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  • 1
    Electronic Resource
    Electronic Resource
    Certification of an animal feed reference material for the organochlorine pesticide contents: BCR CRM 115 (1997)
    Springer
    Fresenius' journal of analytical chemistry 357 (1997), S. 1035-1041 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract  An animal feed reference material has been prepared and enriched with 15 organochlorine pesticides at levels close to the maximum residue limits set up in the European Directive 74/63/EEC. The homogeneity of the material has been assessed on the basis of the pesticide contents at a level of sample intake of 5 g. The one year stability study revealed an instability of heptachlor, o,p′-DDT, p,p′-DDT, α-HCH and γ-HCH (decrease in content) and p,p′-TDE (increase) at +37 °C; at +20 °C no instability could be demonstrated. The material has been certified in an interlaboratory certification study for: HCB (0.0194 mg/kg), β-HCH (0.023 mg/kg), γ-HCH (0.0218 mg/kg), heptachlor (0.019 mg/kg), γ-Chlordane (0.048 mg/kg), α-Endosulfan (0.046 mg/kg), Dieldrin (0.018 mg/kg), Endrin (0.046 mg/kg), o,p′-DDT (0.046 mg/kg) and p,p′-DDE (0.047 mg/kg). The α-HCH isomer, Aldrin, β-Heptachloro-epoxide, p,p′-DDT and p,p′-TDE could not be certified. The methods used for the certification are described as well as the major difficulties encountered in the study.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160050300
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  • 2
    Electronic Resource
    Electronic Resource
    Improvement scheme for the determination of arsenic species in mussel and fish tissues (1999)
    Springer
    Fresenius' journal of analytical chemistry 363 (1999), S. 5-11 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Six interlaboratory studies were organised by the Standard, Measurement and Testing Programme of the European Commission on the determination of arsenic species (arsenobetaine, arsenocholine, monomethylarsonic acid, dimethylarsinic acid, As(III) and As(V)) in marine matrices and soil. A step-by-step approach was used and a meeting was held at the end of each study to help the participants to discover errors and to improve their analytical methods. The successive steps investigated the calibration procedures on various solutions, the separation and derivatisation techniques on solutions and extracts and the extraction on mussel and fish tissues. All materials used for the study were monitored for their stability. Verified calibration solutions and compounds were distributed to the participants in each exercise in order to trace calibration problems. The agreement between the results improved regularly and at the end of the six campaigns allowed the certification of a reference material of tuna-fish tissue (BCR-CRM 627) for its total arsenic, arsenobetaine and dimethylarsinic acid contents.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160051129
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  • 3
    Electronic Resource
    Electronic Resource
    Preparation of pure calibrants (arsenobetaine and arsenocholine) for arsenic speciation studies and certification of an arsenobetaine solution – CRM 626 (1999)
    Springer
    Fresenius' journal of analytical chemistry 363 (1999), S. 12-17 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Interlaboratory studies have been organised by the Standards, Measurement and Testing Programme in order to certify the content of some chemical forms of arsenic in fish and mussel tissue, soil and sediment. Among the six compounds of interest (arsenite, arsenate, dimethylarsinic and monomethylarsonic acids, arsenobetaine and arsenocholine) only four are commercially available. Arsenobetaine and arsenocholine of well defined purity had therefore to be prepared by the pilot laboratories in charge of the management of the project. The present work deals with the synthesis and characterisation of these two compounds and the certification of the content of arsenobetaine in a standard solution (BCR-CRM 626).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160051130
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  • 4
    Electronic Resource
    Electronic Resource
    Certification of total arsenic, dimethylarsinic acid and arsenobetaine contents in a tuna fish powder (BCR-CRM 627) (1999)
    Springer
    Fresenius' journal of analytical chemistry 363 (1999), S. 18-22 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Tuna fishes were collected in the Straits of Messina (Italy), were dissected and dorsal muscles minced, freeze-dried, ground and sieved. The obtained powder was stabilised by γ-irradiation and filled into brown glass bottles. The homogeneity and stability at +20 °C and +40 °C were verified with regards to the total arsenic, dimethylarsinic acid and arsenobetaine contents. Ten laboratories participated in the certification study. All participants had demonstrated beforehand their ability to produce accurate results for the As speciation in fish tissue. The certified values are: total arsenic (4.8 ± 0.3) mg/kg, arsenobetaine (52 ± 3) μmol/kg, dimethylarsinic acid (2.0 ± 0.3) μmol/kg. The material is available from the BCR since early 1998.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160051131
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  • 5
    Electronic Resource
    Electronic Resource
    The preparation of a certified reference material of polar pesticides in freeze-dried water (CRM 606) (1999)
    Springer
    Fresenius' journal of analytical chemistry 363 (1999), S. 632-640 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The preparation of a certified reference material of polar pesticides in freeze-dried water is described. The pesticides selected were atrazine, simazine, carbaryl, propanil, linuron, fenamiphos and permethrin which were added to 6000 litres of tap water at 50–80 μg · L–1 (200–320 μg · L–1 for permethrin) level in presence of NaCl (2.5 g · L–1) prior lyophilization. After the freeze-drying process the residue was rehomogenized, filled into amber glass bottles and stored at –20 °C, +4 °C and +20 °C. All pesticides were determined by HPLC/diode array detector, except permethrin which was determined by GC/ECD. The results obtained for atrazine, simazine, carbaryl, propanil, linuron and fenamiphos showed no within- or between-bottle inhomogeneity, however the material was non-homogeneous for permethrin and therefore this was withdrawn from further studies. With respect to the stability for over one year, all pesticides were stable at –20 °C. At +4 °C all pesticides were stable for at least 9 months and at +20 °C the stability was demonstrated only during the first month of storage. The content (mass fractions) of atrazine, simazine, carbaryl, propanil and linuron in freeze-dried water (CRM 606) was certified by an interlaboratory testing and a certification campaign.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160051263
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  • 6
    Electronic Resource
    Electronic Resource
    Certification of the contents of five polychlorodibenzo-p-dioxins and six polychlorodibenzo furans in milk powder (1997)
    Springer
    Fresenius' journal of analytical chemistry 359 (1997), S. 222-229 
    Details
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract  Preparation, homogeneity and stability studies of a natural milk powder material and subsequent certification of the mass fraction of five polychlorodi-benzo-p-dioxins (D48, D54, D66, D67, D70) and six polychlorodibenzo furans (F83, F94, F114, F118, F121, F130) are described. The material, CRM 607, is intended for use in the method validation and quality control of the complete analytical procedure for congener-specific determination of dioxins in milk powder and similar dairy products and was certified in an interlaboratory study for: 2,3,7,8-TCDD, 0.25 ng/kg; 1,2,3,7,8-PeCDD, 0.79 ng/kg; 1,2,3,4,7,8-HxCDD 0.42 ng/kg; 1,2,3,6,7,8-HxCDD, 0.98 ng/kg; 1,2,3,7,8,9-HxCDD, 0.34 ng/kg; 2,3,7,8-TCDF, 0.05 ng/kg; 1,2,3, 7,8-PeCDF, 0.054 ng/kg; 2,3,4,7,8-PeCDF, 1.81 ng/kg; 1,2,3,4,7, 8-HxCDF, 0.94 ng/kg; 1,2,3,6,7,8-HxCDF, 1.01 ng/kg and 2,3,4,6,7,8-HxCDF, 1.07 ng/kg. An indicative (non-certified) value was assigned to the mass fraction of the hepta- and octachlorinated congeners D73, D75, F131, F134, F135 and the HxCDF F124.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002160050564
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  • 7
    Electronic Resource
    Electronic Resource
    Improvements in the determination of eight polycyclic aromatic hydrocarbons through a stepwise interlaboratory study approach (1996)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 356 (1996), S. 41-48 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A summarising account of a systematic stepwise approach based on interlaboratory studies carried out by a number of laboratories from European Union and EFTA countries is given. This approach has been designed to improve the analytical state of the art in the determination of selected polycyclic aromatic hydrocarbons in different environmental matrices. The approach resulted in a certification exercise to produce a sewage sludge as Certified Reference Material (CRM). The results of the programme showed that HPLC and GC are equally reliable for PAH analysis at submicrogram to microgram per gram levels in various environmental matrices. Major improvements were achieved during the programme, resulting in reduced coefficients of variation and between-laboratory differences. Several recommendations emerging from the programme experience are presented.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s0021663560041
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  • 8
    Electronic Resource
    Electronic Resource
    BCR: a service to quality assurance in analytical chemistry — some experiences and achievements with regard to reference material preparation (1993)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 346 (1993), S. 530-535 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Despite all efforts to improve the quality of results of measurements, intercomparisons demonstrate a considerable discrepancy. This fact was also shown by many of the round robins organised by the BCR (Commission of the European Communities) on inorganic, speciation, and organic determinations in various environmental matrices. It is clear that further efforts have to be made to improve the state of the art of a wide variety of analyses. This means that the demand for certified reference materials (CRMs) is and will be in constant increase. RMs are required for the validation of methods, for proficiency testing or for training purposes. The production of RMs and CRMs resembling the composition of real matrices poses difficult problems for some compounds and is a challenge for the producers. This paper presents some recent experiences and achievements of the BCR in special cases.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00321237
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  • 9
    Electronic Resource
    Electronic Resource
    Reference materials for PCDD and PCDF analysis: production and verification of the contents of twelve congeners in iso-octane reference solutions (1994)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 348 (1994), S. 31-36 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The Community Bureau of Reference (BCR) of the Commission of the European Communities has produced standard solutions of PCDDs and PCDFs (dirty dozen) to guarantee proper calibration and traceability of results in the certification of these compounds in matrix materials. The purity of each individual isomer has been evaluated on the initial crystals using several analytical methods. Solvents have been checked for impurities. The entire procedure of preparation of the twelve solutions has been performed under strict metrological conditions and will be published elsewhere. All results and the preparation procedure followed are described. The solutions are not certified, but may be obtained from BCR together with an analytical report.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00321601
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  • 10
    Electronic Resource
    Electronic Resource
    Round table discussions outcome and recommendations (1994)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 348 (1994), S. 171-179 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The recommendations of the panel of experts are based on the actual knowledge and the best state of the art available in April 1993. A list of the panel of experts is given in Appendix II; an outline of the Programme in Appendix III.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00321625
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