Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-54188 Zeitschriftenartikel Westwood, S.; Martos, G.; Josephs, R.; Choteau, T.; Wielgosz, R.; Davies, S.; Moawad, M.; Tarrant, G.; Chan, B.; Alamgir, M.; de Rego, E.; Wollinger, W.; Garrido, B.; Fernandes, J.; de Sena, R.; Oliveira, R.; Melanson, J.; Bates, J.; Mai Le, P.; Meija, J.; Quan, C.; Huang, T.; Zhang, W.; Ma, R.; Zhang, S.; Hao, Y.; He, Y.; Song, S.; Wang, H.; Su, F.; Zhang, T.; Li, H.; Lam, W.; Wong, W.; Fung, W.; Philipp, Rosemarie; Dorgerloh, Ute; Meyer, Klas; Piechotta, Christian; Riedel, Juliane; Westphalen, Tanja; Giannikopoulou, P.; Alexopoulos, Ch.; Kakoulides, E.; Kitamaki, Y.; Yamazaki, T.; Shimizu, Y.; Kuroe, M.; Numata, M.; Pérez-Castorena, A.; Balderas-Escamilla, M.; Garcia-Escalante, J.; Krylov, A.; Mikheeva, A.; Beliakov, M.; Palagina, M.; Tkachenko, I.; Spirin, S.; Smirnov, V.; Tang Lin, T.; Pui Sze, C.; Juan, W.; Lingkai, W.; Ting, L.; Quinde, L.; Yizhao, C.; Lay Peng, S.; Fernandes-Whaley, M.; Prevoo-Franzsen, D.; Quinn, L.; Nhlapo, N.; Mkhize, D.; Marajh, D.; Chamane, S.; Ahn, S.; Choi, K.; Lee, S.; Han, J.; Baek, S.; Kim, B.; Marbumrung, S.; Jongmesuk, P.; Shearman, K.; Boonyakong, C.; Bilsel, M.; Gündüz, S.; Ün, I.; Yilmaz, H.; Bilsel, G.; Gökçen, T.; Clarkson, C.; Warren, J.; Achtar, E. Mass fraction assignment of Bisphenol-A high purity material 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)%. IOP Publishing Bureau International des Poids et Mesures (BIPM) 2021 Metrologia 58 1A 08015 10.1088/0026-1394/58/1A/08015 2022-01-05 OPUS4-55889 Zeitschriftenartikel Philipp, Rosemarie; Lalere, B.; Gantois, F.; Sánchez, C.; Sáez, A.; Bebić, J.; Banjanac, K.; Alexopoulos, Ch.; Kakoulides, E.; Claramunt, A. V.; Janko, P.; Jotanovic, A.; Hafner-Vuk, K.; Buzoianu, M.; Mihail, R.; Fernández, M. M.; Etcheverry, J.; Mbithi Muendo, B.; Muriira Karau, G.; Silva, A.; Almirón, F.; Marajh, D.; Makgatho, P.; Visser, R.; Alaskar, A. R.; Alosaimi, A.; Alrashed, M.; Yilmaz, H.; Ün, İ.; Gündüz, S.; Topal, K.; Bilsel, M.; Karasinski, J.; Torres, J. Supplementary comparison study - measurement capabilities for the quantification of ethanol in water 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. IOP Publishing 2022 Metrologia 59 1A 08015 10.1088/0026-1394/59/1A/08015 2022-10-06 OPUS4-31072 Zeitschriftenartikel Westwood, S.; Josephs, R.; Choteau, T.; Daireaux, A.; Wielgosz, R.; Davies, S.; Moad, M.; Chan, B.; Munoz, A.; Conneely, P.; Ricci, M.; Do Rego, E.C.P.; Garrido, B.C.; Violante, F.G.M.; Windust, A.; Dai, X.; Huang, T.; Zhang, W.; Su, F.; Quan, C.; Wang, H.; Lo, M.; Wong, W.; Gantois, F.; Lalerle, B.; Dorgerloh, Ute; Koch, Matthias; Klyk-Seitz, Urszula-Anna; Pfeifer, Dietmar; Philipp, Rosemarie; Piechotta, Christian; Recknagel, Sebastian; Rothe, Robert; Yamazaki, T.; Zakaria, O. B.; Castro, E.; Balderas, M.; González, N.; Salazar, C.; Regalado, L.; Valle, E.; Rodríguez, L.; Laguna, L.Á..; Ramírez, P.; Avila, M.; Ibarra, J.; Valle, L.; Arce, M.; Mitani, Y.; Konopelko, L.; Krylov, A.; Lopushanskaya, E.; Lin, T.T.; Liu, Q.; Kooi, L.T.; Fernandes-Whaley, M.; Prevoo-Franzsen, D.; Nhlapo, N.; Visser, R.; Kim, B.; Lee, H.; Kankaew, P.; Pookrod, P.; Sudsiri, N.; Shearman, K.; Gören, A.C.; Bilsel, G.; Yilmaz, H.; Bilsel, M.; Cergel, M.; Coskun, F.G.; Uysal, E.; Gündüz, S.; Ün, I.; Warren, J.; Bearden, D.W.; Bedner, M.; Duewer, D.L.; Lang, B.E.; Lippa, K.A.; Schantz, M.M.; Sieber, J.R. Final report on key comparison CCQM-K55.c (L-(+)-Valine): Characterization of organic substances for chemical purity 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. Bristol Inst. of Physics Publ. 2014 Metrologia 51 08010, 1 44 10.1088/0026-1394/51/1A/08010 2016-02-20 OPUS4-45381 Zeitschriftenartikel Dai, X.; Zhang, W.; Li, H.; Huang, T.; Li, M.; Quan, C.; Zhang, Q.; Davies, S. R.; Warren, J.; Lo, M.-F.; Kakoulides, E.; Gören, A. C.; Marbumrung, S.; Pfeifer, Dietmar; Ün, I.; Gündüz, S.; Yilmaz, H.; Kankaew, P.; Sudsiri, N.; Shearman, K.; Pookrod, P.; Polzer, J.; Radeck, W. CCQM-K104 key comparison (avermectin B(1)a) on the characterization of organic substances for chemical purity Under the Comité Consultatif pour la Quantité de Matière (CCQM), a key comparison, CCQM-K104, was coordinated by the National Institute of Metrology (NIM). The comparison was designed to demonstrate a laboratory's performance in determining the mass fraction of the main component in a complex high purity organic material. Nine NMIs or DIs participated in the comparison. Eight participants reported their results. An additional impurity was resolved from the avermectin B1a peak and was tentatively identified as an unknown impurity by NMIA (National Measurement Institute (Australia)). It was subsequently identified by NIM as a diastereoisomer of avermectin B1a at the C-26 position. Final reference value (KCRV) = 924.63 mg/g, with uncertainty (k=1) = 3.89 mg/g, and expanded uncertainty = 8.97 mg/g. The degrees of equivalence with the avermectin B1a KCRV for each participant were reported. The measurement results and degrees of equivalence should be indicative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of high structural complexity (relative molecular mass range of 500 Da -1000 Da and low polarity (-log KOW ≤ -2). 2017 Metrologia 54 2 32 10.1088/0026-1394/54/1A/08019 2018-07-05 OPUS4-45035 Forschungsbericht Dai, X.; Zhang, W.; Li, H.; Huang, T.; Li, M.; Quan, C.; Zhang, Q.; Davies, S. R; Warren, J.; Lo, M.-F.; Kakoulides, E.; Ceyhan Gören, A.; Marbumrung, S.; Pfeifer, Dietmar; Ün, I.; Gündüz, S.; Yilmaz, H.; Kankaew, P.; Sudsiri, N.; Shearman, K.; Pookrod, P.; Polzer, J.; Radeck, W. CCQM-K104 Key Comparison on the characterization of organic substances for chemical purity - Avermectin B1a Anwendungen von qNMR 2017 1 32 2018-05-30 OPUS4-44999 Zeitschriftenartikel Westwood, S.; Josephs, R.; Choteau, T.; Daireaux, A.; Stoppacher, N.; Wielgosz, R.; Davies, S.; do Rego, E.; Wollinger, W.; Garrido, B.; Fernandes, J.; Lima, J.; Oliveira, R.; de Sena, R.; Windust, A.; Huang, T.; Dai, X.; Quan, C.; He, H.; Zhang, W.; Wei, C.; Li, N.; Gao, D.; Liu, Z.; Lo, M.; Wong, W.; Pfeifer, Dietmar; Koch, Matthias; Dorgerloh, Ute; Rothe, Robert; Philipp, Rosemarie; Hanari, N.; Rezali, M.; Arzate, C.; Berenice, M.; Caballero, V.; Osuna, M.; Krylov, A.; Kharitonov, S.; Lopushanskaya, E.; Liu, Q.; Lin, T.; Fernandes-Whaley, M.; Quinn, L.; Nhlapo, N.; Prevoo-Franzsen, D.; Archer, M.; Kim, B.; Baek, S.; Lee, S.; Lee, J.; Marbumrung, S.; Kankaew, P.; Chaorenpornpukdee, K.; Chaipet, T.; Shearman, K.; Gören, A.; Gündüz, S.; Yilmaz, H.; Un, I.; Bilsel, G.; Clarkson, C.; Bedner, M.; Camara, J.; Lang, B.; Lippa, K.; Nelson, M.; Toman, B.; Yu, L. Mass fraction assignment of folic acid in a high purity material - CCQM-K55.d (Folic acid) Final Report 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% Institute of Physics Publishing (IOP) ; Bureau International des Poids et Mesures 2018 Metrologia 55 Technical Supplement, 2018 08013, 1 38 10.1088/0026-1394/55/1A/08013 2018-05-24