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New mean values for up to 11 major and minor and up to 11 trace elements in soils SO-1 to SO4 have been calculated by two procedures. Analytical results received by CCRMP subsequent to the certification program of 1979 were included. In one instance, the same procedure as used for certification wherein all results except those rejected on chemical and/or statistical considerations was followed, but little improvement over the 1979 calculations was obtained. The other procedure is proposed by the authors for use in identifying concentration range intervals wherein maximum interlaboratory consensus is observed. The application of this procedure has permitted the certification of the four soils for the content of 24 elements not previously certified. 相似文献
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W.S. BOWMAN G.H. FAYE R. SUTARNO J.A. McKEAGUE H. KODAMA 《Geostandards and Geoanalytical Research》1979,3(2):109-113
Four reference soils have been prepared and certified through the cooperation of Energy, Mines and Resources Canada and Agriculture Canada. Their origin and details of preparation and characterization are presented. Thirty-six laboratories participated in the international certification program by providing approximately 16000 results for 65 elements. One or more of the reference soils were certified for 18 elements and preliminary data were obtained for another 47. 相似文献
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电感耦合等离子体质谱法测定砂岩型铀矿样品中分步提取的铀 总被引：1，自引：0，他引：1
本文研究地质样品中铀形态的分析方法及应用技术,以进一步说明铀形态分析在地球化学找矿中的重要作用。该方法参考Tessier流程,将样品中的铀分为可交换离子态、碳酸盐结合态、铁锰氧化物结合态、硫化物及有机物结合态和结晶态,分别提取,提取溶液用高分辨率电感耦合等离子体质谱仪进行测量。设计的形态提取配方具有良好的可选择性和可重复性,经过国家标准物质、国际形态标准物质和人工模拟样品验证,证明形态提取试剂配方适合所定义的形态分析。通过对实际样品(总量铀为635μg/g)验证表明,碳酸盐结合态铀提取结果的可重复性最好(RSD为2.6%),其次为硫化物及有机物结合态铀(RSD为4.0%)、结晶态铀(RSD为6.0%)和铁锰氧化物结合态铀(RSD为6.1%),可交换离子态铀提取结果的可重复性最差(RSD为26%)。碳酸盐结合态铀与结晶态铀之比,可以用于反映地下铀矿的存在概率。 相似文献
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Jean S. Kane Philip J. Potts Thomas Meisel Michael Wiedenbeck 《Geostandards and Geoanalytical Research》2007,31(3):285-288
The International Association of Geoanalysts (IAG) published a protocol for the certification of reference materials in close accord with the International Organisation for Standardisation (ISO) guidelines (Kane et al. 2003). This article supplements that protocol, providing additional discussion of best approaches for pre-selecting laboratories for participation in certification projects. This discussion also makes a distinction between inter-laboratory certifications, where n = 15 is the general standard, and expert laboratory certifications, where a much smaller number of laboratories will be deemed qualified to provide data of the quality needed for certification. 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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研究了野外现场快速准确测定铀矿石中铀的三辛基氧膦(TOPO)萃取α计数法。目前野外现场铀的测量主要采用γ谱法,即利用铀子体的γ射线强度来计算铀的含量,当样品中铀镭处于不平衡状态时,γ谱法测铀存在着较大的测量误差。本文将铀的核性质与化学性质结合起来,采用密闭酸溶法快速溶解样品中的铀,酸溶后的样品不经分离直接在溶样罐中用TOPO萃取,进而测定样品中铀产生的α射线强度获得铀的含量,避免了γ谱法的不足。方法检出限为铀含量2.41μg/g;当铀含量为大约为100μg/g时,测量相对偏差为5.93%;铀的测定范围为7.23μg/g～n%。密闭酸溶法试剂用量少,溶样速度快,且对环境和操作人员污染小;酸溶后的样品用TOPO萃取2 min后即可达到萃取平衡,铀萃取效率在97%以上;所需的仪器设备可以车载形式用于野外现场铀矿石中铀的准确测定,野外应用操作简单、快速、精密度和准确性较高。 相似文献
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用经验模型判断能力验证统计分析结果的合理性 总被引：2，自引：1，他引：1
能力验证是检测实验室识别与同行差异的一种途径,但中国合格评定国家认可委员会( CNAS)在组织能力验证时发现由于种种原因,有些实验室并不能秉承诚信的原则参加能力验证活动,导致统计分析结果“失真”.如何甄别这种情况,确保所有参加CNAS能力验证活动的实验室都获得公平的评价,这是CNAS亟待解决的问题.本文在用国内文献数据对经验模型进行修正的基础上,提出用上报数据目标标准偏差(或稳健标准偏差,sR)与基于经验模型的计算值之比(H值)是否小于0.5作为判据来审核上报数据统计分析结果的合理性.对13套能力验证数据分析表明:其中10套上报数据sR正常,3套数据存在问题.当目标标准偏差偏小,H＜0.5时,建议采用同样是稳健统计方法的迭代法代替四分位法来计算目标标准偏差(sR),或用经验模型计算结果代替实验值计算Z值.通过验证表明,借助Horwitz经验模型可以判断能力验证数据统计分析结果的合理性,并能有效地识别并防止由于某种原因导致对能力验证结果评价失效的情况. 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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为进行核地质分析实验室间比对,采集了南方硬岩和北方砂岩铀矿石样本,按照标准物质制备方法制备了2种铀矿地质样品(编号分别为Albriug-09、Albriug-10),其粒度为小于60μm,铀含量分别为497mg·kg~(-1)和935mg·kg~(-1)。对用于样品均匀性检验的时间分辨紫外脉冲光诱导荧光分析法(TRLIF)进行了分析性能有效性评价。TRLIF测定铀的检出限为0.09mg·kg~(-1),测定范围为0.27~1250mg·kg~(-1);当铀含量范围在4.6~514mg·kg~(-1)之间时,其精密度(RSD%)在9.6%~3.43%之间;当铀含量范围在1.7~514mg·kg~(-1)之间时,其正确度(RE%)在±16.3%~±0.2%之间。应用TRLIF对制备的样品进行了铀含量均匀性测试并采用单因子方差分析法进行了统计检验,其统计量F分别为0.61和0.76,均小于临界值F0.05(9,10)(3.02),表明制备的样品均匀性好,符合实验室间比对测定要求。 相似文献
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Surendra P. Verma Leonides Javier Orduña-Galván Mima Guevara 《Geostandards and Geoanalytical Research》1998,22(2):209-234
A new computer programme was written in programming language TURBOC, which enables us to apply a procedure involving seventeen statistical tests (a total of sixty five single or multiple outlier versions of these tests) for outlier detection in univariate sample at a high confidence level of 99% (significance level α= 0.01). The outlying observations should be evaluated first for technical reasons and then rejected manually from the data base until no more outliers are detected and the final statistical parameters are computed from the remaining data. This programme has been used successfully to process two reference material data bases: WS-E from England and Soil-5 from Peru. The final mean values for WS-E are more reliable (characterized by smaller standard deviations and narrower confidence limits) than those obtained earlier using a different statistical approach. The application of a large number of statistical tests to Soil-5 also resulted in smaller standard deviation values for most elements than the method involving a limited number of such tests. For WS-E, some laboratories seem to have produced multiple data that were detected as statistical outliers. A close analysis of the distribution of outliers as a function of laboratory, country and analytical method leads to a technical justification for these outlying observations, probably in terms of inadequate QA/QC practices. Use of geochemical criteria indicates that the new mean values in WS-E might be closer to the "true" concentrations. This procedure of outlier detection and elimination is therefore recommended in the study of the existing RM. 相似文献
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Xiaohong Wang Yushu Gao Yimin Wang S.I. Andreev 《Geostandards and Geoanalytical Research》2003,27(3):251-257
A research project involving the preparation of three Co-rich crust reference materials (GSMC-1 to 3) has been preliminarily completed. The samples were collected from the eastern and central Pacific seamount zones and their main chemical composition is MnO2 . After the raw materials were dried in ambient air and at low temperature (60-100 C), they were ground in a ball mill to form a well-mixed powder. The proportion of particle size fractions of < 74 μm and < 3 μm was over 98% and 50% respectively. The homogeneity of the materials was tested using wavelength dispersive X-ray fluorescence spectrometry (WD-XRF). The relative standard deviation (% RSD) of the measurements for all the selected elements in forty sub-samples randomly taken from the bottles was less than 0.4%. Sixteen laboratories from Germany, Russia, France, Australia and China participated in the collaborative analysis programme. Fifty seven elements or constituents were analysed, and among those, forty six elements were certified in each sample. The sum of contents of the major and minor elements or components was 99.5% for GSMC-1, 99.6% for GSMC-2 and 99.2% for GSMC-3. 相似文献
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数量化理论Ⅰ模型规定:参与定量估算的预测要素数目小于等于研究区内已确定的典型矿床模型数目。事实上,多数研究区内可作为模型的典型铀矿床数目较少,因而限制了预测要素的选取,降低了预测精度,为解决此局限性,提出了一种新方法——矿床分割法。该方法是将某一典型铀矿床模型按其具有相似预测要素的矿带进行逆向分割,即拆分成一定数目的铀矿模型,扩充了模型数目,并保持分割后各模型区资源量不变。双桥-新路地区试验结果证明:运用"矿床分割法"后,预测要素的选取数目有了明显增加,提高了方向系数值,资源量估算值更接近模型区的实际资源量。 相似文献
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International Association of Geoanalysts'Protocol for the Certification of Geological and Environmental Reference Materials 总被引：2，自引：1，他引：2
Jean S. Kane Philip J. Potts Michael Wiedenbeck Jean Carignan Stephen Wilson 《Geostandards and Geoanalytical Research》2003,27(3):227-244
This protocol has been developed by the International Association of Geoanalysts to demonstrate procedures for the certification of geological and environmental reference materials to comply to the fullest extent possible with recommendations of the International Organisation for Standardisation (ISO Guide 35). A practical approach is described on the assumption that certifications will be normally be based on collaborative analysis programmes in which participating laboratories are preselected on the basis of performance in a proficiency testing programme or on the basis of other criteria of merit. 相似文献
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常量金标准物质定值中离群值的统计识别 总被引：1，自引：0，他引：1
离群值的剔除常用数理统计的方法,如格拉布斯检验法和迪克逊检验法等,但是这些统计方法用于常量金标准物质分析结果的统计检验,都存在着对离群值剔除明显不够的问题.本文建立了以常量金重复分析相对偏差允许限为依据的离群值统计识别方法,包括统计计算待定值样品中金的算术平均值x和相对偏差允许限YG,确定合格的测定结果的数据区间,从而识别出离群值并予以剔除;一次剔除后,按照新的统计量确定下一轮的离群值剔除范围,直到无离群值后,给出金的平均值及其波动范围.以15个人工组合的常量金标准物质为例,模拟金标准物质定值分析,以密码形式分派给不同单位和分析者,共收集10套独立分析结果,采用本法剔除离群值后,所得金算术平均值与金标准参考值更加接近,其相对偏差的质量分数为0.35,达到优秀;而格拉布斯法(或迪克逊法)和中位值法的质量分数分别为0.42和0.40,只能达到良好.应用本文建立的离群值统计识别方法,质量分数等级有了明显提高,增强了数据统计分析的有效性. 相似文献
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The Canadian Certified Reference Materials Project announces the availability of reference uranium tailings sample UTS-1, -2, -3 and -4. Eighteen laboratories participated in the interlaboratory program for total iron, titanium, aluminium, calcium, barium, uranium, thorium, total sulphur, sulphate and arsenic. Eight laboratories participated in the inter-laboratory program for thorium-230, radium-226, lead-210 and polonium-210 in all four samples and for thorium-232, radium-228 and thorium-228 in UTS-1 and UTS-2. 相似文献
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The possibility that the atomic ratio 235u/238U may be slightly variable due to natural nuclear chain reactions such as have been identified in Gabon, West Africa, has prompted a re-examination of very precise gas mass spectrometric isotopic ratio data from a number of laboratories. Two modal values of the isotopic ratio exist in the data. Their relative difference, 0.03%, is statistically significant. The lower mode is due principally to ores from the Colorado Plateau. This difference was recognized in 1963 by the U.S. Atomic Energy Commission but the substantiating data have not been openly published. Insufficient data presently exist to attribute this difference to chemical differentiation of the uranium isotopes, presumably in the ‘sandstone’ type deposits of the Colorado Plateau, or to dilution with Precambrian ore deposits, depleted in 235U by nuclear reactions. 相似文献
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监测中子积分通量是裂变径迹技术的重要组成部分。铀玻璃监测中子积分通量是国际裂变径迹定年标准化工作组推荐的重要方法之一，铀玻璃测定法还普遍用于测定样品中的铀含量及其空间分布。本文介绍的铀标准玻璃，经过多家实验室定值测定，表明其稳定性、均匀性均达到国家一级标准物质的要求，抗酸性能达到Ⅰ级光学玻璃水平，抗潮性能达到Ⅱ级光学玻璃水平。其它性能指标均达到或超过美国国家标准局的同类产品。 相似文献