物质定值元素涵盖了具有生物效应的大部分主微量元素,适用于农业生态环境地球化学调查与评价、生物样品测试、农产品质量与食品安全评价样品测试时的分析仪器校正、分析方法评价和分析质量监控等多个领域。 相似文献
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The Canadian Certified Reference Materials Project reports recommended values of lead-210 activity in four uranium reference materials previously certified for uranium and radium-226. Eleven laboratories participated in the interlaboratory program for DL-1a, BL-4a, DH-1a and BL-5; three measurement techniques were applied. Procedural and instrumental calibrations were performed with a certified lead solution from Amersham International Corp., thereby establishing traceability of the recommended values for lead-210. Activity ratios for uranium-238. radium-226 and lead-210 demonstrate these uranium reference materials to be in secular equilibrium, within experimental uncertainties. 相似文献
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地球化学与环境样品分析标准物质和GeoReM数据库 总被引：7，自引：5，他引：2
在地球化学和环境样品分析中,标准物质发挥着越来越重要的作用。尽管通常要求分析者必须提供量值溯源的测量过程的信息;但大多数论著都未给出标准物质的数据。文章强调标准物质在地球化学分析工作中的重要性,同时将地球化学与环境样品分析标准物质数据库GeoReM介绍给中国的地质分析工作者。GeoReM数据库收录了1880个地球化学和环境样品分析标准物质的定值数据、汇编数据、分析数据及其他相关信息,其中包括156个由中国制备的标准物质的数据。GeoReM数据库还给出了所收录标准物质推荐使用的首选值及其不确定度。尽管这些首选值大多都不是按照国际标准化组织的有关规定而确定的,但是它们的置信度高,因而被广泛应用于仪器校准和分析数据的质量监控。文章还指出要将中国研制的、发表在中文期刊上的标准物质也收录到GeoReM数据库中,这对于促进中国的相关研究,增加国际认可度具有重要意义。 相似文献
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本文以敞开式四酸溶样,电感耦合等离子体质谱测定了新疆、青海区调样品中的Co、Mo、W、Pb等元素,并把ICP-MS、ICP-AES和XRF三个大型仪器对新疆卡克-色帕巴衣地区样品的测定结果进行了比较,确定了区调样品元素分析方法的配套方案,并对溶样过程进行了一系列的优化,其方法检出限和精密度均符合DZ0130.4-2006及补充说明中1﹕5万化探样品标准要求。经国家标准物质验证,结果与标准值相符。优化的分析方法快速灵敏度高,能用于地球化学填图计划中分析测试任务, 同时也用于日常大规模多元素分析。 相似文献
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Jean S. KANE 《Geostandards and Geoanalytical Research》1991,15(1):13-21
Two principal approaches are being used currently to develop reference samples used in geochemistry. The first is typified by work at The National Institute of Standards and Technology (NIST) to develop standard reference materials (SRMs) whose elemental concentrations are certified. All data is collected under stringent quality control (QC). Agreement between average results for replicated analyses (6≤n<20) obtained by two or more analysts using either a single, definitive method or independent methods of analysis is required for certification; a large number of laboratory/method average results is not. The United States Geological Survey (USGS), International Working Group (IWG), and others base recommended concentrations on larger sets of compiled data, which may or may not have been collected under similar conditions of QC. The derived recommended concentrations are updated periodically, on the assumption that recommended concentration quality improves as the size of the data base increases. That assumption is examined in this paper, and the general lack of statistically significant difference between original and updated concentration is demonstrated. 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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A large number of certified and other reference samples are available for use in analytical geochemistry. Certified materials are preferred, but of much more limited availability than other reference samples for most geochemical applications. The availability of rock, sediment, soil, water, and plant reference samples is outlined; ore and mineral separate reference samples are not included in the discussion. The preparation of these materials, including the establishment of certified or recommended concentrations, is then reviewed. It is shown that comparable quality can be achieved for both certified and recommended concentrations, though it has not always been achieved in the past. Finally, the most appropriate ways to use reference samples in quality control and instrumental calibration are discussed. 相似文献
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Suitability of AuRM2 as a Reference Material for Trace Element Microanalysis of Native Gold 下载免费PDF全文
下载免费PDF全文 Mikkel Tetland John Greenough Brian Fryer Michael Hinds Mohamed E. Shaheen 《Geostandards and Geoanalytical Research》2017,41(4):689-700
Microanalysis of native gold specimens has been hampered by the lack of a suitable reference material (RM) known to be sufficiently homogeneous at the scale of microanalytical sampling. The suitability of gold reference material AuRM2 for microanalysis was assessed. This RM was created for bulk analysis of refined gold and was only certified for homogeneity at the bulk scale. However, it contains trace elements in appropriate mass fraction ranges for analysis of native gold. This study was not intended to provide alternative mass fractions from the original certified values, only to assess its suitability for microanalytical methods. Micro‐scale (~ 3.4 μg sample mass) heterogeneity was calculated from measurement repeatability of LA‐ICP‐MS analyses of AuRM2 by factoring in signal (represented by counting statistics) and instrument set‐up‐specific variability (determined using measurement variability of a reference material known to be homogeneous). Elements determined to be homogeneous or to have minor heterogeneity (< 10% calculated heterogeneity RSD) are Mg, Al, Ti, Fe, Ni, Cu, Zn, Se, Rh, Sn, Sb, Pt and Pb. Elements with moderate heterogeneity (10–20% heterogeneity RSD) are: Mn, As, Pd, Te and Bi. Correlation of element mass fractions indicates that micro‐scale inclusions of chalcophile‐rich phases along grain boundaries may be responsible for some of the chemical heterogeneity. However, the level of heterogeneity is statistically negligible compared with the ranges of chemical signatures observed in sample populations of native gold. Therefore, AuRM2 is shown to be sufficiently homogenous at a micro‐scale for use as a RM for microanalysis of native gold. 相似文献