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1.
The 2-year international joint project HYCREF (Contract-No. G6RD-CT-2002-00854), funded by the European Commission in the 5th Framework programme, aimed to develop methods to prepare homogenous and stable water-, soil- and waste reference materials contaminated with mineral oil hydrocarbons and to test certify the mineral oil content by gas chromatographic methods. As mineral oil products are important sources for environmental contaminations, appropriate reference materials certified by using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: prEN 14039 and KW/04, water: ISO 9377-2) are highly needed. Additional to the HYCREF-results presented in part I–mineral contaminated soils–this second paper gives an overview of the feasibility study for the preparation and test certification of three waste reference materials (offshore marine sediment, building material and industrial waste). The following specifications, which had been defined in the project work plan, were reached successfully: uncertainty of the mineral oil content resulting from the certification exercise ≤5% and a between-bottle inhomogeneity of ≤3%. All three materials have been evaluated for long- and short term stability. They contain different levels and types of mineral oil and cover the full application range of ISO/FDIS 16703 and prEN 14039 (100–10,000 mg/kg). The expanded uncertainties U cert of the three materials are about 6%. In this way, they are comparable to ERM®-CC015a (U cert=7.1%, mineral oil in a river sediment) and are suited to close the present gap of commercially available CRM for mineral oil determination in waste.  相似文献   

2.
 Until quite recently, Australia has not been much involved in the preparation and certification of matrix reference materials for chemical testing. Even today, the vast bulk of chemical reference materials used in Australia are imported from other world producers. Increased international focus on the accuracy, traceability and comparability of chemical measurements has led to the establishment of the National Analytical Reference Laboratory (NARL) within the Australian Government Analytical Laboratories. Part of the work of NARL will be to supply matrix reference materials, not available from existing sources, to meet specific Australian requirements. This need has been addressed in the past by a combination of industry and government initiatives. Examples include a series of certified matrix reference materials for chemical testing of iron ore, coal and mineral sands produced by Standards Australia and a series of three animal fat matrix reference materials certified for a range of pesticide residues produced by the Australian Chemical Standards Laboratory (now part of NARL). To make effective use of limited resources, it will be important for NARL to focus on identified priorities and to maximise the use of available Australian resources and expertise through technical collaboration for reference material production. An important part of this process should be input on needs and priorities from reference material "users" such as government legislators, regulatory authorities, standards setting bodies, industry and the analytical community. The aim will be to produce matrix certified reference materials that are traceable to SI or other international standards at a stated level of measurement uncertainty.  相似文献   

3.
Four mineral oil certified reference materials (CRMs), NMIJ CRM 7902-a, CRM 7903-a, CRM 7904-a, and CRM 7905-a, have been issued by the National Metrology Institute of Japan, which is part of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST), for the determination of polychlorinated biphenyls (PCBs). The raw materials for the CRMs were an insulation oil (CRM 7902-a and CRM 7903-a) and a fuel oil (CRM7904-a and CRM 7905-a). A solution of PCB3, PCB8, and technical PCB products, comprising four types of Kaneclor, was added to the oil matrices. The total PCB concentrations in the PCB-fortified oils (CRM 7902-a and CRM 7904-a) are approximately 6 mg kg−1. In addition, the mineral oils which were not fortified with PCBs were also distributed as CRMs (CRM 7903-a and CRM 7905-a). Characterization of these CRMs was conducted by the NMIJ/AIST, where the mineral oils and the PCB solution were analyzed using multiple analytical methods such as dimethylsulfoxide extraction, normal-phase liquid chromatography, gel permeation chromatography, reversed-phase liquid chromatography, and chromatography using sulfoxide-bonded silica; and/or various capillary columns for gas chromatography, and two ionization modes for mass spectrometry. The target compounds in the mineral oils and those in the PCB solution were determined by one of the primary methods of measurement, isotope dilution–mass spectrometry (ID-MS). Certified values have been provided for 11 PCB congeners (PCB3, 8, 28, 52, 101, 118, 138, 153, 180, 194, and 206) in the CRMs. These CRMs have information values for PCB homologue concentrations determined by using a Japanese official method for determination of PCBs in wastes and densities determined with an oscillational density meter. Because oil samples having arbitrary PCB concentrations between respective property values of the PCB-fortified and nonfortified CRMs can be prepared by gravimetric mixing of the CRM pairs, these CRMs can be used for validation of PCB analyses using various instruments which have different sensitivities. Figure Preparation and certification processes of the mineral oil CRMs (example shown is polychlorinated biphenyls in insulation oil, high/low concentrations) Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

4.
The main objective of the reference materials for biofuel specifications (BIOREMA) project is the development of two test materials (one bio-ethanol material and one biodiesel material) with well-established reference values. Of a series of three papers, this part describes the material preparation, homogeneity study, stability study, and characterisation of the bio-ethanol material. The test material thus obtained was used in an interlaboratory comparison (ILC) to assess current practices and comparability amongst laboratories providing bio-ethanol testing services. Only 13 participants provided data, resulting in a small dataset for evaluation. Further, it appeared that for a number of laboratories, there was not sufficient material for the determination of all requested parameters. In most cases, as far as the data permit, it can be concluded that the consensus values (based on participant’s results) are in good agreement with the reference or the BIOREMA values (obtained by NMIs participating in the project). For three parameters, namely ethanol content, water content, and density, there is good agreement between the reference and consensus values. For these parameters, the reproducibility standard deviation is close to, or even smaller than, the expanded uncertainty associated with the reference value. A number of parameters show very poor reproducibility, for example, pHe, electrolytic conductivity, and acidity. The same applies to sodium and copper content, which are very low and therefore challenging parameters to measure accurately. The results of the ILC underpin the need for certified reference materials and demonstrate the requirement for more robust quality control to improve the precision and trueness of the results from testing laboratories.  相似文献   

5.
VKI, the Danish national reference laboratory for environmental chemistry, has prepared a range of reference materials for quality control of nutrient analyses in environmental samples. The relevant concentration levels and potential matrix interference effects vary with the sample type. In sea water, nutrient concentrations are in the g/L range and salt concentrations can cause matrix interferences. Two certified reference materials for nutrient analyses were prepared representing the salinities in the Kattegat (20–25 parts per thousand) and the Baltic sea (below 10 parts per thousand). The preparation and certification were an integrated part of a larger project conducted by VKI on the optimisation of nutrient analyses in sea water. Part of the project has been participation in a European interlaboratory trial exercise QUASIMEME [1], which has enabled the Danish reference material data to be traced back to other European data. Denmark has now a certified reference material that will help to ensure the quality of marine analyses that are part of the ongoing national water monitoring plan.  相似文献   

6.
A number of reference materials for oxygen in different non-ferrous metals have been certified by BCR in the frame of a multidisciplinary Community project. The contribution of nuclear analysis methods is illustrated by several examples concerning the optimization of sample preparation techniques, the analysis of low and high oxygen non-ferrous metals and the extension of the program to other non-metals, especially nitrogen and carbon. Communication presented at the 5th Symposium on the Recent Development in Activation Analysis, Oxford, 17–21, July 1978. Scientific Secretary of BCR-Sub Working Group “Non-metals in non-ferrous metals”.  相似文献   

7.
Summary The analytical difficulties in mycotoxin determination have given rise to the development of mycotoxin reference materials by the European Community Bureau of Reference (BCR) in cooperation with several European Laboratories, among them the National Institute of Public Health and Environmental Protection. The first project undertaken concerned four milk powders certified for their aflatoxin M1 content (concentrations 0, 0.1, 0.3 and 0.8 g/ kg). Projects that are well-advanced include two peanut meals (aflatoxin B1 contents 0 and ca. 200 g/kg) and two compounded animal feedingstuffs (aflatoxin B1 contents 0 and 10 g/kg). Mycotoxin reference materials are also under development for zearalenone in wheat and maize, and for ochratoxin A in wheat.The general approach followed in the development and certification of mycotoxin reference materials (preparation, testing for homogeneity and stability, intercomparisons of methods and certification exercise) will be discussed and exemplified with the help of the completed project on aflatoxin M1 in milk powder.
Entwicklung von Mycotoxin-Referenzmaterialien
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8.
A modified three-step sequential extraction procedure proposed by the Commission of European Communities Bureau of Reference (BCR) was applied to certified reference materials of three different soil groups (rendzina, luvisol, cambisol) and sewage sludge of different composition originating from a municipal water treatment plant in order to assess potential mobility and the distribution of vanadium in the resulting fractions. Analysis of the extracts was carried out by electrothermal atomic absorption spectrometry with Zeeman background correction using transversely heated graphite atomizers. Extracts showed significant matrix interferences which were overcome by the standard addition technique. The original soil and sludge certified reference materials (CRMs) and the extraction residue from the sequential extraction were decomposed by a mixture of HNO3–HClO4–HF in an open system. The content of V determined after decomposition of the samples was in very good agreement with the certified total values. The accuracy of the sequential extraction procedure was checked by comparing the sum of the vanadium contents in the three fractions and in the extraction residue with the certified total content of V. The amounts of vanadium leached were in good correlation with the certified total contents of V in the CRMs of soils and sewage sludge. In the soils examined, vanadium was present almost entirely in the mineral lattice, while in the sewage sludge samples 9–14% was found in the oxidizable and almost 25% in the reducible fractions. The recovery ranged from 93–106% and the precision (RSD) was below 10%.  相似文献   

9.
为建立采用催化裂解-金汞齐富集-冷原子吸收光谱仪即直接测汞仪测定土壤样品中汞含量的方法,本研究配制汞总量为0~2 ng、0~15 ng和25~1023 ng的三种不同汞浓度系列的标准工作曲线,选取9个土壤样品,3种国家土壤有证标准物质,同一样品分别进行6组平行测定,并抽取3个土壤样品进行3种不同浓度加标回收试验,以对其方法精密度和准确度进行论证。 结果显示:仪器信号值与Hg总量之间均呈良好的线性关系。根据仪器多次测定空白数据结果,按照称样量0.1 g计算,方法最小检出量为0.09 ng/g;平行测定结果相对标准偏差均小于10%,土壤标准物质测定值与标准物质标准参考值均相符,不同浓度的加标回收率范围为78.4%~92.7%。结果表明催化裂解-金汞齐富集-冷原子吸收光谱仪,可用于批量土壤样品中汞含量的快速测定分析,方法的精密度和准确度可满足测定分析要求,且实验过程中无需前处理消煮,操作方便、快速高效。  相似文献   

10.
食品和食品接触材料中矿物油的潜在危害性引起了国内外的普遍关注和深入研究。矿物油是石油提炼过程中的副产物,成分复杂,为分析检测带来了很大的挑战,也促使相关检测技术不断向前发展。目前,针对不同样品基质,已有多种提取、净化方法;国内外也先后建立起了固相萃取/气相色谱法、气相色谱-质谱法、液相色谱-气相色谱联用法、二维气相色谱法、核磁共振等测定方法。该文将对食品和食品接触材料中矿物油检测技术的应用及进展进行综述,并对新技术的发展进行展望,为后续的应用提供借鉴和参考。  相似文献   

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