TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods JF - Metrologia N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.M. A1 - Li, H.M. A1 - Zhang, Q.H. A1 - Lu, X.H. A1 - Li, S.Q. A1 - Koch, Matthias A1 - Polzer, J. A1 - Hackenber, R. A1 - Moniruzzaman, M. A1 - Khan, M. A1 - Kakoulides, E. A1 - Pak-Wing, K. A1 - Richy, A1 - Chi-Shing, N. A1 - Lu, T. A1 - Gui, E.M. A1 - Cheow, P.S. A1 - Teo, T.L. A1 - Rego, E. A1 - Garrido, B. A1 - Carvalho, L. A1 - Leal, R. A1 - Violante, F. A1 - Baek, S.Y. A1 - Lee, S. A1 - Choi, K. A1 - Kim, B. A1 - Bucar-Miklavcic, M. A1 - Hopley, C. A1 - Nammoonnoy, J. A1 - Murray, J. A1 - Wilson, W. A1 - Toman, B. A1 - Itoh, N. A1 - Gokcen, T. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil JF - Metrologia N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. 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). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix. KW - Metrology KW - CCQM KW - Food KW - PAH PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1a/08017 VL - 57 IS - 1a SP - 08017 AN - OPUS4-52435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liaskos, C. A1 - Rhoderick, G. A1 - Hodges, J. A1 - Possolo, A. A1 - Wilke, Olaf T1 - Pilot comparison CCQM-P177 - monoterpenes in nitrogen at 2.5 nmol/mol - final report JF - Metrologia N2 - Growing awareness of the impact of monoterpenes on climate, atmospheric chemistry, and indoor air quality has necessitated the development of measurement standards to globally monitor and control their emissions. For National Metrology Institutes to develop such standards, it is essential that they demonstrate measurement equivalence for assigned values at the highest levels of accuracy. This report describes the results of a pilot comparison for 4 key monoterpene species: α-pinene, 3-carene, R-limonene and 1,8-cineole, at a nominal amount-of-substance fraction of 2.5 nmol mol-1. The objective of this comparison is to evaluate participant capabilities to measure trace-level monoterpenes using their own calibration techniques. KW - Pilot comparison KW - CCQM KW - Monoterpene KW - Accuracy PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08018 SN - 0026-1394 SN - 1681-7575 VL - 57 IS - 1A SP - 08018-1 EP - 08018-21 PB - IOP Science AN - OPUS4-51111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Gökçen, T. A1 - Binici, B. A1 - Isleyen, A. A1 - Piechotta, Christian A1 - Kar-wai, A. A1 - Krylov, A. A1 - Miheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - chenko, Irina Tka A1 - Perkola, N. A1 - Lewin, M. A1 - Hua, T. T1 - High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water JF - Metrologia N2 - The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA). Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA. This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media. Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - PFAS KW - Surface water KW - ILC KW - CCQM PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08016 VL - 59 IS - 1A SP - 1 EP - 3 PB - IOP Publishing AN - OPUS4-58941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -