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1.
Results are presented from the seventy two laboratories participating in GeoPT5, round five of the international proficiency testing programme for analytical geochemistry laboratories. The sample for round five, AMH-1 (Mount Hood andesite), was distributed during March 1999 and participating laboratories were asked to analyse the sample using their routine techniques and submit results to the steering by 15th June 1999. In this report, contributed data are listed together with the derived z-scores from which participating laboratories can assess their analytical performance. Z-scores in the range -2 to 2 are considered satisfactory. Z-score values that lie outside this range may indicate unsuspected analytical bias. The distinctive feature of the present round is that AMH-1 is a candidate reference material prepared by the USGS and it is intended that the present proficiency testing data will contribute to the reference material characterisation programme.  相似文献   

2.
The analytical data received in an inter-laboratory study of four Canadian reference samples were treated by two different methods in order to arrive at "usable values" for the concentration of each constituent. The first method ("Select Laboratories"), proposed by S. Abbey (S.A.), is based on the fact that some laboratories consistently produce better results than others. S.A. suggests an approach which permits isolation of results from such laboratories, calculation of a mean or a median of such results and use of one or the other as the concentration of a constituent. That approach involves a degree of subjectivity and S.A. attempts to demonstrate the validity of his approach by means of several tests applied to the results obtained for the four samples.  相似文献   

3.
The results of the first international proficiency test (GeoPT1) of geochemical laboratories are presented. A total of 49 laboratories contributed analytical data on G94, a sample of Threlkeld microgranite which had been collected at the International Conference, Geoanalysis 94. Assigned values were derived by robust statistical analysis of contributed data for 12 major elements and 39 trace elements, of which 3 (As, Pb and The) were provisional values. Z-scores were calculated, as required by the protocol using either 'pure geochemistry'or 'applied geochemistry'fitness for purpose criteria selected by contributing laboratories. An overview of the z-score results indicates that 28.7% of contributed data fell outside the -2相似文献   

4.
郑存江 《岩矿测试》2005,24(4):284-286
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   

5.
Organic matter in eight rock samples has been analyzed by nineteen laboratories and the results show that source rock data from any one laboratory cannot be directly compared to data from any other laboratory. A high degree of variability exists among the data reported by the nineteen participating laboratories, most of which can be explained by differences in the sample preparation steps and analytical procedures used in these laboratories. Differences also exist in the definition of basic units of measurement being reported. In order to make the data more comparable, standard rock samples and analytical methods should be developed and used by all laboratories. Until then, extreme caution must be used when comparing source rock data from different laboratories.  相似文献   

6.
Results from seventy two laboratories participating in GeoPT3, round three of the international proficiency testing programme for analytical geochemistry laboratories, are presented. The report includes analytical results contributed by participating laboratories, together with the z-scores derived from these results using appropriate fitness for purpose criteria. These data are available for use as part of the laboratories' quality control procedures to assess the reliability of analysed results.  相似文献   

7.
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   

8.
赵伟  王烨  徐靖  王君玉  陈爱平 《岩矿测试》2010,29(4):419-424
介绍了黑色页岩样品中6个铂族元素铂、钯、钌、锇、铑、铱的标准物质研制过程。黑色页岩样品采自贵州黄家湾,为一次采集、一次混样的原始样品,随机抽取包装好后的样品进行检验与定值。均匀性、稳定性符合要求后,按照国际标准化组织(ISO)34、35指南的基本要求和我国一级标准物质的技术规范,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6个铂族元素进行定值。以各实验室组数据作为最小统计单元,用Grubbs准则、Dixon法检验剔除离群数据,Shapiro-Wilk法检验各元素数据分布的正态性。检验结果100%的元素呈正态或近似正态分布。定值的6个元素均符合标准值水平。  相似文献   

9.
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   

10.
Abbey's select laboratories method has been applied to the reported data for major and minor elements in the proposed GIT-IWG reference sample IF-G. The final values obtained by this method have been compared with the recommended values published by Govindaraju in 1984. Slightly different percentages are suggested for MgO, K2O and Fe2O3T. The importance of applying the Abbey method by participants in co-operative studies is emphasized. Such an application gives a better understanding of data treatment and of the degree of reliability of published final values; furthermore the objective score obtained for laboratory quality will stimulate participating laboratories to improve their analytical methods and procedures. As an illustration some improvements in the laboratory of the authors are mentioned.  相似文献   

11.
高翔云 《岩矿测试》2010,29(5):593-596
根据《地质矿产实验室测试质量管理规范》的要求,为保证地下水污染调查中样品的准确测定,需采取质量控制方法。文章阐述了地下水样品的前处理和测定过程的质量控制措施,建立了地下水有机组分分析过程的质量控制流程,确保其检测数据达到规范所允许的范围。  相似文献   

12.
Software designed for analytical laboratories to guarantee traceability and accessibility of rocks with their geochemical properties has been developed. The software documents the sample origin, current sample location and the location of any sample subsets (e.g., thin sections, solutions, etc.), and archives all associated geochemical data sets. The software can be installed on a personal computer so is available for use in any laboratory and allows curation before and after publication. The software will be of use in integrating and sharing geological reference materials within and among institutes. In this article, the system design and implementation are detailed. All source codes for the software are available at http://dream.misasa.okayama-u.ac.jp/ .  相似文献   

13.
A new proficiency testing sample, OPY‐1 (ultramafic rock), the basis of the twentieth international proficiency test of analytical geochemistry laboratories (GeoPT 20), was recently prepared by the International Association of Geoanalysts (IAG). This paper reports analytical data for Os, Ir, Ru, Rh, Pt and Pd with different digestion techniques, including an improved Carius tube, Carius tube combined with HF dissolution and alkaline fusion. About 4–15% of the PGEs are in the silicate phase, which cannot be leached by aqua regia even when digested at 300 °C with the Carius tube technique. Both the Carius tube technique combined with HF dissolution and alkaline fusion can obtain reliable data. The results demonstrated that OPY‐1 is sufficiently homogeneous at a 2 g test portion level to be suitable as a reference material for method validation. The procedure for sealing the Carius tube was simplified and the recommended digestion procedures are provided.  相似文献   

14.
生物成分系列标准物质的研制   总被引：4，自引：7，他引：4  
GSB系列生物标准物质包括大米、小麦、玉米、黄豆、圆白菜、菠菜、茶叶、奶粉、鸡肉和苹果等10种生物样品，用冷冻干燥等技术制备。由14个分析水平较高的实验室协作，采用等离子体质谱、等离子体光谱和仪器中子活化为主的10余种分析方法测试，共进行了22477次测定，取得了5136组平均值数据，定值元素59种，定标准值元素54种。  相似文献   

15.
Results are presented for round one of a new international proficiency testing programme designed for microprobe laboratories involved in the routine analysis of silicate minerals. The sample used for this round was TB-1, a basaltic glass fused and prepared by the USGS. Thirty nine laboratories contributed data to this round, the majority of major element results being undertaken by EPMA and the majority of trace elements by LA-ICP-MS. Assigned values were derived from the median of results produced by nine selected laboratories that analysed powdered material by conventional ICP-MS, INAA and XRF techniques using bulk powders of the sample. Submitted microprobe results were evaluated using a target precision calculated using the Horwitz function, adopting the same criteria as those used for "applied" geochemistry laboratories in the companion GeoPT proficiency testing programme for laboratories involved in the routine bulk analysis of silicate rocks. An evaluation of results from participating microprobe laboratories indicated that overall, data were compatible with this precision function. A comparison between the performance of bulk and microprobe techniques used in the analysis of the basaltic glass showed remarkably good agreement, with significant bias only observed for the major oxide MgO.  相似文献   

16.
Enantiomeric (d/l) ratios of eight amino acids in three homogeneous powdered fossil Pleistocene mollusk samples have been compared. Eleven laboratories have contributed results to this effort. Three gas chromatographic methods and one ion-exchange chromatographic method were used. In general, the coefficients of variation (c.v.) are best for alanine, glutamic acid, and aspartic acid (3–8%). For leucine and phenylalanine, the c.v.'s are between 5 and 10%. For isoleucine, proline, and valine the c.v.'s range from 10 to 18%. Individual laboratories usually report analytical precision of between 2 and 5%, but it is clear that significant differences between laboratories' results are often encountered, and that these analytical differences could, in some cases, lead to very significant differences (25% or more) in age estimates based upon enantiomeric ratios. Multiple analyses of desalted hydrolyzates of these powder samples suggest that interlaboratory differences are often caused by instrumental and/or derivatization procedures rather than the wet-chemical sample preparative steps. It is proposed that the powder samples described here be used in all future publications of fossil amino acid enantiomeric ratio data.  相似文献   

17.
Results from sixty laboratories participating in GeoPT2, the international proficiency testing programme for analytical geochemistry laboratories, are reported. Compared with 71.3% in the last round, 74.6% of the reported data complied with the laboratories' selected fitness for purpose criteria.  相似文献   

18.
WITS-1 is a sample of silicified komatiite collected from close to the Komati River type section, near Barberton in South Africa. Two thousand kg of this komatiite was crushed and prepared for standardization. Noble metal analysis of WITS-1 has been carried out by six laboratories using four different analytical methods. The data obtained from these sources were subjected to statistical analysis (F ratio and Student t test) and a suite of "preferred" values for the noble metal concentrations are reported.  相似文献   

19.
Most laboratories aim to produce data of the highest quality. Trying to lower uncertainties to infinitesimal figures and push detection limits even lower are valid goals. However, is it possible to overachieve? Are old data still of good enough quality to be usable? In a geochemical context, the main goal of producing analytical results is to answer geological or environmental questions. Not all scientific problems require the same data quality. What is really required are data of adequate quality – i.e., ‘fit-for-purpose’– to ensure that the geological problem at hand can be solved. Furthermore, it is doubtful that uncertainties and reproducibilities associated with field sampling are better than those from laboratories. It is thus proposed that, as geoanalysts, we encourage data users (students, colleagues or referees) to ensure that their analytical results are of sufficient quality to solve the problem. However, authors have to demonstrate, through the use of reproducibility testing, reference and quality control materials, that the quality of their results is sufficient to solve the problem. Uncertainties and detection limits in publications should not only be evaluated with respect to a set value, such as 10%, but also with regard to the geological problem to be solved.  相似文献   

20.
Four silicate glasses were prepared by the fusion of about 1 kg powder each of a basalt, syenite, soil and andesite to provide reference materials of natural composition for microanalytical work. These glasses are referred to as ‘Chinese Geological Standard Glasses’ (CGSG) ‐1, ‐2, ‐4 and ‐5. Micro and bulk analyses indicated that the glasses are well homogenised with respect to major and trace elements. Some siderophile/chalcophile elements (e.g., Sn, Pt, Pb) may be heterogeneously distributed in CGSG‐5. This paper provides the first analytical data for the CGSG reference glasses using a variety of analytical techniques (wet chemistry, XRF, EPMA, ICP‐AES, ICP‐MS, LA‐ICP‐MS) performed in nine laboratories. Most data agree within uncertainty limits of the analytical techniques used. Discrepancies in the data for some siderophile/chalcophile elements exist, mainly because of possible heterogeneities of these elements in the glasses and/or analytical problems. From the analytical data, preliminary reference and information values for fifty‐five elements were calculated. The analytical uncertainties [2 relative standard error (RSE)] were estimated to be between about 1% and 20%.  相似文献   

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