TY - RPRT A1 - Lehnik-Habrink, Petra A1 - Hein, Sebastian A1 - Philipp, Rosemarie A1 - Nehls, Irene A1 - Win, Tin T1 - Einarbeitung und Validierung von Verfahren zur Bestimmung von polychlorierten Biphenylen und polychlorierten Terphenylen in organischen Materialien N2 - ISBN: Im Zuge der Harmonisierung der Rechtsvorschriften der Mitgliedsstaaten der Europäischen Gemeinschaft wurde im September 1996 die Richtlinie 96/59/EG des Rates über die Beseitigung polychlorierter Biphenyle und polychlorierter Terphenyle (PCB/PCT) verabschiedet. Ziel dieser Richtlinie ist die Angleichung der Rechtsvorschriften der Mitgliedstaaten über die kontrollierte Beseitigung der PCB, die Dekontaminierung oder Beseitigung PCB-haltiger Geräte und die Beseitigung von PCB-Abfall. In der Bundesrepublik Deutschland wurde mit der Verabschiedung der PCB/PCT- Abfallverordnung vom 26. Juni 2000 die EU-Richtlinie umgesetzt. Entsprechend der PCB/PCT-Abfallverordnung wird für PCB-haltigen Abfall ein Grenzwert von 50 mg/kg festgelegt. Beim Haupteinsatzgebiet der PCB - als Isolierflüssigkeiten in Transformatoren - ist die Bestimmung des PCB-Gehaltes durch DIN-Normen geregelt. Polychlorierte Biphenyle wurden auch als Weichmacher in Dichtungsmassen und Kunststoffen, z.B. in Kabelummantelungen, und als Flammschutzmittelanstrich für Holz eingesetzt. Für feste Abfallmatrices gibt es keine verbindliche Prüfvorschrift. Ziel des Projektes war die Erarbeitung und Validierung eines Prüfverfahrens zur Bestimmung von PCB und PCT in organischen Abfallmatrices wie Kabelshredder und Altholz. T3 - BAM Forschungsberichtreihe - 274 PY - 2006 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-1773 SN - 978-3-86509-481-3 SN - 0938-5533 VL - 274 SP - 1 EP - 55 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-177 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schultze, Karin A1 - Philipp, Rosemarie A1 - Redlich, Christel A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Win, Tin A1 - Nehls, Irene T1 - Development, preparation and certification of a reference material for the determination of chlorinated pesticides in soil T2 - Symposium "Reference Materials for Technologies in the New Millenium" CY - Berlin, BAM, Germany DA - 2000-05-22 PY - 2000 SP - 1(?) EP - 4(?) AN - OPUS4-1313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Ermittlung der Messunsicherheit in der organisch-chemischen Analytik - ein Beispiel aus der Praxis T2 - DAP-Sektorkomitee Chemie CY - --- DA - 2000-10-26 PY - 2000 AN - OPUS4-1007 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Retter, Utz T1 - Elektrochemische und massenspektrometrische Untersuchungen zum Abbau von Siloxantensiden im Wasser T2 - ELACH 3 CY - Zeuthen, Germany DA - 1997-09-29 PY - 1997 AN - OPUS4-5673 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Unsicherheitsbudget für Referenzlösungen Ethanol in Waseer T2 - BAM Zirkel "Ergebnisunsicherheit der Abt.I" CY - Berlin, Germany DA - 2001-04-10 PY - 2001 AN - OPUS4-5821 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Ermittlung von Messunsicherheiten in der organisch-chemischen Analytik T2 - DAP-Gutachterschulung des Sektorkomitees Chemie CY - Berlin, Germany DA - 2000-11-26 PY - 2000 AN - OPUS4-5764 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Win, Tin T1 - CCQM-P20 Purity Assessment of Organic Substances - Methods, Results, Uncertainties T2 - OAWG Meeting CY - Beijing, China DA - 2004-10-20 PY - 2004 AN - OPUS4-10835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Win, Tin T1 - CCQM-P61 Analysis of Volatile Organic Compounds in Solution - Methods, Results, Uncertainties T2 - OAWG Meeting CY - Paris, France DA - 2004-04-11 PY - 2004 AN - OPUS4-10836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Win, Tin T1 - CCQM-K40 Analysis of PCB Congeners in Solution - Methods, Results, Uncertainties T2 - OAWG Meeting CY - Paris, France DA - 2005-04-11 PY - 2005 AN - OPUS4-10837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Mechanisms of anodic film formation of organic substances on mercury T2 - Fachkolloquium Institute of Biophysics CY - Brno, Czech Republic DA - 1995-10-18 PY - 1995 AN - OPUS4-5615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Retter, Utz T1 - Keimbildung und -wachstum bei der anodischen Filmbildung organischer Verbindungen an der Quecksilberelektrode T2 - ELACH 3 CY - Zeuthen, Germany DA - 1997-09-29 PY - 1997 AN - OPUS4-5640 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Elektrochemische Messverfahren zur Analyse von Thioharnstoff T2 - Analytica Conference '96 CY - Munich, Germany DA - 1996-04-23 PY - 1996 AN - OPUS4-5667 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hein, Sebastian A1 - Philipp, Rosemarie A1 - Duewer, D.L. A1 - Gasca-Aragon, H. A1 - Lippa, K. A1 - Toman, B. A1 - Bremser, Wolfram A1 - Calderon, M.A.Á. A1 - Castorena, A.P. A1 - Caixeiro, J.M.R. A1 - Do Rego, E.C.P. A1 - Rosso, A. A1 - De Arechavaleta, R. A1 - O'Connor, G. A1 - Holcombe, G. A1 - Ellison, S.L.R. A1 - Splett, J.D. A1 - Schantz, M.M. A1 - Sharpless, K.E. A1 - Croft, M. A1 - Archer, M. A1 - De Vos, J. A1 - Konopelko, L.A. A1 - Kustikov, Y. T1 - Final report on CCQM-K79: Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous matrix N2 - The 2010 CCQM-K79 'Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous media' is the second key comparison directly testing the chemical measurement services provided to customers by National Metrology Institutes (NMIs) and Designated Institutes (DIs). CCQM-K79 compared the assigned ethanol values of proficiency test (PT) and certified reference materials (CRMs) using measurements made on these materials under repeatability conditions. Nine NMIs submitted 27 CRM or value-assigned PT materials for evaluation. These materials represent many of the higher-order reference materials then available for this commercially and forensically important measurand. The assigned ethanol mass fraction in the materials ranged from 0.1 mg/kg to 334 mg/kg. All materials were stored and prepared according the specifications provided by each NMI. Samples were processed and analyzed under repeatability conditions by one analytical team using a gas chromatography with flame ionization detection (GC-FID) method of demonstrated trueness and precision. Given the number of materials and the time required for each analysis, the majority of the measurements were made in two measurement campaigns ('runs'). Due to a shipping delay from one NMI, an unanticipated third campaign was required. In all three campaigns, replicate analyses (three injections of one preparation separated in time) were made for one randomly selected unit of each of the 27 materials. Nine of the 27 materials were gravimetrically diluted before measurement to provide solutions with ethanol mass fraction in the established linear range of the GC-FID method. The repeatability measurement value for each analyzed solution was estimated as the mean of all replicate values. The within- and between-campaign variance components were estimated using one-way ANOVA. Markov Chain Monte Carlo Bayesian analysis was used to estimate 95% level-of-confidence coverage intervals for the mean values. Uncertainty-weighted generalized distance regression was used to establish the key comparison reference function (KCRF) relating the assigned values to the repeatability measurements. On the basis of leave-one-out cross-validation, all of the assigned values for all 27 materials were deemed equivalent at the 95% level of confidence. These materials were used to define the KCRF. Parametric bootstrap Monte Carlo was used to estimate 95% level-of-confidence coverage intervals for the degrees of equivalence of materials, d ± U95(d), and of the participating NMIs, D ± U95(D). Because of the very wide range of ethanol mass fraction in the materials, these degrees of equivalence are expressed in percent relative form: %d ± U95(%d) and %D ± U95(%D). The median of the absolute values of the %D for the participating NMIs is less than 0.05% with a median U95(%D) of less than 1%. These results demonstrate that the participating NMIs have the ability to correctly value-assign CRMs and proficiency test materials for ethanol in aqueous media and similar measurands. PY - 2013 U6 - https://doi.org/10.1088/0026-1394/50/1A/08005 SN - 0026-1394 SN - 1681-7575 VL - 50 IS - 1A / Technical Suppl. 2013 / 08005 SP - 1 EP - 49 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-27730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Piechotta, Christian A1 - Fettig, Ina T1 - Primary methods for emerging pollutants and their transformation products T2 - EURAMET TC-MC Meeting CY - Braunschweig, Germany DA - 2013-02-07 PY - 2013 AN - OPUS4-27719 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sturgeon, R. E. A1 - Wahlen, R. A1 - Brandsch, T. A1 - Fairman, B. A1 - Wolf-Briche, C. A1 - Alonso, J. I. G. A1 - González, P. R. A1 - Encinar, J. R. A1 - Sanz-Medel, A. A1 - Inagaki, K. A1 - Takatsu, A. A1 - Lalere, B. A1 - Monperrus, M. A1 - Zuloaga, O. A1 - Krupp, E. A1 - Amouroux, D. A1 - Donard, O. F. X. A1 - Schimmel, H. A1 - Sejeroe-Olsen, B. A1 - Konieczka, P. A1 - Schultze, P. A1 - Taylor, P. A1 - Hearn, R. A1 - Mackay, L. A1 - Myors, R. A1 - Win, Tin A1 - Liebich, Almuth A1 - Philipp, Rosemarie A1 - Yang, L. A1 - Willie, S. T1 - Determination of tributyltin in marine sediment: Comité Consultatif pour la Quantité de Matière (CCQM) pilot study P-18 international intercomparison N2 - The capabilities of National Metrology Institutes (NMIs—those which are members of the Comité Consultatif pour la Quantité de Matière (CCQM)of the CIPM) and selected outside "expert" laboratories to quantitate (C4H9)3Sn+ (TBT) in a prepared marine sediment were assessed. This exercise was sanctioned by the 7th CCQM meeting, April 4–6, 2001, as an activity of the Inorganic Analysis Working Group and was jointly piloted by the Institute for National Measurement Standards of the National Research Council of Canada (NRC) and the Laboratory of the Government Chemist (LGC), UK. A total of 11 laboratories submitted results (7 NMIs, and 4 external labs). Two external laboratories utilized a standard calibration approach based on a natural abundance TBT standard, whereas all NMIs relied upon isotope dilution mass spectrometry for quantitation. For this purpose, a species specific 117Sn-enriched TBT standard was supplied by the LGC. No sample preparation methodology was prescribed by the piloting laboratories and, by consequence, a variety of approaches was adopted by the participants, including mechanical shaking, sonication, accelerated solvent extraction, microwave assisted extraction and heating in combination with Grignard derivatization, ethylation and direct sampling. Detection techniques included ICP–MS (with GC and HPLC sample introduction), GC–MS, GC–AED and GC–FPD. Recovery of TBT from a control standard (NRCC CRM PACS-2 marine sediment) averaged 93.5±2.4% (n=14). Results for the pilot material averaged 0.680±0.015 µmol kg–1 (n=14; 80.7±1.8 µg kg–1) with a median value of 0.676 µmol kg–1. Overall, performance was substantially better than state-of-the-art expectations and the satisfactory agreement amongst participants permitted scheduling of a follow-up Key comparison for TBT (K-28), a Pilot intercomparison for DBT (P-43), and certification of the test sediment for TBT content and its release as a new Certified Reference Material (HIPA-1) with a TBT content of 0.679±0.089 µmol kg–1 (expanded uncertainty, k=2, as Sn) (80.5±10.6 µg kg–1). Electronic Supplementary Material Supplementary material is available in the online version of this article at http://dx.doi.org/10.1007/s00216-003-2016-9. KW - Tributyltin KW - Marine sediment KW - International intercomparison PY - 2003 U6 - https://doi.org/10.1007/s00216-003-2016-9 SN - 1618-2642 SN - 1618-2650 VL - 376 IS - 6 SP - 780 EP - 787 PB - Springer CY - Berlin AN - OPUS4-10905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Hanebeck, Olaf A1 - Töpfer, Antje A1 - Win, Tin A1 - Nehls, Irene T1 - High precision measurement for quality control of the CRM ethanol in water T2 - BERM 9 - 9th International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 2003-06-15 PY - 2003 AN - OPUS4-4791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, Ina A1 - Piechotta, Christian A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert T1 - Tributylzinn in Gesamtwasserproben - Entwicklung eines Referenzverfahrens für die EU-Wasserrahmenrichtlinie PY - 2013 SN - 0016-3538 IS - 9 SP - 2 EP - 4 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-29040 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Cabillic, J. A1 - Emteborg, H. A1 - Fettig, Ina A1 - Gonzales-Gago, A. A1 - Petrov, Panayot A1 - Rodriguez Cea, A A1 - Swart, C. T1 - ENV08 Traceable measurements for monitoring critical pollutants under the European Water Framework Directive T2 - EMRP Mid-term Review Conference CY - Teddington, England DA - 2013-10-21 PY - 2013 AN - OPUS4-29531 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philipp, Rosemarie A1 - Schantz, M. A1 - Urquiza, M.P. A1 - Calderón, M.A.A. A1 - Torres, M.M. A1 - Carter, D. A1 - O'Connor, G. A1 - Sejeroe-Olsen, B. A1 - Ricci, M. A1 - Lalere, B. A1 - Peignaux, M. A1 - Kim, D.-H. A1 - Itoh, N. A1 - Wong, S.-K. A1 - Man, T.O. A1 - Caixeiro, J.M.R. T1 - CCQM-K50: Polycyclic aromatic hydrocarbons (PAHs) in soil/particulate matter PY - 2010 U6 - https://doi.org/10.1088/0026-1394/47/1A/08006 SN - 0026-1394 SN - 1681-7575 VL - 47 SP - 08006-1 - 08006-47 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-20821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philipp, Rosemarie A1 - Hanebeck, Olaf A1 - Hein, Sebastian A1 - Bremser, Wolfram A1 - Win, Tin A1 - Nehls, Irene T1 - Ethanol/water solutions as certified reference materials for breath alcohol analyzer calibration N2 - The Federal Institute for Materials Research and Testing (BAM), Germany, has issued a series of large volume ethanol in water certified reference materials (CRMs), primarily developed for the calibration of evidential breath alcohol analyzers in Germany. The certified parameter is the ethanol mass concentration at 20 °C. When used in a wet bath simulator, the solutions deliver gas samples that meet the requirements set by the Organization of Legal Metrology for calibration of breathalyzers. The materials were prepared gravimetrically by spiking of ethanol into water in single 5 L units. A complete uncertainty budget for the preparation process has been established. The purity of the commercial ethanol stock solution was identified to be the main source of uncertainty. For stability and homogeneity measurements and for the verification of the gravimetric mass concentration of the CRMs, a robust high-precision gas chromatography, with flame-ionization detection method for ethanol determination in aqueous samples was developed and validated. The good performance of this method has been demonstrated in several international comparisons organized by the Consultative Committee for Amount of Substance-Metrology in Chemistry at the International Bureau of Weights and Measures. KW - Certified reference material KW - Ethanol in water KW - Breath alcohol KW - GC-FID PY - 2010 U6 - https://doi.org/10.1007/s00769-009-0605-9 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 3 SP - 141 EP - 146 PB - Springer CY - Berlin AN - OPUS4-20999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Duewer, D.L. T1 - Comparison of Value-Assigned CRMs and PT MAterials for Ethanol in Aqeous Matrix T2 - CCQM Organic Analysis Working Group Meeting CY - Paris, France DA - 2010-04-13 PY - 2010 AN - OPUS4-21168 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Mesquida, C. A1 - Wielgosz, R. A1 - Rosso, A. A1 - de Arechavaleta, M.R. A1 - Davies, S. A1 - Wang, H. A1 - do Rego, E.C.P. A1 - Rodrigues, J.M. A1 - de Freitas Guimaraes, E. A1 - Sousa, M.V.B. A1 - Monteiro, T.M. A1 - das Neves Valente, L.A. A1 - Violante, F.G.M. A1 - Almeida, R. R. R. A1 - Quaresma, M.C.B. A1 - Nogueira, R. A1 - Windust, A. A1 - Dai, X. A1 - Li, X. A1 - Zhang, W. A1 - Li, M. A1 - Shao, M. A1 - Wei, C. A1 - Wong, S.-K. A1 - Cabillic, J. A1 - Gantois, F. A1 - Philipp, Rosemarie A1 - Pfeifer, Dietmar A1 - Hein, Sebastian A1 - Klyk-Seitz, Urszula-Anna A1 - Ishikawa, K. A1 - Castro, E. A1 - Gonzalez, N. A1 - Krylov, A. A1 - Lin, T.T. A1 - Kooi, L.T. A1 - Fernandes-Whaley, M. A1 - Prévoo, D. A1 - Archer, M. A1 - Visser, R. A1 - Nlhapo, N. A1 - de Vos, B. A1 - Ahn, S. A1 - Pookrod, P. A1 - Wiangnon, K. A1 - Sudsiri, N. A1 - Muaksang, K. A1 - Cherdchu, C. A1 - Gören, A.C. A1 - Bilsel, M. A1 - LeGoff, T. A1 - Bearden, D. A1 - Bedner, M. A1 - Duewer, D. A1 - Hancock, D. A1 - Lang, B. A1 - Lippa, K. A1 - Schantz, M. A1 - Sieber, j. T1 - Final report on key comparison CCQM-K55.b (aldrin): An international comparison of mass friction purity assignment of aldrin N2 - Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.b, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2010/2011. Nineteen national measurement institutes and the BIPM participated. Participants were required to assign the mass fraction of aldrin present as the main component in the comparison sample for CCQM-K55.b which consisted of technical grade aldrin obtained from the National Measurement Institute Australia that had been subject to serial recrystallization and drying prior to sub-division into the units supplied for the comparison. Aldrin was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molar mass range 300 Da to 500 Da] and low polarity (pKOW < -2) for which related structure impurities can be quantified by capillary gas phase chromatography (GC). The key comparison reference value (KCRV) for the aldrin content of the material was 950.8 mg/g with a combined standard uncertainty of 0.85 mg/g. The KCRV was assigned by combination of KCRVs assigned by consensus from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 0.3% to 0.6% using a mass balance approach and 0.5% to 1% using a qNMR method. The major analytical challenge posed by the material proved to be the detection and quantification of a significant amount of oligomeric organic material within the sample and most participants relying on a mass balance approach displayed a positive bias relative to the KCRV (overestimation of aldrin content) in excess of 10 mg/g due to not having adequate procedures in place to detect and quantify the non-volatile content–specifically the non-volatile organics content–of the comparison sample. There was in general excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content and the residual solvent content of the sample. The comparison demonstrated the utility of 1H NMR as an independent method for quantitative analysis of high purity compounds. In discussion of the participant results it was noted that while several had access to qNMR estimates for the aldrin content that were inconsistent with their mass balance determination they decided to accept the mass balance result and assumed a hidden bias in their NMR data. By contrast, laboratories that placed greater confidence in their qNMR result were able to resolve the discrepancy through additional studies that provided evidence of the presence of non-volatile organic impurity at the requisite level to bring their mass balance and qNMR estimates into agreement. PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08014 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - CCQM-K55.b Final Report October 2012 SP - 1 EP - 41 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-26831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Riedel, Juliane A1 - Proske, Matthias A1 - Hein, Sebastian A1 - Koch, Matthias T1 - CCQM-K95 Mid-polarity pesticides in tea, BAM methods and results T2 - CCQM, OAWG Meeting CY - Paris, France DA - 2012-04-16 PY - 2012 AN - OPUS4-25858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Daireaux, A. A1 - Wielgosz, R. A1 - Davies, S. A1 - Wang, H. A1 - Rodrigues, J. A1 - Wollinger, W. A1 - Windust, A. A1 - Kang, M. A1 - Fuhai, S. A1 - Philipp, Rosemarie A1 - Kuhlich, Paul A1 - Wong, S.-K. A1 - Shimizu, Y. A1 - Pérez, M. A1 - Avila, M. A1 - Fernandes-Whaley, M. A1 - Prevoo, D. A1 - de Vos, J. A1 - Visser, R. A1 - Archer, M. A1 - LeGoff, T. A1 - Wood, S. A1 - Bearden, D. A1 - Bedner, M. A1 - Boroujerdi, A. A1 - Duewer, D. A1 - Hancock, D. A1 - Lang, B. A1 - Porter, B. A1 - Schantz, M. A1 - Sieber, J. A1 - White, E. A1 - Wise, S. A. T1 - Final report on key comparison CCQM-K55.a (estradiol): an international comparison of mass fraction purity assignment of estradiol N2 - Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.a, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2009/2010. Eleven national measurement institutes and the BIPM participated. Participants were required to assign the mass fraction of estradiol present as the main component in the comparison sample (CCQM-K55.a) which consisted of a bulk estradiol hemihydrate material obtained from a commercial supplier that had been extensively but not exhaustively dried prior to sub-division into the units supplied for the comparison. Estradiol was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molar mass range 300–500 Da] and low polarity (pKOW < -2) for which related structure impurities can be quantified by capillary gas phase chromatography (GC) or by high performance liquid chromatography (LC). The majority of participants used a mass balance approach to determine the estradiol content. The key comparison reference value (KCRV) for estradiol in CCQM-K55.a was assigned by combination of KCRVs assigned by consensus from participant results for each orthogonal impurity class. This allowed participants to demonstrate the efficacy (or otherwise) of their implementation of the mass balance approach and to demonstrate that their assigned value for the main component agreed with the KCRV through use of internally consistent contributing methods. The KCRV for the estradiol content of the material was 984.3 mg/g with a combined standard uncertainty of 0.42 mg/g. The individual participant results showed that a relative expanded uncertainty for the purity assignment of 0.2% is a reasonable estimate of the best achievable result by an individual laboratory for a material of this complexity available in this amount at this level of purity. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 0.2% to 0.8%. The review of results that were biased from the KCRV showed that two major analytical challenges are posed by the material: the measurement of its water content and controlling for related substance artefact formation during the analysis process. The results displaying a positive bias relative to the KCRV (overestimation of estradiol content) were due to underestimation of the water content of the material, while those with a negative bias (underestimation of estradiol) overestimated the total related substance impurities through a failure to detect and control for artefact formation arising from in situ oxidative dimerization of estradiol in neutral solution prior to analysis. There was however good agreement between all participants in the identification and the quantification of the individual related structure impurities actually present in the sample. The comparison also demonstrated the utility of high-field 1H NMR for both quantitative and qualitative analysis of high purity compounds. It is noted that all the participants who used qNMR as a major or contributing technique and included it as part of, combined it or confirmed it with a conventional 'mass balance' data estimate, obtained results consistent with the KCRV. PY - 2012 U6 - https://doi.org/10.1088/0026-1394/49/1A/08009 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 1A Tech. Suppl. / 08009 SP - 1 EP - 33 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-26411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Fettig, Ina A1 - Hein, Sebastian A1 - Swart, C. A1 - Petrov, Panayot A1 - Cabillic, J. A1 - Emteborg, H. T1 - ENV08 WFD Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD 2000/60/EC) T2 - EURAMET TC-MC Meeting CY - Teddington, England DA - 2014-02-05 PY - 2014 AN - OPUS4-30160 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. T1 - EURAMET.QM-S14 Measurement capabilities for the quantification of ethanol in water N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value (KCRV) are discussed. A Bayesian approach is finally used to estimate the KCRV and the degrees of equivalence of participants. T2 - EURAMET TC-MC Sector Committee Bio- and Organic Analysis Meeting CY - Online meeting DA - 02.02.2021 KW - Certified reference material KW - EMPIR project KW - Interlaboratory comparison PY - 2021 AN - OPUS4-52615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. A1 - Sánchez, C. A1 - Sáez, A. A1 - Bebić, J. A1 - Banjanac, K. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Claramunt, A. V. A1 - Janko, P. A1 - Jotanovic, A. A1 - Hafner-Vuk, K. A1 - Buzoianu, M. A1 - Mihail, R. A1 - Fernández, M. M. A1 - Etcheverry, J. A1 - Mbithi Muendo, B. A1 - Muriira Karau, G. A1 - Silva, A. A1 - Almirón, F. A1 - Marajh, D. A1 - Makgatho, P. A1 - Visser, R. A1 - Alaskar, A. R. A1 - Alosaimi, A. A1 - Alrashed, M. A1 - Yılmaz, H. A1 - Ün, İ. A1 - Gündüz, S. A1 - Topal, K. A1 - Bilsel, M. A1 - Karasinski, J. A1 - Torres, J. T1 - Supplementary comparison study - measurement capabilities for the quantification of ethanol in water N2 - The accurate quantification of ethanol in water is essential for forensic applications such as blood and breath alcohol testing and for commercial applications such as the assessment of alcoholic beverages. The intercomparison EURAMET.QM-S14 is part of a capacity building project named ALCOREF “Certified forensic alcohol reference materials” that is running within the European Metrology Programme for Innovation and Research (EMPIR). The intercomparison should allow project partners and other interested National Metrology Institutes (NMIs) and Designated Institutes (DIs) to benchmark their analytical methods for the quantification of ethanol in water. The study plan was agreed by the European Association of National Metrology Institutes (EURAMET) Subcommittee Bio- and Organic Analysis (SCBOA) and the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) in February and April 2019, respectively. The intercomparison was coordinated by BAM. Two concentration levels relevant for the calibration and verification of evidential breath alcohol analysers were distributed to study participants. Fifteen institutes from 15 countries registered for the intercomparison and returned results. Participants mostly applied gas chromatography with flame ionisation detection (GC-FID) or mass spectroscopy (GC-MS), one participant used titrimetry and one participant employed a test bench for breath analyser calibration (“bubble train”). Participants did either in-house purity assessment of their commercial ethanol calibrants by Karl-Fischer titration, chromatographic methods, quantitative nuclear magnetic resonance spectroscopy (qNMR) and/or density measurements; or they used ethanol/water Certified Reference Materials (CRMs) from NMIs/DIs for calibration. CCQM OAWG agreed to use a consensus value from participants results that utilizes the reported uncertainties as Key Comparison Reference Value (KCRV). The Gaussian Random effects model with Hierarchical Bayesian solution (HB-REM) is a reasonable approach in this case. The KCRVs and Degrees of Equivalence (DoEs) were calculated with the NIST consensus builder version 1.2 Hierarchical Bayes procedure. Successful participation in the interlaboratory comparison has demonstrated the capabilities in determining the mass fraction of ethanol in aqueous matrices in the range 0.1 mg/g to 8 mg/g. Fourteen out of 15 participants have successfully quantified both samples, one participant successfully quantified only the lower-level (0.6 mg/g) sample. KW - Certified reference material KW - EURAMET KW - EMPIR KW - ALCOREF KW - Ethanol in water KW - Supplementary comparison PY - 2022 U6 - https://doi.org/10.1088/0026-1394/59/1A/08015 VL - 59 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-55889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, I. A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Fisicaro, P. A1 - Alasonati, E. T1 - Determination of tributyltin in whole water matrices under the European water framework directive N2 - Monitoring of water quality is important to control water pollution. Contamination of the aquatic systemhas a large effect on human health and the environment. Under the European Water Framework Directive(WFD) 2000/60/EC and the related directive on environmental quality standards (EQS) in the field of waterpolicy 2008/105/EC, the need for sensitive reference methods was highlighted. Since tributyltin (TBT) isone of the WFD listed priority substances a method was developed which is capable to qualify and quantifythe pollutant at the required low WFD EQS of 0.2 ng L⁻¹ in whole water bodies, i.e. in non-filtered watersamples with dissolved organic carbon and suspended particulate matter. Therefore special attention waspaid on the interaction of TBT with the suspended particulate matter and humic substances to obtain acomplete representation of the pollution in surface waters. Different water samples were investigatedvarying the content of organic dissolved and suspended matter. Quantification was performed usingspecies-specific isotope dilution (SSID) and gas chromatography with inductively coupled plasma massspectrometry (GC-ICP-MS). Different sample treatment strategies were evaluated and compared. Theprocess of internal standard addition was investigated and optimized, hence the equilibrium betweeninternal standards and matrix is of primary importance to perform accurate SSID. Samples spiked at EQSlevel were analyzed with a recovery between 95 and 105 %. Additionally real surface water samples wereinvestigated and the TBT concentration for the whole water body was determined and compared withconventional routine analysis method. KW - Tributyltin (TBT) KW - Environmental quality standard (EQS) KW - Isotope dilution KW - Humic acid KW - Surface water KW - Suspended particulate matter PY - 2016 U6 - https://doi.org/10.1016/j.chroma.2016.06.068 SN - 0021-9673 VL - 1459 SP - 112 EP - 119 AN - OPUS4-36930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Kotzeva, B. A1 - Bim, S. A1 - Alasonati, E. A1 - Fisicaro, P. T1 - Development of an analytical method for TBT speciation in coastal lyes and sea water (Pomorie Lake, Black Sea, Bulgaria) T2 - 38th International Symposium on Environmental Analytical Chemistry CY - Lausanne, Schweiz DA - 2014-06-17 PY - 2014 AN - OPUS4-31857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Urquiza, M.P. A1 - Torres, M.M. A1 - Mitani, Y. A1 - Schantz, M.M. A1 - Duewer, D.L. A1 - May, W.E. A1 - Parris, R.M. A1 - Wise, S. A. A1 - Kaminski, Katja A1 - Philipp, Rosemarie A1 - Win, Tin A1 - Rosso, A. A1 - Kim, D.H. A1 - Ishikawa, K. A1 - Krylov, A.I. A1 - Kustikov, Y.A. A1 - Baldan, A. T1 - Final report on CCQM-K47: Volatile organic compounds in methanol N2 - KEY COMPARISON At the October 2005 CCQM Organic Analysis Working Group Meeting (IRMM, Belgium), the decision was made to proceed with a Key Comparison study (CCQM-K47) addressing the calibration function for the determination of volatile organic compounds (VOCs) used for water quality monitoring. This was coordinated by CENAM and NIST. Benzene, o-xylene, m-xylene and p-xylene were chosen as representative VOCs. The solvent of choice was methanol. Key Comparison CCQM-K47 demonstrated the capabilities of participating NMIs to identify and measure the four target VOCs in a calibration solution using GC-based methods. The measurement challenges in CCQM-K47, such as avoiding volatility loss, achieving adequate chromatographic resolution and isolating potential interferences, are typical of those required for value-assigning volatile reference materials. Participants achieving comparable measurements for all four VOCs in this Key Comparison should be capable of providing reference materials and measurements for VOCs in solutions when present at concentration levels greater than 10 µg/g. PY - 2013 U6 - https://doi.org/10.1088/0026-1394/50/1A/08021 SN - 0026-1394 SN - 1681-7575 VL - 50 SP - 08021, 1 EP - 24 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-31071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Schiel, D. A1 - Cabilic, J. A1 - Goenaga-Infante, H. A1 - Emteborg, H. A1 - Buzoianu, M. A1 - Milacic, R. A1 - Sainio, P. A1 - Cankur, O. A1 - Duffek, A. A1 - Pröfrock, D. A1 - Win, Tin A1 - Piechotta, Christian A1 - Nehls, Irene A1 - Panne, Ulrich T1 - Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC T2 - EMRP Review Conference CY - Budapest, Hungary DA - 2010-11-22 PY - 2010 AN - OPUS4-22422 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Cabillic, J. A1 - Schiel, D. A1 - Ernteborg, H. A1 - Goenaga-Infante, H. A1 - LAlere, B. T1 - Joint Research Project ENV08 "Traceable Measurements for Monitoring Critical Pollutants under the European Water Framework Directive (WFD) 2000/60/EC" T2 - 15th International Congress of Metrology CY - Paris, France DA - 2011-10-03 PY - 2011 AN - OPUS4-24123 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D.L. A1 - May, W.E. A1 - Parris, R.M. A1 - Schantz, M.M. A1 - Wise, S. A. A1 - Piechotta, Christian A1 - Philipp, Rosemarie A1 - Win, Tin A1 - Avila, M. A1 - Pérez Urquiza, M. A1 - Ulberth, F. A1 - Kim, B. A1 - Ishikawa, K. A1 - Chen, D. A1 - Krylov, A.I. A1 - Kustidov, Y.A. A1 - Lopushanskaya, E.M. T1 - Final report on CCQM-K38: Determination of PAHs in solution PY - 2009 U6 - https://doi.org/10.1088/0026-1394/46/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 46 IS - 08003 SP - 1 EP - 13 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-20029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Daireaux, A. A1 - Wielgosz, R. A1 - Davies, S. A1 - Kang, M. A1 - Ting, H. A1 - Philipp, Rosemarie A1 - Malz, Frank A1 - Shimizu, Y. A1 - Frias, E. A1 - Pérez, M. A1 - Apps, P. A1 - Fernandes-Whaley, M. A1 - De Vos, B. A1 - Wiagnon, K. A1 - Ruangrittinon, N. A1 - Wood, S. A1 - Duewer, D.L. A1 - Schantz, M.M. A1 - Bedner, M. A1 - Hancock, D. A1 - Esker, J. T1 - An international comparison of mass fraction purity assignment of theophylline: CCQM pilot study CCQM-P20.e (Theophylline) PY - 2009 U6 - https://doi.org/10.1088/0026-1394/46/1A/08019 SN - 0026-1394 SN - 1681-7575 VL - 46 IS - 08019 SP - 1 EP - 37 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-20030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Elordui-Zapatarietxe, S. A1 - Fettig, Ina A1 - Philipp, Rosemarie A1 - Gantois, F. A1 - Lalère, B. A1 - Swart, C. A1 - Petrov, P. A1 - Goenaga-Infante, H. A1 - Vanermen, G. A1 - Boom, G. A1 - Emteborg, H. T1 - Novel concepts for preparation of reference materials as whole water samples for priority substances at nanogram-per-liter level using model suspended particulate matter and humic acids N2 - One of the unresolved issues of the European Water Framework Directive is the unavailability of realistic water reference materials for the organic priority pollutants at low nanogram-per-liter concentrations. In the present study, three different types of ready-to-use water test materials were developed for polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) at nanogram-per-liter levels. The first type simulated the dissolved phase in the water and comprised of a solution of humic acids (HA) at 5 mg L-1 dissolved organic carbon (DOC) and a spike of the target compounds. The second type of water sample incorporated the particulate phase in water. To this end, model suspended particulate matter (SPM) with a realistic particle size was produced by jet milling soil and sediments containing known amounts of PAHs, PBDEs and TBT and added as slurry to mineral water. The most complex test materials mimicked 'whole water' consequently containing both phases, the model SPM and the HA solution with the target analytes strongly bound to the SPM. In this paper, the development of concepts, processing of the starting materials, characterisation of the HA and model SPMs as well as results for homogeneity and stability testing of the ready-to-use test materials are described in detail. KW - Slurry KW - PBDE KW - PAH KW - TBT KW - Reference materials KW - Suspended particulate matter KW - Whole water KW - Water Framework Directive PY - 2015 U6 - https://doi.org/10.1007/s00216-014-8349-8 SN - 1618-2642 SN - 1618-2650 VL - 407 IS - 11 SP - 3055 EP - 3067 PB - Springer CY - Berlin AN - OPUS4-33087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Fettig, Ina A1 - Richter, Janine A1 - Piechotta, Christian A1 - Elordui-Zapatarietxe, S. A1 - Emteborg, H. A1 - Swart, C. A1 - Cabilic, J. A1 - Alasonati, E. T1 - Reference methods and materials for European water ligistlation T2 - Anakon 2015 CY - Graz, Austria DA - 2015-03-23 PY - 2015 AN - OPUS4-33646 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, Ina A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert T1 - Tributyltin - critical pollutant in whole water samples - development of traceable measurement methods for monitoring under the European water framework directive (WFD) 2000/60/EC N2 - Tributyltin is listed as one of the priority substances in the European Water Framework Directive (WFD). Despite its decreasing input in the environment, it is still present and has to be monitored. In the European Metrology Research Programme project ENV08, a sensitive and reliable analytical method according to the WFD was developed to quantify this environmental pollutant at a very low limit of quantification. With the development of such a primary reference method for tributyltin, the project helped to improve the quality and comparability of monitoring data. An overview of project aims and potential analytical tools is given. KW - Tributyltin KW - European Water Framework Directive KW - Whole water body KW - Reference method PY - 2015 U6 - https://doi.org/10.1007/s11356-015-4614-4 SN - 0944-1344 SN - 1614-7499 VL - 22 IS - 13 SP - 9589 EP - 9594 PB - Springer CY - Berlin; Heidelberg AN - OPUS4-33734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alasonati, E. A1 - Fabbri, B. A1 - Fettig, Ina A1 - Yardin, C. A1 - Del Castillo Busto, M.E. A1 - Richter, Janine A1 - Philipp, Rosemarie A1 - Fisicaro, P. T1 - Experimental design for TBT quantification by isotope dilution SPE-GC-ICP-MS under the European water framework directive N2 - In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L-1 in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP–MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250–1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the experimental conditions are drawn. This work shows that SPE is a convenient technique for TBT pre-concentration at pico-trace levels and a robust approach: in fact (i) number of different experimental conditions led to satisfactory results and (ii) the participation of two institutes to the experimental work did not impact the developed model. KW - Tributyltin KW - Organotin compounds KW - Solid-phase extraction KW - Experimental design KW - Water framework directive KW - Isotope dilution PY - 2015 U6 - https://doi.org/10.1016/j.talanta.2014.11.064 SN - 0039-9140 VL - 134 SP - 576 EP - 586 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-32696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Philipp, Rosemarie T1 - Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC N2 - The European Water Framework Directive (WFD) 2000/60/EC specifies a list of 33 priority water pollutants. For these substances, Environmental Quality Standards (EQS), equivalent to the maximum allowable concentrations, had been defined at very low levels. EQS values refer to the whole water body, i.e. include contaminants which are associated to suspended solids or colloids present in the natural water. For several priority pollutants primary analytical methods capable of measuring the target analytes at EQS level in natural water are still missing. The project has developed and validated such methods for three selected compounds, namely Tributyltin (TBT), Polybrominated Diphenylether (PBDE) and Polycyclic Aromatic Hydrocarbons (PAH). KW - Water polluntants KW - Monitoring KW - Water analysis KW - Tributyltin KW - Polybrominated diphenylether KW - Polycyclic aromatic hydrocarbons PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-386230 SP - 1 EP - 3 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alasonati, E. A1 - Fettig, I. A1 - Richter, Janine A1 - Philipp, Rosemarie A1 - Milačič, R. A1 - Sčančar, J. A1 - Zuliani, T. A1 - Tunç, M. A1 - Bilsel, M. A1 - Gören, A. A1 - Fisicaro, P. T1 - Towards tributyltin quantification in natural water at the Environmental Quality Standard level required by the Water Framework Directive N2 - The European Union (EU) has included tributyltin (TBT) and its compounds in the list of priority water pollutants. Quality standards demanded by the EU Water Framework Directive (WFD) require determination of TBT at so low concentration level that chemical analysis is still difficult and further research is needed to improve the sensitivity, the accuracy and the precision of existing methodologies. Within the frame of a joint research project “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive” in the European Metrology Research Programme (EMRP), four metrological and designated institutes have developed a primary method to quantify TBT in natural water using liquid–liquid extraction (LLE) and species-specific isotope dilution mass spectrometry (SSIDMS). The procedure has been validated at the Environmental Quality Standard (EQS) level (0.2 ng L−1 as cation) and at the WFD-required limit of quantification (LOQ) (0.06 ng L−1 as cation). The LOQ of the methodology was 0.06 ng L−1 and the average measurement uncertainty at the LOQ was 36%, which agreed with WFD requirements. The analytical difficulties of the method, namely the presence of TBT in blanks and the sources of measurement uncertainties, as well as the interlaboratory comparison results are discussed in detail. KW - Tributyltin KW - Water Framework Directive KW - Metrological traceability KW - ICP-MS KW - Isotope dilution PY - 2016 U6 - https://doi.org/10.1016/j.talanta.2016.07.056 SN - 0039-9140 SN - 1873-3573 VL - 160 SP - 499 EP - 511 PB - Elsevier B.V. AN - OPUS4-37407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Certified forensic alcohol reference materials N2 - The poster presents a project proposal for the production and certification of ethanol/water reference materials suitable for the calibration and type approval of breath alcohol analysers. T2 - EURAMET EMPIR Research Potential Review Conference 2016 CY - Rotterdam, The Netherlands DA - 23.11.2016 KW - Reference material KW - Breath alcohol analyser KW - Interlaboratory comparison PY - 2016 AN - OPUS4-38455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - 16RPT02 ALCOREF - Certified forensic alcohol reference materials N2 - The presentation shows the outline of a new project on certified reference materials for the calibration of evidential breath alcohol analyzers in the 2016 EMPIR Research Potential call. T2 - EURAMET TC-MC Meeting CY - Warsaw, Poland DA - 31.01.2017 KW - Breath alcohol KW - Certified reference material KW - EMPIR PY - 2017 AN - OPUS4-39158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Stoppacher, N. A1 - Wielgosz, R. A1 - Davies, S. A1 - do Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - Lima, J. A1 - Oliveira, R. A1 - de Sena, R. A1 - Windust, A. A1 - Huang, T. A1 - Dai, X. A1 - Quan, C. A1 - He, H. A1 - Zhang, W. A1 - Wei, C. A1 - Li, N. A1 - Gao, D. A1 - Liu, Z. A1 - Lo, M. A1 - Wong, W. A1 - Pfeifer, Dietmar A1 - Koch, Matthias A1 - Dorgerloh, Ute A1 - Rothe, Robert A1 - Philipp, Rosemarie A1 - Hanari, N. A1 - Rezali, M. A1 - Arzate, C. A1 - Berenice, M. A1 - Caballero, V. A1 - Osuna, M. A1 - Krylov, A. A1 - Kharitonov, S. A1 - Lopushanskaya, E. A1 - Liu, Q. A1 - Lin, T. A1 - Fernandes-Whaley, M. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Prevoo-Franzsen, D. A1 - Archer, M. A1 - Kim, B. A1 - Baek, S. A1 - Lee, S. A1 - Lee, J. A1 - Marbumrung, S. A1 - Kankaew, P. A1 - Chaorenpornpukdee, K. A1 - Chaipet, T. A1 - Shearman, K. A1 - Gören, A. A1 - Gündüz, S. A1 - Yilmaz, H. A1 - Un, I. A1 - Bilsel, G. A1 - Clarkson, C. A1 - Bedner, M. A1 - Camara, J. A1 - Lang, B. A1 - Lippa, K. A1 - Nelson, M. A1 - Toman, B. A1 - Yu, L. T1 - Mass fraction assignment of folic acid in a high purity material - CCQM-K55.d (Folic acid) Final Report N2 - The comparison required the assignment of the mass fraction of folic acid present as the main component in the comparison sample. Performance in the comparison is representative of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molecular weight range 300–500] and high polarity (pKOW < −2). Methods used by the eighteen participating NMIs or DIs were based on a mass balance (summation of impurities) or qNMR approach, or the combination of data obtained using both methods. The qNMR results tended to give slightly lower values for the content of folic acid, albeit with larger associated uncertainties, compared with the results obtained by mass balance procedures. Possible reasons for this divergence are discussed in the report, without reaching a definitive conclusion as to their origin. The comparison demonstrates that for a structurally complex polar organic compound containing a high water content and presenting a number of additional analytical challenges, the assignment of the mass fraction content property value of the main component can reasonably be achieved with an associated relative standard uncertainty in the assigned value of 0.5% KW - CCQM key comparison KW - Purity assessment KW - Folic acid PY - 2018 UR - https://www.bipm.org/utils/common/pdf/final_reports/QM/K55/CCQM-K55.d.pdf U6 - https://doi.org/10.1088/0026-1394/55/1A/08013 VL - 55 IS - Technical Supplement, 2018 SP - 08013, 1 EP - 38 PB - Institute of Physics Publishing (IOP) ; Bureau International des Poids et Mesures AN - OPUS4-44999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. T1 - EMPIR Project ALCOREF - Proposal for EURAMET SCOA intercomparisons N2 - The talk presents a short summary of the EMPIR Project ALCOREF "Certified forensic alcohol reference materials". An interlaboratory comparison of analytical methods for the quantification of ethanol in water and a comparison of certified ethanol in water reference materials are proposed. T2 - CCQM Organic Analysis Working Group Meeting CY - Paris, France DA - 08.04.2019 KW - Certified reference material KW - EMPIR KW - EURAMET PY - 2019 AN - OPUS4-47988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EURAMET.QM-S14 Measurement capabilities for the quantification of ethanol in water - Summary of results N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value are discussed. T2 - CCQM Organic Analysis Working Group videoconference CY - Online meeting DA - 05.06.2020 KW - Certified Reference Material KW - EURAMET KW - Key comparison PY - 2020 AN - OPUS4-50890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Elordui-Zapatarietxe, S. A1 - Fettig, Ina A1 - Richter, Janine A1 - Philipp, Rosemarie A1 - Vanermen, G. A1 - Monteyne, E. A1 - Boom, G. A1 - Emteborg, H. T1 - Preparation and evaluation of sufficiently homogeneous and stable reference materials for priority hazardous substances in whole water N2 - We have prepared and evaluated three whole water test materials containing eight polycyclic aromatic hydrocarbons (PAHs), six polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) with respect to homogeneity and short-term stability. The test materials were used as samples in two inter-laboratory comparisons. The materials were composed of natural mineral water and model suspended particulate matter (SPM) containing the target compounds at ng L-1 levels. The expanded uncertainty of the estimated mass concentrations in the final test materials was obtained by combining contributions from the homogeneity, the stability and the model SPM characterization. The whole water materials were sufficiently homogeneous and stable at 4 °C for their intended use. In total, 12 out of 15 investigated target parameters could be assessed to be present with a relative combined expanded uncertainty below 25 %. The outcome of the two interlaboratory comparisons confirmed the good quality of the test materials and the level of uncertainties associated with the estimated mass concentrations. These findings are an important contribution towards the development of whole water matrix reference materials certified for PAH, PBDE and TBT in support of the Water Framework Directive of the European Union. KW - Reference material KW - Referenzmaterial KW - Water Framework Directive KW - Wasserrahmenrichtlinie KW - Whole water sample KW - Gesamtwasserprobe PY - 2016 U6 - https://doi.org/10.1007/s00769-015-1189-1 SN - 0949-1775 SN - 1432-0517 VL - 21 IS - 2 SP - 113 EP - 120 PB - Springer AN - OPUS4-35728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Elordui-Zapatarietxe, S. A1 - Emteborg, H. A1 - Fettig, Ina A1 - Cabillic, J. A1 - Alasonati, E. A1 - Gantois, F. A1 - Swart, C. A1 - Gokcen, T. A1 - Tunc, M. A1 - Binici, B. A1 - Rodriguez-Cea, A. A1 - Zuliani, T. A1 - Gonzalez Gago, A. A1 - Pröfrock, D. A1 - Nousiainen, M. A1 - Sawal, G. A1 - Buzoianu, M. A1 - Philipp, Rosemarie T1 - An interlaboratory comparison on whole water samples N2 - The European Water Framework Directive 2000/60/EC requires monitoring of organic priority pollutants in so-called whole water samples, i.e. in aqueous nonfiltered samples that contain natural colloidal and suspended particulate matter. Colloids and suspended particles in the liquid phase constitute a challenge for sample homogeneity and stability. Within the joint research project ENV08 ‘‘Traceable measurements for monitoring critical pollutants under the European Water Framework Directive 2000/60/EC’’, whole water test materials were developed by spiking defined amounts of aqueous slurries of ultrafinely milled contaminated soil or sediment and aqueous solutions of humic acid into a natural mineral water matrix. This paper presents the results of an European-wide interlaboratory comparison (ILC) using this type of test materials. Target analytes were tributyltin, polybrominated diphenyl ethers and polycyclic aromatic hydrocarbons in the ng/L concentration range. Results of the ILC indicate that the produced materials are sufficiently homogeneous and stable to serve as samples for, e.g. proficiency testing or method validation. To our knowledge, this is the first time that ready-to-use water materials with a defined amount of suspended particulate and colloidal matter have been applied as test samples in an interlaboratory exercise. These samples meet the requirements of the European Water Framework Directive. Previous proficiency testing schemes mainly employed filtered water samples fortified with a spike of the target analyte in a water-miscible organic solvent. KW - Water Framework Directive KW - Wasserrahmenrichtlinie KW - Interlaboratory comparison KW - Ringversuch KW - Whole water sample KW - Gesamtwasserprobe PY - 2016 U6 - https://doi.org/10.1007/s00769-015-1190-8 SN - 0949-1775 SN - 1432-0517 VL - 21 IS - 2 SP - 121 EP - 129 PB - Springer AN - OPUS4-35730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabillic, J. A1 - Fallot, C. A1 - Hein, Sebastian A1 - Lalere, B. A1 - Philipp, Rosemarie T1 - Développement et validation d’une méthode de référence pour l’analyse des HAP dans l’eau totale dans le contexte de la DCE T1 - Development and validation of a reference method for the analysis of PAHs in whole water in accordance to the WFD N2 - Afin de garantir la qualité des eaux en Europe, la Commission Européenne a demandé aux États Membres, de leur fournir des résultats de mesure comparables et traçables pour l’analyse des polluants critiques. Devant ces enjeux considérables pour la protection de l’environnement, l’apport de la métrologie est nécessaire pour améliorer la fiabilité des analyses et permettre la comparabilité des résultats. C’est pourquoi, le projet de recherche européen Euramet/EMRP/ENV08 « Traçabilité des mesures pour la surveillance des polluants critiques de la DCE, Directive Cadre européenne sur l’Eau (2000/60/CE) », financé par l’EMRP, avait pour objectif de fournir des éléments pour la mise en place d’une base métrologique. Des méthodes de référence primaires permettant d’analyser des substances dangereuses prioritaires y sont développées pour répondre aux exigences de la DCE en termes de niveaux de performance (limites de quantification et incertitudes). Les hydrocarbures aromatiques polycycliques (HAP), substances dangereuses prioritaires « orphelines » de méthodes DCE compatibles, font partie des polluants ciblés par le projet. Le développement et la validation de la méthode d’analyse des HAP dans l’eau totale ont été réalisés. La méthode qui satisfait au mieux les exigences de la DCE en termes de concentrations et d’incertitudes accessibles est l’extraction en phase solide (SPE) sur un support disque suivie d’une analyse par dilution isotopique associée à la chromatographie en phase gazeuse couplée à la spectroscopie de masse (DI-CG/SM). N2 - To ensure the water quality in Europe, the European Commission asked the member states to provide comparable and traceable measurement results for the analysis of critical pollutants. Considering the increasing environmental challenges, the contribution of metrology is necessary both for the improvement of analysis reliability and the comparability of results. For this reason the European research project Euramet/EMRP/ENV08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD-2000/60/EC)”, funded by the EMRP, aimed to provide the elements for the development of a metrological basis. The project develops primary reference methods enabling the analysis of priority hazardous substances in order to meet the WFD requirements in terms of performance levels (limit of quantification and uncertainties). Polycyclic aromatic hydrocarbons (PAHs) – priority hazardous substances for which no DCE compatible methods exist – are among the three families of pollutants targeted by the project. This paper tackles the development and validation of the PAH analysis method on whole water samples. The method that best meets the requirements of the WFD in terms of level of concentration and uncertainty is the solid phase extraction (SPE) method with SPE-disks, followed by isotope dilution analysis combined with gas chromatography mass spectrometry (ID-GC/MS). KW - Reference method KW - Referenzmethode KW - Limit of quantification KW - Bestimmungsgrenze KW - Polycyclic aromatic hydrocarbons KW - Polyzyklische aromatische Kohlenwasserstoffe PY - 2015 UR - http://www.metrologie-francaise.fr/publications/revue_francaise_metrologie/2015-04/RFM40-1514.pdf U6 - https://doi.org/10.1051/rfm/2015014 SN - 1772-1792 VL - 2015-4 IS - 40 SP - 3 EP - 12 AN - OPUS4-35731 LA - fra AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Elordui-Zapatarietxe, S. A1 - Fettig, Ina A1 - Richter, Janine A1 - Philipp, Rosemarie A1 - Gantois, F. A1 - Lalère, B. A1 - Swart, C. A1 - Emteborg, H. T1 - Interaction of 15 priority substances for water monitoring at ng L-1 levels with glass, aluminium and fluorinated polyethylene bottles for the containment of water reference materials N2 - Certified water reference materials are currently not available for most of the hydrophobic organic pollutants listed in the EU Water Framework Directive. To find the most suitable container type for subsequent reference material productions, feasibility studies for the preparation of waters with polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) close to environmental quality standards in water have been performed. Due to the hydrophobic nature of these compounds and their tendency to adsorb onto container walls, an adequate selection of the most appropriate material for containment, storage and transport of water reference materials is crucial. Three different materials (aluminium, amber glass and fluorinated polyethylene, FPE) and three volumes (500/600 mL, 1000/1200 mL and 2000/3000 mL, depending on commercial availability) were tested at ng L-1 level of the target compounds. FPE shows by far the highest loss of analytes due to adsorption onto the container walls for all compounds studied. Aluminium and glass are equally suited for PAHs and PBDEs, but aluminium is unsuitable as container material for TBT due to acid cleaning requirements. The volume of the containers had no dramatic effect on the adsorption behaviour of target compounds for the different volumes tested. KW - Water framework directive KW - Reference materials KW - Hydrophobic organic pollutants KW - Bottles KW - Adsorption KW - Glass KW - Aluminium KW - Fluorinated polyethylene PY - 2015 U6 - https://doi.org/10.1007/s00769-015-1150-3 SN - 0949-1775 SN - 1432-0517 VL - 20 IS - 6 SP - 447 EP - 455 PB - Springer CY - Berlin AN - OPUS4-34946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. T1 - EURAMET.QM-S14 "Measurement capabilities for the quantification of ethanol in water" - Summary of results N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value are discussed. T2 - EURAMET TC-MC Meeting 2020 CY - Bern, Switzerland DA - 05.02.2020 KW - EURAMET KW - Key comparison KW - Ethanol in water PY - 2020 AN - OPUS4-50391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Fettig, I. A1 - Piechotta, Christian A1 - Philipp, Rosemarie A1 - Geißen, S. U. T1 - A novel GC-MS method for the determination and quantification of metformin in surface water N2 - Drug therapy for diabetes mellitus has increased significantly in recent years. 1,1-Dimethylbiguanide hydrochloride (metformin) is the most common drug used for the treatment of diabetes. Metformin is not metabolized in the human body and enters thewater cycle via sewage. A new gas chromatography-mass spectrometry (GC-MS) method has been developed which enables the quantification of metformin in surface water samples even at low concentrations in the ng L-1 range. A solid phase extraction (SPE) method for the preconcentration of metformin and the internal standard 1-butylbiguanide (buformin) was established, and the method parameters such as the composition and volume of the eluent were optimized. Derivatization of metformin and buformin was obtained by using n-methyl-bis (trifluoroacetamide)(MBTFA). The reaction conditions of the derivatization, such as the reaction temperature and volume of the derivatization agent, were evaluated. The limit of detection (LOD) and limit of quantification (LOQ) were determined to be 3.9 ng L-1 and 12 ng L-1 in surface water samples. Linearity was shown over a concentration range of 10–50 ng L-1. The good performance of the method was demonstrated by comparison with a liquid chromatography tandemmass spectrometry (LC-MS/MS) method. The results indicate that the GC-MS method is a reliable and sensitive alternative for the quantification of metformin in surface water. 1. KW - Metformin KW - GC-MS KW - Surface water PY - 2017 U6 - https://doi.org/10.1039/c6ay02606k SN - 1759-9679 SN - 1759-9660 VL - 9 IS - 10 SP - 1580 EP - 1584 PB - Royal Society of Chemistry AN - OPUS4-40243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Hein, Sebastian T1 - Preparation and certification of ethanol/water CRMs at BAM N2 - The presentation describes the preparation and certification of ethanol/water certified reference materials for the calibration of evidential breath alcohol analysers at BAM. T2 - ALCOREF kick-off meeting and training CY - Berlin, Germany DA - 16.10.2017 KW - Certified Reference Material KW - Breath alcohol analyser KW - Calibration PY - 2017 AN - OPUS4-43057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Hein, Sebastian T1 - BAM GC-FID method for the quantification of ethanol in water N2 - The talk presents an analytical method for the quantification of ethanol in water. The method is based on gas chromatography with flame ionisation detection and on-column injection. It is used at BAM for the certification and quality assurance of reference materials for the calibration of evidential breath alcohol analysers. T2 - ALCOREF kick-off meeting and training CY - Berlin, Germany DA - 16.10.2017 KW - GC-FID KW - Certified reference material KW - Breath alcohol analysis PY - 2017 AN - OPUS4-43061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. T1 - EMPIR project ALCOREF - certified forensic alcohol reference materials N2 - The talk presents a short summary of the EMPIR Project ALCOREF "Certified forensic alcohol reference materials". An interlaboratory comparison of analytical methods for the quantification of ethanol in water and a comparison of certified ethanol in water reference materials are proposed. T2 - EURAMET SCOA Meeting CY - Brno, Czech Republic DA - 05.02.2019 KW - Breath alcohol analyser KW - Certified reference material KW - Interlaboratory comparison PY - 2019 AN - OPUS4-47333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-471430 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Sander, L. C. A1 - Wise, S. A. A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Chan, P. A1 - Lee, H. A1 - Tang, H. A1 - Tang, P. A1 - Yip, Y. A1 - Lu, T. A1 - Cheow, P. S. A1 - Teo, T. L. A1 - Sega, M. A1 - Rolle, F. A1 - Baek, S. A1 - Kim, B. A1 - Lee, S. A1 - Cabillic, J. A1 - Fallot, C. A1 - Hua, T. A1 - Dazhou, C. A1 - Changjun, Y. A1 - Chunxin, L. A1 - Hongmei, L. A1 - Lippa, K. A1 - Itoh, N. A1 - Quinn, L. A1 - Prevoo-Franzsen, D. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. A1 - Gündüz, S. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Baldan, A. A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. T1 - CCQM-K131 Low-polarity analytes in a multicomponent organic solution: Polycyclic aromatic hydrocarbons (PAHs) in acetonitrile N2 - Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile". Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %. Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Naphthalene (Nap) KW - Organic calibration solution KW - Polycyclic aromatic hydrocarbon (PAH) PY - 2019 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-471442 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08003, 1 EP - 102 PB - IOP Science AN - OPUS4-47144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - 16RPT02 ALCOREF - Certified forensic alcohol reference materials N2 - The presentation summarises main achievements obtained in the first half of the EMPIR project ALCOREF. T2 - EMPIR Mid-term Review Conference 2019 CY - Berlin, Germany DA - 28.02.2019 KW - Certified reference material KW - Breath alcohol analyser KW - EMPIR PY - 2019 AN - OPUS4-47482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie A1 - Topal, K. A1 - Calzado, M. A1 - Bebic, J. A1 - Lalere, B. T1 - Certified reference materials for breath alcohol control – the ALCOREF project N2 - ALCOREF is a project within the European Metrology Programme for Innovation and Research (EMPIR. It is part of the 2016 EMPIR Research Potential Call dedicated to build up metrological and research capacity in less developed National Metrology Institutes (NMIs). The project will develop long term expertise for the production and certification of ethanol/water reference materials in the participating NMIs. Materials to be developed will be suitable for the calibration and approval of evidential breath alcohol analysers as defined by recommendation R 126 of the International Organization of Legal Metrology (OIML). Certification includes the characterisation of the materials, assessment of homogeneity, stability and uncertainty. Target certified values and volumes will address end-users’ needs regarding regional legal limits for alcohol in traffic and the instrumentation for breath analyser calibration available in different countries. Thus, the project supports the law enforcement of national drink-driving legislation. The consortium comprises of 11 institutions from 10 European countries. Project participants will establish reliable analytical methods for the purity assessment of ethanol, such as Karl-Fischer titration, to achieve traceability of their certified values. Chromatographic or density methods for the quantification of ethanol in water will also be established, validated and applied for homogeneity and stability assessment. An interlaboratory comparison will be conducted within the European Association of National Metrology Institutes’ (EURAMET) Technical Committee Metrology in Chemistry to test the equivalence of the new certified reference materials and the analytical methods implemented. The poster will present the outline and first results of the ALCOREF project. T2 - BERM-15 International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 24.09.2018 KW - Certified Reference Material KW - Breath alcohol control KW - ALCOREF PY - 2018 AN - OPUS4-46061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Martos, G. A1 - Josephs, R. A1 - Choteau, T. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moawad, M. A1 - Tarrant, G. A1 - Chan, B. A1 - Alamgir, M. A1 - de Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - de Sena, R. A1 - Oliveira, R. A1 - Melanson, J. A1 - Bates, J. A1 - Mai Le, P. A1 - Meija, J. A1 - Quan, C. A1 - Huang, T. A1 - Zhang, W. A1 - Ma, R. A1 - Zhang, S. A1 - Hao, Y. A1 - He, Y. A1 - Song, S. A1 - Wang, H. A1 - Su, F. A1 - Zhang, T. A1 - Li, H. A1 - Lam, W. A1 - Wong, W. A1 - Fung, W. A1 - Philipp, Rosemarie A1 - Dorgerloh, Ute A1 - Meyer, Klas A1 - Piechotta, Christian A1 - Riedel, Juliane A1 - Westphalen, Tanja A1 - Giannikopoulou, P. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Kitamaki, Y. A1 - Yamazaki, T. A1 - Shimizu, Y. A1 - Kuroe, M. A1 - Numata, M. A1 - Pérez-Castorena, A. A1 - Balderas-Escamilla, M. A1 - Garcia-Escalante, J. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - Tkachenko, I. A1 - Spirin, S. A1 - Smirnov, V. A1 - Tang Lin, T. A1 - Pui Sze, C. A1 - Juan, W. A1 - Lingkai, W. A1 - Ting, L. A1 - Quinde, L. A1 - Yizhao, C. A1 - Lay Peng, S. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Mkhize, D. A1 - Marajh, D. A1 - Chamane, S. A1 - Ahn, S. A1 - Choi, K. A1 - Lee, S. A1 - Han, J. A1 - Baek, S. A1 - Kim, B. A1 - Marbumrung, S. A1 - Jongmesuk, P. A1 - Shearman, K. A1 - Boonyakong, C. A1 - Bilsel, M. A1 - Gündüz, S. A1 - Ün, I. A1 - Yilmaz, H. A1 - Bilsel, G. A1 - Gökçen, T. A1 - Clarkson, C. A1 - Warren, J. A1 - Achtar, E. T1 - Mass fraction assignment of Bisphenol-A high purity material N2 - The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g. Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content. The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%. KW - Bisphenol-A KW - Purity assessment KW - Interlaboratory key comparison KW - Metrology PY - 2021 U6 - https://doi.org/10.1088/0026-1394/58/1A/08015 VL - 58 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-54188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moad, M. A1 - Chan, B. A1 - Munoz, A. A1 - Conneely, P. A1 - Ricci, M. A1 - Do Rego, E.C.P. A1 - Garrido, B.C. A1 - Violante, F.G.M. A1 - Windust, A. A1 - Dai, X. A1 - Huang, T. A1 - Zhang, W. A1 - Su, F. A1 - Quan, C. A1 - Wang, H. A1 - Lo, M. A1 - Wong, W. A1 - Gantois, F. A1 - Lalerle, B. A1 - Dorgerloh, Ute A1 - Koch, Matthias A1 - Klyk-Seitz, Urszula-Anna A1 - Pfeifer, Dietmar A1 - Philipp, Rosemarie A1 - Piechotta, Christian A1 - Recknagel, Sebastian A1 - Rothe, Robert A1 - Yamazaki, T. A1 - Zakaria, O. B. A1 - Castro, E. A1 - Balderas, M. A1 - González, N. A1 - Salazar, C. A1 - Regalado, L. A1 - Valle, E. A1 - Rodríguez, L. A1 - Laguna, L.Á.. A1 - Ramírez, P. A1 - Avila, M. A1 - Ibarra, J. A1 - Valle, L. A1 - Arce, M. A1 - Mitani, Y. A1 - Konopelko, L. A1 - Krylov, A. A1 - Lopushanskaya, E. A1 - Lin, T.T. A1 - Liu, Q. A1 - Kooi, L.T. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Nhlapo, N. A1 - Visser, R. A1 - Kim, B. A1 - Lee, H. A1 - Kankaew, P. A1 - Pookrod, P. A1 - Sudsiri, N. A1 - Shearman, K. A1 - Gören, A.C. A1 - Bilsel, G. A1 - Yilmaz, H. A1 - Bilsel, M. A1 - Cergel, M. A1 - Coskun, F.G. A1 - Uysal, E. A1 - Gündüz, S. A1 - Ün, I. A1 - Warren, J. A1 - Bearden, D.W. A1 - Bedner, M. A1 - Duewer, D.L. A1 - Lang, B.E. A1 - Lippa, K.A. A1 - Schantz, M.M. A1 - Sieber, J.R. T1 - Final report on key comparison CCQM-K55.c (L-(+)-Valine): Characterization of organic substances for chemical purity N2 - KEY COMPARISON Under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a key comparison, CCQM K55.c, was coordinated by the Bureau International des Poids et Mesures (BIPM) in 2012. Twenty National Measurement Institutes or Designated Institutes and the BIPM participated. Participants were required to assign the mass fraction of valine present as the main component in the comparison sample for CCQM-K55.c. The comparison samples were prepared from analytical grade L-valine purchased from a commercial supplier and used as provided without further treatment or purification. Valine was selected to be representative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of low structural complexity [molecular weight range 100–300] and high polarity (pKOW > –2). The KCRV for the valine content of the material was 992.0 mg/g with a combined standard uncertainty of 0.3 mg/g. The key comparison reference value (KCRV) was assigned by combination of KCRVs assigned from participant results for each orthogonal impurity class. The relative expanded uncertainties reported by laboratories having results consistent with the KCRV ranged from 1 mg/g to 6 mg/g when using mass balance based approaches alone, 2 mg/g to 7 mg/g using quantitative 1H NMR (qNMR) based approaches and from 1 mg/g to 2.5 mg/g when a result obtained by a mass balance method was combined with a separate qNMR result. The material provided several analytical challenges. In addition to the need to identify and quantify various related amino acid impurities including leucine, isoleucine, alanine and a-amino butyrate, care was required to select appropriate conditions for performing Karl Fischer titration assay for water content to avoid bias due to in situ formation of water by self-condensation under the assay conditions. It also proved to be a challenging compound for purity assignment by qNMR techniques. There was overall excellent agreement between participants in the identification and the quantification of the total and individual related structure impurities, water content, residual solvent and total non-volatile content of the sample. Appropriate technical justifications were developed to rationalise observed discrepancies in the limited cases where methodology differences led to inconsistent results. The comparison demonstrated that to perform a qNMR purity assignment the selection of appropriate parameters and an understanding of their potential influence on the assigned value is critical for reliable implementation of the method, particularly when one or more of the peaks to be quantified consist of complex multiplet signals. PY - 2014 U6 - https://doi.org/10.1088/0026-1394/51/1A/08010 SN - 0026-1394 SN - 1681-7575 VL - 51 SP - 08010, 1 EP - 44 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-31072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -