TY - JOUR A1 - Arroyo-Abad, Uriel A1 - Lischka, Susanne A1 - Piechotta, Christian A1 - Mattusch, J. A1 - Reemtsma, T. T1 - Determination and identification of hydrophilic and hydrophobic arsenic species in methanol extract of fresh cod liver by RP-HPLC with simultaneous ICP-MS and ESI-Q-TOF-MS detection N2 - The present study was focused on the determination and identification of arsenic species in methanolic extracts of cod liver. Arsenic species were fractionated and the fractions analysed by RP-HPLC-ICP-MS coupled with ESI-Q-TOF-MS. The total concentration of arsenic in the fresh cod liver was analysed by ICP-MS to be 1.53 ± 0.02 mg As kg-1 w.w. and the extraction recovery was ca. 100% and the column recovery >93%. Besides polar inorganic and methylated arsenic species (>70%) more hydrophobic arsenic-containing fatty acids and hydrocarbons occurred. Based on the mass spectrometric data proposals for molecular structures were elaborated for 20 of the organic As species included 10 arsenic-containing fatty acids (AsFA) and an arsenic-containing hydrocarbon (AsHC) mentioned for the first time in fresh cod liver. Arsenobetaine was found as main water-soluble arsenic compound in cod liver followed by higher molecular mass arsenic-containing fatty acids and hydrocarbons. KW - Arsenic species KW - Arsenolipids KW - Marine fish KW - Cod liver KW - HPLC-ICP-MS/ESI-Q-TOF-MS PY - 2013 DO - https://doi.org/10.1016/j.foodchem.2013.05.152 SN - 0308-8146 VL - 141 IS - 3 SP - 3093 EP - 3102 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-28852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Identifizierung und analytische Betrachtung von Arsenolipiden in Hering T2 - ANAKON 2013 CY - Essen, Germany DA - 2013-03-04 PY - 2013 AN - OPUS4-27780 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Einsatz eines isotopenmarkierten Kalibrierstandards zur Bestimmung von Arsenobetain mittels HPLC-ESI-MS/MS T2 - CANAS 2013 CY - Freiberg, Germany DA - 2013-03-18 PY - 2013 AN - OPUS4-27781 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lischka, Susanne A1 - Arroyo-Abad, Uriel A1 - Mattusch, J. A1 - Kühn, Andreas A1 - Piechotta, Christian T1 - The high diversity of arsenolipids in herring fillet (Clupea harengus) N2 - Arsenolipids represent a relevant step in the biosynthesis of organoarsenicals from inorganic arsenic compounds. Their fate after human consumption is still uncertain. By means of a HPLC-ICP-MS/ESI-Q-TOF-MS method, 16 lipid soluble arsenic compounds, including seven formerly unknown organoarsenicals, have been identified in commercial herring fillet. The structural assignment was done by exact mass and high resolution MS/MS data. This is the first identification of arsenolipids in herring (Clupea harengus). They contribute with (3.6±0.2) mg kg-1 arsenic to 62.3% of the total arsenic content of (5.7±0.3) mg of arsenic per kg dry mass. Current studies indicate that a metabolization by humans to cancerous dimethylarsinic acid is very likely. The presented results are highly relevant as herring is a very popular food fish species in Europe. Moreover, the screening of different fish species revealed that arsenolipids are more widespread than previously assumed. KW - Arsenic species KW - Arsenolipids KW - Fish KW - Herring KW - ESI-MS/MS KW - ICP-TOF-MS PY - 2013 DO - https://doi.org/10.1016/j.talanta.2013.02.051 SN - 0039-9140 VL - 110 SP - 144 EP - 152 PB - Elsevier CY - Amsterdam AN - OPUS4-28302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Identification and Characterization of New Disinfections By-products of Polycyclic Musks (AHTN and HHCB) in Swimming pool water T2 - ICCE 2013 CY - Barcelona, Spain DA - 2013-06-24 PY - 2013 AN - OPUS4-28773 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Isotopic labeled standard for the routine analysis of arsenobetaine T2 - Metallomic 2013 CY - Oviedo, Spain DA - 2013-07-08 PY - 2013 AN - OPUS4-28775 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Durmaz, V. A1 - Schmidt, Sebastian A1 - Sabri, P. A1 - Piechotta, Christian A1 - Weber, M. T1 - Hands-off linear interaction energy approach to binding mode and affinity estimation of estrogens N2 - With this work we target the development of a predictictive model for the identification of small molecules which bind to the estrogen receptor alpha and, thus, may act as endocrine disruptors. We propose a combined thermodynamic approach for the estimation of preferential binding modes along with corresponding free energy differences using a linear interaction energy (LIE) ansatz. The LIE model is extended by a Monte Carlo approach for the computation of conformational entropies as recently developed by our group. Incorporating the entropy contribution substantially increased the correlation with experimental affinity values. Both squared coefficients for the fitted data as well as the more meaningful leave-one-out cross-validation of predicted energies were elevated up to rFit2 = 0.87 and qLOO2 = 0.82, respectively. All calculations have been performed on a set of 31 highly diverse ligands regarding their structural properties and affinities to the estrogen receptor alpha. Comparison of predicted ligand orientations with crystallographic data retrieved from the Protein database pdb.org revealed remarkable binding mode predictions. KW - Estrogenes KW - Modeling KW - Affinity PY - 2013 DO - https://doi.org/10.1021/ci400392p SN - 1549-9596 SN - 0095-2338 SN - 1549-960X VL - 53 IS - 10 SP - 2681 EP - 2688 CY - Washington, DC AN - OPUS4-29611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Weathering scenarios – Changes in polymer surface morphologies and leaching of brominated flame retardants N2 - In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification. Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil). The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials. Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - BFR KW - Weathering KW - PP KW - PS PY - 2018 AN - OPUS4-47029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Piechotta, Christian A1 - Bandow, Nicole T1 - Comparing PFAS analysis in batch leaching and column leaching tests N2 - Laboratory leaching tests are tools to assess the mobility of environmental contaminants released from granular materials. Comparative leaching tests were performed using four PFAS-contaminated soils whose concentration patterns of 10 selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) differed due to the two types of contamination sources. This study aimed to evaluate the equivalence of two usual laboratory-scale leaching test procedures, batch and column percolation tests, at liquid-to-solid ratios (L/S) of 2 l/kg, which is the current practice within the German assessment framework, and 10 l/kg (relevant for some EU regulations such as the landfill directive). The differences between the replicates of leaching tests investigating PFAS were smaller for column percolation tests than for batch tests, probably mainly due to the greater sample size and the better representativeness of the sample portion analyzed. It was observed that batch tests overestimate the release of shorter-chain PFAS, whereby the effect was greater with carboxylic than with sulfonic acids. Currently, the limits of detection of analyses given by the DIN standard with regard to PFCA and PFSA in soils are partly not sufficient to detect very low contents, whereas the detection of selected PFCA and PFSA in eluates is more sensitive, in accordance with the available standards. This results in limitations when calculating mass balances. KW - PFAS KW - Leaching KW - Column percolation test KW - Batch test KW - Soil PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618187 DO - https://doi.org/10.1007/s11356-024-35510-0 SN - 1614-7499 VL - 31 IS - 57 SP - 65233 EP - 65251 PB - Springer Science and Business Media LLC AN - OPUS4-61818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Entwicklung eines simultanen Bestimmungs- und Anreicherungsverfahrens für Östrogene und östrogenwirksame Verbindungen in Abwasser T2 - ANAKON 2009 CY - Berlin, Germany DA - 2009-03-17 PY - 2009 AN - OPUS4-18222 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - LAS-Kalibrierstandards T2 - ANAKON 2007 CY - Jena, Germany DA - 2007-03-27 PY - 2007 AN - OPUS4-13741 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - A TBT reference method for European water legislation T2 - ANAKON 2013 CY - Essen, Germany DA - 2013-03-04 PY - 2013 AN - OPUS4-27720 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Arsenolipide im Hering - Eine Quelle für kanzerogene Arsenverbindungen im Urin? T2 - ANAKON 2013 CY - Essen, Germany DA - 2013-03-04 PY - 2013 AN - OPUS4-27858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - LA-ICP-MS- und RFA-Messungen für die Bestimmung von polybromierten Flammschutzmitteln (PBFSM) in Polystyrol- und Polypropylenproben N2 - To investigate the release and migration of flame retardants from polypropylene (PP) and polysytrene (PS) we use samples of with defined content of flame retardants as additives. Therefore we use HBCD in the concentration of 1% wt. resp. BDE-209 in the concentration of 0.1% wt. For the preparation of the samples granular of PP resp. PS are extruded together with the BFRs additives. Even the result of this process may lead to homogenous partition of the BFRs additives, this has to be proven before using the samples in the experimental setup for weathering studies. In accordance to the regulation of RoHS, where the use of XRF is recommended for the proof of flame retardants in electronic consumer products, we use this method as a reference to the laser ablation ICP/MS. Therefore we present the correlation of these experiments. The experimental setup for the XRF experiment is like a standard addition: in cavities, which are introduced in the sample plates subsequently, solutions of defi ned concentration of flame retardants are put in these cavities. According to the idea of standard addition, we get an information of the originating concentration of flame retardant in each sample and we can monitor the release and migration of these additives during/after the weathering experiment with high precision. Therefore to the designated plates an internal standard is added as a marker and can be analyzed after the weathering experiment. As awaited, the light exposed site, shows a deviating content in flame retardants compared to the sheltered site. N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz, die jeweils mit polybromierten Flammschutzmitteln (PBFSM) versehen sind. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Auch soll mit Hilfe der RFA und der LA-ICP-MS die Abreicherung der PBFSM in den Modellmaterialien beschrieben werden. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - PBFSM KW - RFA KW - LA-ICP-MS KW - Polypropylen KW - Polystyrol PY - 2018 AN - OPUS4-47028 LA - deu 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 DO - 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 - CONF A1 - Kalbe, Ute A1 - Berger, Wolfgang A1 - Bredow, Andrea A1 - Krüger, Oliver A1 - Piechotta, Christian A1 - Schoknecht, Ute T1 - Säulenperkolationsversuche mit perfluorierten Tensiden und Bioziden in Böden N2 - Säulenperkolationsversuche werden u.a. zur Ermittlung der Freisetzung von Schadstoffen aus Böden durchgeführt. Im Entwurf der novellierten Bundesboden-schutz- und Altlastenverordnung ist neben Schüttelverfahren (DIN 19527 und 19529) ein Säulenperkolationsverfahren (DIN 19528) zur Eluatgewinnung aus Böden festgeschrieben. Mit diesem Verfahren kann im Vergleich zu den Schüttelversuchen auch der zeitliche Verlauf der Schadstofffreisetzung erfasst und bewertet werden. Allerdings sind die Verfahren bisher nur für anorganische Stoffe und wenige prioritäre organische Schadstoffe validiert worden (PAK, MKW, PCB, Phenole). Aber auch Schadstoffe wie perfluorierte Tenside (PFT), die z.B. für die Veredlung von Papier, Textilien und Haushaltsgeräten eingesetzt werden oder Biozide, mit denen Bauprodukte zum Schutz vor mikrobiellem Befall ausgerüstet werden (z.B. Fassadenbeschichtungen und Holz), geraten auf Grund ihrer gesundheits- und umwelt-schädlichen Eigenschaften immer stärker in die Diskussion. T2 - DBG-Jahrestagung 2013 - Kommission VI - Böden - Lebensgrundlage und Verantwortung CY - Rostock, Germany DA - 07.09.2013 KW - Elutionsverfahren KW - Säulenperkolationsverfahren KW - Kontaminierte Böden KW - Organische Schadstoffe PY - 2013 N1 - Serientitel: Berichte der DBG – Series title: Berichte der DBG SP - 1 EP - 3 PB - DBG (Deutsche Bodenkundliche Gesellschaft) CY - Göttingen AN - OPUS4-29453 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Bandow, Nicole A1 - Bredow, Andrea A1 - Mathies, Helena A1 - Piechotta, Christian T1 - Column leaching tests on soils containing less investigated organic pollutants N2 - Column tests are a common tool to investigate the leaching behavior of contaminated soil and waste materials. In contrast to inorganic analytes, fewer studies with organic contaminants are available based on column tests. This paper is aimed at the question if soil materials contaminated with organic pollutants can be reliably investigated by column tests. Soils contaminated with TPH (total petrol hydrocarbons), PFC (perfluorinated surfactants) and the biocide tebuconazole were used for column percolation tests. Differences in the leaching behavior are mainly driven by partitioning behavior between organic carbon and water, which can be estimated from log KOW values and size and shape of molecules. PFC show higher release (10–50% for individual compounds) than pesticides (3.7–5.3%) and TPH (< 1%) at liquid to solid ratio of 4 l/kg. All eluate concentrations are low with maximum concentrations of 50 µg/l for PFC and 1–2 mg/l for pesticides and TPH. Despite this, the observed standard deviations are quite small suggesting good repeatability. In general the observed concentration trends are similar to that from lysimeter studies found in the literature and thus, it can be concluded that laboratory column experiments are a reliable tool for organic compounds with various physico-chemical properties. KW - Column percolation leaching KW - Total petrol hydrocarbons KW - Perfluorinated surfactants KW - Pesticides PY - 2014 DO - https://doi.org/10.1016/j.gexplo.2014.06.014 SN - 0375-6742 VL - 147 IS - Part B SP - 291 EP - 297 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-32144 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 DO - 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 - TY - CONF A1 - Piechotta, Christian T1 - Development, Validation and Application of an Accelerated Weathering Protocol for Assessing Bisphenol A Release from Polycarbonate Materials into the environment N2 - Bisphenol A (BPA) is under continuous regulatory scrutiny and listed as substance of very high concern (SVHC). Particular concern is related to its frequent detection in surface waters, despite being readily biodegradable. Several studies have been conducted to investigate sources and pathways of BPA in the environment, concluding that its main use as monomer in polycarbonate (PC) contributes only marginally to environmental BPA releases over its life cycle. To better understand the actual releases of BPA from PC under environmental conditions, a newly developed methodology (Federal Institute for Materials Research and Testing, BAM) was applied, which comprises a novel accelerated weathering protocol for polycarbonate (PC) materials, combined with an advanced analytical setup allowing for improved detection of BPA at trace level concentrations. The weathering protocol achieves a 13.6-fold acceleration compared to Central European outdoor conditions and simulates environmental stressors (global radiation, rain, temperature variations) in a laboratory weathering chamber, with simultaneous BPA release measurements using an organic isotope dilution calibration LC-MS/MS approach. Validation was performed in parallel outdoor exposure tests, by using haze and yellowness index measurements as reference parameters. PC sample types representative of major polycarbonate applications were examined: Samples with different levels of UV-protection as used in transparent sheets used outdoor in construction or housings in Electro- and Electronic applications as well as samples with a protective coating as used in automotive applications (headlamps, glazing and construction). Results demonstrated consistently low total BPA releases of around 0.3 mg m⁻² for samples with exposed PC surfaces, while releases from coated samples were significantly reduced by around two orders of magnitude. In all cases examined, the BPA release ceased to zero after a period of four to six weeks, equivalent to approximately 1 to 1.5 years of outdoor exposure. This suggests that potential BPA releases diminish to virtually zero after that timespan. While the newly developed test method is not suitable for routine laboratory implementation, it provides crucial quantitative data on BPA release from PC materials during accelerated environmental weathering. T2 - Umwelt 2025 CY - Dessau, Germany DA - 22.09.2025 KW - Bisphenol A KW - Polycarbonate KW - Weathering PY - 2025 AN - OPUS4-64664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - The European Metrology Network for Pollution Monitoring – EMN POLMO N2 - The EU’s Green Deal acknowledges that « the EU needs to better monitoring, report, prevent and remedy pollution from air, water, soil and consumer products and to look more systematically at all policies and regulations ». In order to address these challenges, the Commission launched a new Strategy for Sustainability in October 2020, and adopted a Zero-pollution Action Plan for air, water and soil, in 2021. The comparability and trueness of measurements are often compromised by the lack of intact traceability chains and appropriate quality controls, for example attained by the use of matrix-matched certified reference materials, participation in interlaboratory comparisons and other validation schemes . Noticeable improvements are apprehended after practical demonstrations and scientific discussions on the importance of traceability to the SI with stakeholders and end-users . The European Metrology Network for Pollution Monitoring (EMN POLMO) was created in 2022 to provide metrology support to the environmental community and industry involved in the monitoring of variety of pollutants, including chemical pollutants, radionuclides, biological & microbiological, and nano and micro particles, in the three environmental compartments (air, water and soil). Recently, light pollution and noise pollution have been included in the scope of the network. One of the main goals of POLMO is to bridge the interests of the different stakeholder and end-user, and to contribute to environmental sustainability through the provision of tools and resources, required to perform accurate, comparable measurements. The POLMO Strategic Research Agenda identifies the key measurement challenges and opportunities in pollution monitoring and sets out a roadmap for future research and development. T2 - BIPM - 150 years of meter convention CY - Versailles, France DA - 20.05.2025 KW - POLMO KW - EMN PY - 2025 AN - OPUS4-64662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Development, Validation and Application of an Accelerated Weathering Protocol for Assessing Bisphenol A Release from Polycarbonate Materials into the environment N2 - Bisphenol A (BPA) is under continuous regulatory scrutiny and listed as substance of very high concern (SVHC). Particular concern is related to its frequent detection in surface waters, despite being readily biodegradable. Several studies have been conducted to investigate sources and pathways of BPA in the environment, concluding that its main use as monomer in polycarbonate (PC) contributes only marginally to environmental BPA releases over its life cycle. To better understand the actual releases of BPA from PC under environmental conditions, a newly developed methodology (Federal Institute for Materials Research and Testing, BAM) was applied, which comprises a novel accelerated weathering protocol for polycarbonate (PC) materials, combined with an advanced analytical setup allowing for improved detection of BPA at trace level concentrations. The weathering protocol achieves a 13.6-fold acceleration compared to Central European outdoor conditions and simulates environmental stressors (global radiation, rain, temperature variations) in a laboratory weathering chamber, with simultaneous BPA release measurements using an organic isotope dilution calibration LC-MS/MS approach. Validation was performed in parallel outdoor exposure tests, by using haze and yellowness index measurements as reference parameters. PC sample types representative of major polycarbonate applications were examined: Samples with different levels of UV-protection as used in transparent sheets used outdoor in construction or housings in Electro- and Electronic applications as well as samples with a protective coating as used in automotive applications (headlamps, glazing and construction). Results demonstrated consistently low total BPA releases of around 0.3 mg m⁻² for samples with exposed PC surfaces, while releases from coated samples were significantly reduced by around two orders of magnitude. In all cases examined, the BPA release ceased to zero after a period of four to six weeks, equivalent to approximately 1 to 1.5 years of outdoor exposure. This suggests that potential BPA releases diminish to virtually zero after that timespan. While the newly developed test method is not suitable for routine laboratory implementation, it provides crucial quantitative data on BPA release from PC materials during accelerated environmental weathering. T2 - Umwelt 2025 CY - Dessau, Germany DA - 22.09.2025 KW - Bisphenol A KW - Polycarbonate KW - Weathering PY - 2025 AN - OPUS4-64665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Comparison of three different TOP Assay approaches for the determination of PFAS concentration in soil N2 - Within a project by the German Environmental Agency (Umweltbundesamt – UBA) soil samples are taken at different sites all over Germany. The concentration of 30 PFAS - 13 carboxylic acids (C4-C18), 5 sulfonic acids (C4-C10) and 12 precursor substances) - was determined in these soil samples using three different sample preparation approaches: 1) ultrasonic extraction of the soil samples with Methanol; 2) preparation of eluates to test the leaching behaviour of the PFAS and 3) TOP assays following the method published by Houtz & Sedlak. Targeted LC-MS/MS is used to determine PFAS concentration after all three preparation steps. For the TOP assay, the concentration of all 30 PFAS is compared prior to and after the oxidation reaction. Besides the ‘classic’ TOP assay, two other TOP assay approaches, the dTOP assay and the photoTOP assay, are tested and compared. First, all three TOP assay approaches will be tested on a reference soil spiked with a solution including all 30 PFAS measured in the project. Later, soil samples taken within the the priorly described project will were tested. This work is financed by the UBA via the ReFoPlan2021 project, FKZ372171. T2 - Euroanalysis 2025 CY - Barcelona, Spain DA - 31.08.2025 KW - PFAS KW - TOP-Assay KW - Soil PY - 2025 AN - OPUS4-64666 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Lischka, Susanne A1 - Piechotta, Christian T1 - Analysis of arsenic species in fish after derivatization by GC-MS N2 - The derivatization of organoarsenic compounds by different reagents like thioglycolates or dithiols and the subsequent analysis by GC–MS as a molecular specific technique was investigated and described. The possible derivatization reagents methyl- and ethylthioglycolate (TGM and TGE), 1,3-propane- and 1,5-pentanedithiol (PDT and PeDT), which transfer the polar and nonvolatile analytes dimethylarsenate (DMA), monomethylarsonate (MMA), arsenite and arsenate into volatile compounds, were evaluated. The application for real samples like fish material was also studied. In addition the gas chromatographic separation and resolution was optimized and experiments were carried out to determine the highest derivatization rates. Derivatization reagents were evaluated in terms of quantity and stability of the formed chemical species. All derivatization products were characterized by mass spectrometry in order to identify the separated arsenic species. The most efficient conversion of DMA and MMA was observed by using ethylthioglycolate as derivatization agent. Finally, the derivatization procedure and the GC–MS-method were validated to determine linearity, precision, selectivity, analytical limiting values and recoveries. For the proposed method a limit of detection (LOD) of 5.8 pg for DMA and 14.0 pg for MMA was found. The accuracy was established by comparing the mean value measured for DMA in the certified reference material BCR-627 (tuna fish) with the certified one. MMA was not quantified in marine samples due to its low content. In shrimp samples DMA was not detectable. For codfish a DMA-content of 0.20±0.004 mg kg-1, for 'Surströmming' an amount of 0.38±0.02 mg kg-1 and for herring, which showed the highest amount of DMA, a content of 1.15±0.03 mg kg-1 was determined. KW - Arsenic species analysis KW - Monomethylarsonate KW - Dimethylarsenate KW - Derivatization KW - Gas chromatography KW - Mass spectrometry PY - 2012 DO - https://doi.org/10.1016/j.talanta.2012.10.021 SN - 0039-9140 VL - 101 SP - 524 EP - 529 PB - Elsevier CY - Amsterdam AN - OPUS4-26931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frenzel, Olivia A1 - Westphalen, Tanja A1 - Kaminski, Katja A1 - Kluge, Stephanie A1 - Bücker, Michael A1 - Piechotta, Christian T1 - Evaluation and Validation of an Accelerated Weathering Procedure to Characterise the Release of Bisphenol A from Polycarbonate Under Exposure to Simulated Environmental Conditions N2 - Bisphenol A (BPA) has been listed as a substance of very high concern (SVHC) due to its endocrine-disrupting properties according to REACH in 2017. European competent authorities have prepared a REACH restriction proposal to reduce BPA levels in the environment. The proposed limit for the concentration of free BPA and other bisphenols in articles is 10 mg kg−1. If exceeded, migration testing can demonstrate that no more than 0.04 mg L−1 is released from the product or material over its lifetime. German authorities are drafting a new restriction proposal after the original was temporarily withdrawn. The residual and migration limits mentioned above were key requirements from the previous restriction proposal. Numerous national and international standards exist for assessing how environmental factors affect the physical and chemical properties of products and materials—such as notch impact strength and tensile strength—but these standards do not cover the release of pollutants. A standardised procedure that covers all aspects of artificial weathering and monitors the subsequent release of pollutants is necessary, especially in the context of the regulation of these substances. An accelerated weathering procedure was established for non-protected samples. This material was not intended for outdoor applications. The testing procedure applied a typical weathering scenario that represents Central European climate conditions. The procedure was validated and applied to samples under distinct quality assurance aspects. Released BPA is quantified via an organic isotope dilution LC-MS/MS method. In parallel, identical samples were weathered outdoors on a weathering rack. Haze and yellowness index are measured to compare outdoor and weathering chamber results. KW - Artificial weathering KW - Polycarbonate KW - Bisphenol A KW - Simulated environmental conditions PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645020 DO - https://doi.org/10.3390/app151910361 SN - 2076-3417 VL - 15 IS - 19 SP - 1 EP - 15 PB - MDPI AG AN - OPUS4-64502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Bewitterungsszenarien im Vergleich – Veränderungen in der Oberflächenmorphologie von Polypropylen (PP) und Polystyrol (PS) unter dem Aspekt des Austrags von polybromierten Flammschutzmitteln N2 - In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification. Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil). The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials. Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere. N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz, die jeweils mit polybromierten Flammschutzmitteln (PBFSM) versehen sind. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Auch soll mit Hilfe der RFA und der LA-ICP-MS die Abreicherung der PBFSM in den Modellmaterialien beschrieben werden. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - 47. Jahrestagung der GUS 2018 CY - Stutensee - Blankenloch, Germany DA - 21.03.2018 KW - Polypropylen KW - Polystyrol KW - Flammschutzmittel KW - XRF KW - LA-ICP-MS PY - 2018 AN - OPUS4-47024 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -