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 DO - 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 - Piechotta, Christian T1 - Development of an enzymatic digestion method for the quantification of mercury species in biota and fish N2 - The toxicity and transport mechanisms of mercury and its species in the environment are dependent on the chemical form. Here, the knowledge of the species analysis of organic and inorganic mercury compounds is of interest. Only measuring the total mercury content gives just a little information about the potential risk to human beings and the health of biota and fish respectively. In comparison methyl mercury is the more toxic species than the inorganic form due to its solubility in lipids and it binds strongly to bio ligands like sulfur containing amino acids bound in proteins. This could affect the functionality of enzymes. A variety of analytical methods have been used for the measurement of mercury species like liquid and gas chromatographic separation and the detection by inductively coupled plasma mass spectrometry and common electron impact mass spectrometry. T2 - Workshop on mercury monitoring and regulation CY - Berlin, Germany DA - 04.04.2017 KW - Methyl mercury KW - Enzymatic digestion KW - Fish PY - 2017 AN - OPUS4-40246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Umweltverträglichkeit und -beständigkeit von Materialien und Produkten hinsichtlich der Migration von Schadstoffen N2 - Gegenstand des Projekts 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 Polycarbonat, Polytetrafluorethylen, Polystyrol und Polypropylen zum Einsatz. 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. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden, die es gestatten, Schnellprüfverfahren zu etablieren, die die Simulation der realen Beanspruchungen im Zeitraffermodell anwendbar machen. Somit sollen standardisierbare Schnellbean-spruchungsverfahren erarbeitet werden, die als Prüfeinrichtungen etabliert werden und von externen Auftraggebern zur Prüfung der Umweltbeständigkeit und -verträglichkeit von neuen Materialien genutzt werden können. Die Umweltwirkungen (chemisch-physikalisch und mikrobiologisch) sollen so definiert eingesetzt werden, dass eine reproduzierbare Prüfung möglich wird. Aus diesen Verfahren und Methoden sollen Normen abgeleitet werden, die eine standardisierte Materialprüfung ermöglichen. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Materialien KW - Freisetzung KW - Umweltschadstoffe PY - 2017 AN - OPUS4-40247 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Identifizierung und analytische Charakterisierung von unbekannten Arsenolipiden in Hering T2 - CANAS - Colloquium Analytische Atomspektroskopie CY - Leipzig, Germany DA - 2015-03-08 PY - 2015 AN - OPUS4-33545 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Neue Methoden zur Arsenspezies-Analyse in Wasser und Biotaproben T2 - Anakon 2015 CY - Graz, Austria DA - 2015-03-23 PY - 2015 AN - OPUS4-33546 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Sojref, Regine A1 - Nguyen, Thi Yen A1 - Piechotta, Christian T1 - Immobilization of photocatalytically active TiO2 nanopowder by high shear granulation N2 - Nano-TiO2 powder is known to show high photocatalytic reactivity in the degradation of several organic pollutants. In thiswork, the powderwas fixed on the surface of SiO2 granuleswith the size of several micrometers using a high shear granulation process. Nanozirconia sol was applied as an inorganic binder. When the samples were tempered at 300 °C, they showed high stability in an aqueous solution for several hours. An energy dispersive x-ray spectroscopy (EDX) analysis confirmed that the cores and shells of the granules consisted solely of SiO2 and TiO2 respectively, and that ZrO2 was found throughout the whole granules. Methylene blue (MB) was employed as amodel systemto evaluate the photocatalytic activity of the TiO2 nanopowder and coated granules. Itwas shown that the TiO2-coated granules lead to the degradation ofMB under UV irradiation,whereas no effect was observed in the dark. After the Degradation experiments the granules could be recovered and they remained active for further applications. KW - Heterogeneous photocatalysis KW - Water treatment KW - Advanced oxidation KW - Nanozirconia KW - Methylene blue PY - 2017 DO - https://doi.org/10.1016/j.powtec.2017.06.025 SN - 0032-5910 SN - 1873-328X VL - 318 SP - 465 EP - 470 AN - OPUS4-41608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Arsenic and Mercury speciation in fish T2 - GSF Speciation 2008 CY - Munich, Germany DA - 2008-05-25 PY - 2008 AN - OPUS4-17790 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Determination and quantification of LAS-siomers using GC-MS and GC-FID T2 - ICS 2008 CY - Münster, Germany DA - 2008-09-21 PY - 2008 AN - OPUS4-17791 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Hyphenated techniques for the analysis of linear alkylbenzenesulfonates in technical formulation T2 - ISC 2010 CY - Valencia, Spain DA - 2010-09-12 PY - 2010 AN - OPUS4-21851 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhlich, Paul A1 - Göstl, Robert A1 - Metzinger, R. A1 - Piechotta, Christian A1 - Nehls, Irene T1 - 3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydro-2-naphthoic acid (AHTN-COOH) KW - AHTN KW - Tonalide KW - Cyclilc musk KW - AHTN-COOH KW - Disinfection by-product KW - Haloform reaction PY - 2010 DO - https://doi.org/10.1107/S1600536810038572 SN - 1600-5368 VL - 66 IS - 10 SP - o2687, sup-1 - sup-12 PB - Munksgaard CY - Copenhagen AN - OPUS4-23006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Commercial Linear AlkylbenzeneSulfonate (LAS) - Analysis by GC-FID/MS and 1H-qNMR - T2 - 5. Conference über Ionenanalyse CY - Berlin, Germany DA - 2009-03-02 PY - 2009 AN - OPUS4-19017 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Determination of Tributyltin (TBT) at sub-ppt level in waters samples T2 - TraceSpec 2009 CY - Mainz, Germany DA - 2009-09-15 PY - 2009 AN - OPUS4-19977 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Commercial Linear Alkylbenzene Sulonates (LAS)-Analysis by GC-FID/MS- T2 - WetPol 2009 CY - Barcelona, Spain DA - 2009-09-21 PY - 2009 AN - OPUS4-19978 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 DO - 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 - CONF A1 - Piechotta, Christian T1 - Determination of Tributyltin (TBT) at Sub-ppt Level in Whole Water Samples T2 - The Future of Reference Materials - Science and Innovation - IRMM CY - Geel, Belgium DA - 2010-11-23 PY - 2010 AN - OPUS4-22457 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Quantification of Tributyltin (TBT) at Sub-ppt Level in Whole Water Samples T2 - Canas 2011 CY - Leipzig, Germany DA - 2011-03-13 PY - 2011 AN - OPUS4-23249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Chemische Brandspurenanalytik - Methoden zum Nachweis von Brandbeschleunigern in Brandrückständen T2 - ANAKON 2011 CY - Zurich, Switzerland DA - 2011-03-22 PY - 2011 AN - OPUS4-23251 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Janzen, R. A1 - Sperling, M. A1 - Buscher, W. A1 - Bösel, A. A1 - Ehlbeck, J. A1 - Lischka, Susanne A1 - Piechotta, Christian T1 - Spezies-Analyse von Quecksilber-, Zinn- und Bleiverbindungen - Neues GC-MIP-OES-System N2 - Quecksilber-, Blei- und Zinnverbindungen gehören aufgrund Ihrer Toxizität zu den bedrohlichsten Umweltkontaminationen. Dabei können besonders die organischen Verbindungen bereits in kleinsten Mengen überaus schwerwiegende Folgen für Lebewesen verursachen. Während die anorganischen (mineralischen) Verbindungen dieser Elemente auch durch natürliche Prozesse wie Erosion aus Gestein und durch Vulkanismus in die Umwelt eingetragen werden, entstehen die meisten Kontaminationen der Umwelt aufgrund ihres jahrzehntelangen weltweiten Einsatzes in verschiedenen Pestiziden, Antifouling Anstrichen, Treibstoffen und zahlreichen industriellen Großprozessen, sowie ihrer Emission bei der Verfeuerung fossiler Brennstoffe. KW - GC-PED KW - Methylquecksilber KW - MIP PY - 2011 SN - 0016-3538 VL - 1 SP - 22 EP - 27 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-23374 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhlich, Paul A1 - Göstl, Robert A1 - Teichert, Philip A1 - Piechotta, Christian A1 - Nehls, Irene T1 - Transformations of polycyclic musks AHTN and HHCB upon disinfection with hypochlorite: two new chlorinated disinfection by-products (CDBP) of AHTN and a possible source for HHCB-lactone N2 - In this work, the behavior of the polycyclic musks 6-acetyl-1,1,2,4,4,7-hexamethyltetraline (AHTN) and 1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethylcyclopenta- γ-2-benzopyran (HHCB) was investigated upon disinfection by using sodium hypochlorite as disinfectant in a model disinfection basin in order to find new disinfection byproducts (DBP). In the case of AHTN, the carboxylic acid 3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalene-2- carboxylic acid (AHTN-COOH) was generated by a haloform reaction, being the origin for two new chlorinated DBPs. In the case of HHCB, disinfection via hypochlorite led to the HHCB-lactone. All reaction products and intermediates were synthesized and isolated. The relevant degradation mechanisms are discussed in detail. KW - Musk KW - AHTN KW - HHCB KW - HHCB-lactone KW - Chlorination KW - Disinfection PY - 2011 DO - https://doi.org/10.1007/s00216-011-4674-3 SN - 1618-2642 SN - 1618-2650 VL - 399 IS - 10 SP - 3579 EP - 3588 PB - Springer CY - Berlin AN - OPUS4-23622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Determination and Quantification of LAS-isomers using GC-MS and GC-FID T2 - EMEC 9 CY - Girona, Spain DA - 2008-12-03 PY - 2008 AN - OPUS4-18394 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimm, T. A1 - Kleine-Benne, E. A1 - Senz, R. A1 - Piechotta, Christian T1 - Stoffwechselprozesse analysieren und überwachen KW - SPME KW - GC KW - Stoffwechselprodukte PY - 2008 SN - 0344-1733 SN - 1610-8256 IS - 10 SP - 46 EP - 49 PB - Vogel CY - Würzburg AN - OPUS4-18431 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Garbe, L.A. A1 - Würtz, A. A1 - Piechotta, Christian A1 - Tressl, R. T1 - The Peptide-catalyzed Maillard Reaction - Characterization of 13C Reductones N2 - The reaction pathways of amino acids and reducing sugars are now fully understood. The focus in the last few years, however, has turned to the reaction of peptides and proteins with reducing sugars. We have investigated the reaction of γ-aminobutanoic acid, the heptapeptide Nα-Acetyl-Lys-Lys-β-Ala-Lys-β-Ala-Lys-Gly, and the model protein β-casein in Maillard reactions with 1-13C arabinose. Characterization of 13C-labeled acetic acid and norfuraneol by gas chromatography–mass spectrometry and nuclear magnetic resonance revealed new formation pathways. The results demonstrate significant differences in the labeling pattern of the products depending on the amine used, indicating different formation pathways of acetic acid and norfuraneol. KW - Norfuraneol KW - 13C labeling KW - Pathway KW - Casein KW - Peptide PY - 2008 DO - https://doi.org/10.1196/annals.1433.046 SN - 0077-8923 SN - 1749-6632 SN - 0094-8500 VL - 1126 SP - 244 EP - 247 PB - New York Academy of Sciences CY - New York, NY AN - OPUS4-18432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Screening von aeroben mikrobiellen Konversionsvorgängen in Biotransformationen, Abbau- und Stoffwechselprozessen mit direkter GC-SPME-Analytik T2 - ANAKON 2009 CY - Berlin, Germany DA - 2009-03-17 PY - 2009 AN - OPUS4-20775 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Becker, Roland A1 - Jung, Christian A1 - Piechotta, Christian A1 - Nehls, Irene T1 - Investigation of extraction procedures and HPLC-DAD/MS for the determination of the brominated flame retardant tetrabromobisphenol A bis(2,3-dibromopropylether) in environmental samples N2 - A method for the determination of the novel brominated flame retardant tetrabromobisphenol A bis(2,3-dibromopropylether), 1,1'-(isopropylidene)bis[3,5-dibromo-4-(2,3-dibromo-propoxy)-benzene] (TBBPA-dbpe), was developed. Technical TBBPA-dbpe was purified and the results of a thorough physical characterisation are reported. The application of APCI-MS is discussed and the fragmentation patterns are described. Quantification of TBBPA-dbpe was done by HPLC-DAD using external calibration. The validation of the method was accomplished using sediment and sewage sludge samples spiked with defined amounts of authentic TBBPA-dbpe. The average recovery rates of TBBPA-dbpe from spiked samples ranged from 35 to 91% (sediment) and from 57 to 98% (sewage sludge) depending on the respective extraction method. Pressurised fluid extraction (PFE) and fluidised bed extraction were superior to classical Soxhlet and sonication procedures and yielded recovery rates between 90 and 98% with relative standard deviations of 2%. The limits of detection (DTC), identification (ID) and determination (DTM) using HPLC-DAD were 10, 21 and 30 ng g-1 in sediment and 22, 44 and 72 ng g-1 in sewage sludge, respectively. KW - Extraction KW - TBBPA-dbpe KW - Sewage sludge KW - Sediment KW - LC-MS KW - Mass spectrometry KW - APCI KW - HPLC-DAD PY - 2006 DO - https://doi.org/10.1007/s00216-006-0339-z SN - 1618-2642 SN - 1618-2650 VL - 384 IS - 7-8 SP - 1485 EP - 1492 PB - Springer CY - Berlin AN - OPUS4-12255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Bestimmung von CAS in Klärschlämmen T2 - Jahrestagung 2006 der GDCh, Fachgruppe "Umweltchemie und Ökotoxikologie", Martin-Luther-Universität Halle-Wittenberg CY - Halle (Saale), Germany DA - 2006-10-04 PY - 2006 AN - OPUS4-12428 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Methylquecksilber-Bestimmung in Fischmatrizes mittels massenspektrometrischer Methoden T2 - 12. Varian-MS-Anwendertreffen, Akademie Schloss Hohenkammer CY - Hohenkammer, Germany DA - 2007-01-16 PY - 2007 AN - OPUS4-14306 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Arsen- und Quecksilberspezies in Fisch T2 - 4. Conference über Ionenanalyse, Technische Universität Berlin CY - Berlin, Germany DA - 2007-03-12 PY - 2007 AN - OPUS4-14307 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Entwicklung eines LAS-Kalibrierstandards T2 - 4. Conference über Ionenanalyse CY - Berlin, Germany DA - 2007-03-12 PY - 2007 AN - OPUS4-14308 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Bestimmung toxikologisch relevanter Schwermetall-Spezies in Fisch T2 - 36. Deutscher Lebensmittelchemikertag 2007 CY - Nuremberg, Germany DA - 2007-09-10 PY - 2007 AN - OPUS4-14605 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Synthetic linear alkylbenzenesulfonates (LAS) as calibration standard T2 - EUROanalysis XIV CY - Antwerp, Belgium DA - 2007-09-09 PY - 2007 AN - OPUS4-14772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Development and validation of a method for the quantification of tributyltin at subnanogram per liter concentrations T2 - TraceSpec 2007 CY - Münster, Germany DA - 2007-09-04 PY - 2007 AN - OPUS4-14816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Lineare Alkylbenzolsulfonate (LAS) - Die Entwicklung eines Kalibrierstandards T2 - Jahrestagung 2007, Umweltchemie und Ökotoxikologie, Von der Chemodynamik in Ökosystemen zur Stoffbewertung CY - Osnabrück, Germany DA - 2007-09-26 PY - 2007 AN - OPUS4-14817 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Sebastian A1 - Piechotta, Christian A1 - Godejohann, M. A1 - Win, Tin A1 - Nehls, Irene A1 - Mügge, C. T1 - Characterisation of commercially available linear alkylbenzenesulfonates by LC-SPE-NMR/MS (liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectroscopy) N2 - Commercially available linear alkylbenzenesulfonates (LASs) are a mixture of various homologues and isomers, leading to 20 major species. In this work we investigated the commercial product by liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectrometry (LC-SPE-NMR/MS). The commercial product was separated into 17 fractions by liquid chromatography (LC). After chromatographic separation, 5% of the flow was split to a mass spectrometer (MS) while 95% was send to post-column solid phase extraction cartridges for enrichment of the analytes (LC-SPE). After elution from the SPE-cartridges a NMR-spectrometer equipped with a cryo-probe was used for the characterisation of the different LASs species. For the first time H-1-1D and H-H-COSY spectra for 14 LASs species out of 20 major isomers are presented, whereas the 6 remaining species are detected as mixtures in 3 H-1-1D and H-H-COSY spectra. These data were used to correlate the chromatographic retention of the LASs isomers to the substitution pattern of the alkyl chain. KW - Linear alkylbenzenesulfonates KW - NMR KW - SPE KW - Liquid chromatography KW - Mass spectrometry KW - Surfactants PY - 2010 DO - https://doi.org/10.1016/j.talanta.2010.04.011 SN - 0039-9140 VL - 82 IS - 1 SP - 143 EP - 150 PB - Elsevier CY - Amsterdam AN - OPUS4-24004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faust, R. A1 - Nauroozi, D. A1 - Bruhn, C. A1 - Koch, B. A1 - Kuhlich, Paul A1 - Piechotta, Christian A1 - Nehls, Irene T1 - (3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)methanol: a possible metabolite of the synthetic musk fragrance AHTN N2 - The title compound (AHTN-OH), C17H26O, was prepared in order to provide standard materials for the qualitative and quantitative analysis of environmental pollutants. The molecule possesses a chiral C atom, although the structure determination was performed on racemic material, expressed in the structure as disordered chiral sites. The asymmetric unit consists of four AHTN-OH molecules containing an hydroxy group and forming a tetrameric cyclic motif built up by four strong hydrogen bonds between these hydroxy groups and additionally by two weak C–H···π interactions. Furthermore, these tetramers are linked via very weak C–H···π interactions, forming chains along the c axis. PY - 2011 DO - https://doi.org/10.1107/S1600536811018009 SN - 1600-5368 VL - 67 SP - o1462-o1463, sup1-15 PB - Munksgaard CY - Copenhagen AN - OPUS4-24310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - A New Approach for the Characterization of Commercial Linear Alkylbenzene Sulfonate (LAS) T2 - 5. Conference über Ionenanalyse (CIA) CY - Berlin, Germany DA - 2011-09-26 PY - 2011 AN - OPUS4-24371 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lischka, Susanne A1 - Körte, F. A1 - Faust, R. A1 - Nehls, Irene A1 - Piechotta, Christian T1 - Synthesis, characterization and application of a two-fold 13C-labeled calibration standard for the analysis of arsenobetaine using HPLC-ESI-MS/MS without high resolution mass spectrometry N2 - A procedure has been developed for the determination of arsenobetaine in fish matrix by HPLC–ESI-MS/MS. Hereby (trimethylarsonium)-1,2-13C-acetate (arsenobetaine) is used as internal calibration standard. Arsenobetaine was determined in a fish material (Sea Bass) with an expanded uncertainty of 3.8%. KW - Arsenobetaine KW - ESI-MS/MS KW - Isotopic labeled KW - 13C PY - 2011 DO - https://doi.org/10.1016/j.talanta.2011.07.047 SN - 0039-9140 VL - 85 IS - 4 SP - 1996 EP - 1999 PB - Elsevier CY - Amsterdam AN - OPUS4-25163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Simone A1 - Deubel, Jan A1 - Raspe, Tina A1 - Fettig, Ina A1 - Piechotta, Christian T1 - Chemische Brandspurenanalytik T2 - Vfdb 2012 -Jahresfachtagung CY - Köln, Deutschland DA - 2012-05-21 KW - Brandbeschleuniger KW - Brandgase KW - Brand KW - Partikel KW - Analytik PY - 2012 SP - 517 EP - 539 PB - VdS Schadenverhütung CY - Köln AN - OPUS4-25933 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Analyse von perfluorierten Chemikalien - LC-MS vs. GC-MS T2 - LC-MS in der Umweltanalytik 2012 CY - Leipzig, Germany DA - 2012-06-11 PY - 2012 AN - OPUS4-26048 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Simone A1 - Deubel, Jan A1 - Werrel, Martin A1 - Fettig, Ina A1 - Raspe, Tina A1 - Piechotta, Christian T1 - Experimental studies on the effect of fire accelerant during living room fires N2 - The influence of fire accelerants on the fire behavior during living room fires was experimentally investigated by performing 5 different room fire scenarios. During the tests flre-technological quantities were determined as well as chemical-analytical studies were carried out. The focus was on the detection of smoke gases and the proof of used fire accelerants. The evaluation of traceable fire accelerants and the reconstruction of the fire development are based on a precise Chemical analysis of the combustion products. In this work an innovative methodology was developed to combine available analyticai techniques to draw conclusions from solid, liquid and gaseous fire residues about the fire process. Each ofthe fire rooms was equipped with the same living room inventory. The location and amount of fire accelerant (a mixture of diesel/gasoline) differed in 4 of 5 tests. Orte room fire experiment was carried out without fire accelerant. The following fire technological characteristics were determined during the room fire experiments: mass loss (of the complete room), temperatures (at several locations in the room), heat release and smoke gas emission (measured at three different locations: in the chimney, in the fire room and at the door opening). While the smoke gases were analysed by using Fourier Transform Infrared spectroscopy, the fire residues and swipe samples (particles) were examined by Headspace-Solid Phase Microextraction- Gaschromatography-Mass spectrometry. These procedures make it possible to detect low concentrations of volatile components of the fire accelerants. The Chemical analyticai results of the fire accelerant detection are presented. T2 - Fire and materials 2013 - 13th International conference and exhibition CY - San Francisco, CA, USA DA - 28.01.2013 KW - Accelerant KW - Chemical analysis KW - Toxicity PY - 2013 SP - 729 EP - 743 PB - Interscience Communications CY - London, UK AN - OPUS4-27708 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 - 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 - Roesch, Philipp A1 - Vogel, Christian A1 - Wittwer, Philipp A1 - Huthwelker, T. A1 - Borca, C. A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Piechotta, Christian A1 - Kalbe, Ute A1 - Simon, Franz-Georg T1 - Taking a Look at the Surface: µ-XRF Mapping and Fluorine K-edge µ-XANES Spectroscopy of Organofluorinated Compounds in Environmental Samples and Consumer Products N2 - For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples. KW - PFAS KW - XRF KW - LC-MS/MS KW - XANES KW - Fluoride KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576109 DO - https://doi.org/10.1039/D3EM00107E SN - 2050-7887 SP - 1 EP - 12 PB - Royal Society of Chemistry AN - OPUS4-57610 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 - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Piechotta, Christian A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Herzel, Hannes A1 - Huthwelker, T. A1 - Borca, C. A1 - Simon, Franz-Georg T1 - Levels of per- and polyfluoroalkyl substances (PFAS) in various wastewater-derived fertilizers - Analytical investigations from different perspectives N2 - Solid wastewater-based fertilizers were screened for per- and polyfluoroalkyl substances (PFAS) by the extractable organic fluorine (EOF) sum parameter method. The EOF values for ten sewage sludges from Germany and Switzerland range from 154 to 7209 mg kg−1. For thermal treated sewage sludge and struvite the EOF were lower with values up to 121 mg kg−1. Moreover, the application of PFAS targeted and suspect screening analysis of selected sewage sludge samples showed that only a small part of the EOF sum parameter values can be explained by the usually screened legacy PFAS. The hitherto unknown part of EOF sum parameter contains also fluorinated pesticides, pharmaceutical and aromatic compounds. Because these partly fluorinated compounds can degrade to (ultra-)short PFAS in wastewater treatment plants they should be considered as significant sources of organic fluorine in the environment. The combined results of sum parameter analysis and suspect screening reveal the need to update current regulations, such as the German fertilizer ordinance, to focus not solely on a few selected PFAS such as perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) but consider an additional sum parameter approach as a more holistic alternative. Moreover, diffusion gradient in thin-films (DGT) passive samplers were utilized as an alternative simplified extraction method for PFAS in solid wastewater-based fertilizers and subsequently quantified via combustion ion chromatography. However, the DGT method was less sensitive and only comparable to the EOF values of the fertilizers in samples with >150 mg kg−1, because of different diffusion properties for various PFAS, but also kinetic exchange limitations. KW - Combustion ion chromatography KW - Per- and polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Fertilizer PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583429 DO - https://doi.org/10.1039/d3va00178d SN - 2754-7000 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-58342 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 A1 - Iznaguen, Hassan A1 - Traub, Heike A1 - Feldmann, Ines A1 - Köppen, Robert A1 - Witt, Angelika A1 - Jung, Christian A1 - Becker, Roland A1 - Oleszak, Katrin A1 - Bücker, Michael A1 - Urban, Klaus A1 - Reger, Christian A1 - Ostermann, Markus T1 - Bewitterungsszenarien im Vergleich – Veränderungen in der Oberflächenmorphologie von Polypropylen (PP) und Polystyrol (PS) unter dem Aspekt des Austrags von polybromierten Flammschutzmitteln N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit 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. 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. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - 47. Jahrestagung der GUS CY - Blankenloch-Stutensee, Germany DA - 21.03.2018 KW - Schadstoffaustrag KW - Umweltsimulation KW - Bewitterung PY - 2018 SN - 978-981-18507-2-7 VL - 47 SP - 115 EP - 128 AN - OPUS4-49802 LA - deu 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 - TY - CONF A1 - Piechotta, Christian T1 - TF-Projekt MaUS: Material und Umweltsimulation N2 - Gegenstand des Projekts 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 Polycarbonat, Polytetrafluorethylen, Polystyrol und Polypropylen zum Einsatz. 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. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden, die es gestatten, Schnellprüfverfahren zu etablieren, die die Simulation der realen Beanspruchungen im Zeitraffermodell anwendbar machen. Somit sollen standardisierbare Schnellbeanspruchungs-verfahren erarbeitet werden, die als Prüfeinrichtungen etabliert werden und von externen Auftraggebern zur Prüfung der Umweltbeständigkeit und -verträglichkeit von neuen Materialien genutzt werden können. Die Umweltwirkungen (chemisch-physikalisch und mikrobiologisch) sollen so definiert eingesetzt werden, dass eine reproduzierbare Prüfung möglich wird. Aus diesen Verfahren und Methoden sollen Normen abgeleitet werden, die eine standardisierte Materialprüfung ermöglichen. T2 - Projektmeeting BAM - Covestro CY - Leverkusen, Germany DA - 29.05.2018 KW - Umweltsimulation KW - Schadstoffaustrag PY - 2018 AN - OPUS4-47025 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Mülow-Stollin, Ulrike A1 - Hering, S. A1 - Richter, Janine A1 - Piechotta, Christian A1 - Paul, Andrea A1 - Braun, Ulrike T1 - A first pilot study on the sorption of environmental pollutants on various microplastic materials N2 - With the drastic increase in plastic production, the input of plastic particles into the environment has become a recognised problem. Xenobiotics are able to sorb to polymer materials, and this process is further enhanced where they Encounter microplastics (plastic fragments <5 mm). In this work we studied the sorption of metformin, a type-2 diabetes drug, and difenoconazole, a fungicide, onto the virgin polymer materials polyamide (PA), polypropylene (PP), and polystyrene (PS). Additionally, PP was cryo-milled and PA was treated with acid to investigate the influence of an increase in surface area and chemical modification. The material properties were also studied by dynamic scanning calorimetry (DSC), gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FTIR). Sorption experiments were performed on the basis of a full factorial design examining the effect of agitation, pH value, and salinity. Experimental results showed that difenoconazole sorbs readily to all microplastics, whereas the more polar analyte metformin did not show any affinity to the materials used. For difenoconazole the governing factor in all cases is agitation, while both pH and salinity exhibited only a slight influence. The modification of polymers leads to enhanced sorption, indicating that an increase in surface area (cryo-milled PP) or inner volume (acid-treated PA) strongly favours adsorption. Moreover, long-term experiments demonstrated that the time until equilibrium is reached depends strongly on the particle size. KW - Difenoconazole KW - Metformin KW - Plastic debris KW - Polymer KW - Dynamic scanning calorimetry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-402393 DO - https://doi.org/10.4172/2380-2391.1000191 SN - 2380-2391 VL - 4 IS - 1 SP - Article 1000191, 1 EP - 8 PB - Omics International CY - Los Angeles AN - OPUS4-40239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Environmental sustainability and –stability of Materials concerning the Migration of pollutants N2 - MaUS is an acronym for ”Material und Umweltsimulationen“. Plastics are in the focus of environmental politics due to their long-term behaviour and therefore to their persistence. Not only that they appear as visible contaminants in the sea and on the beach, but their unknown behaviour concerning their additives as well as the related transformation products are anxious. Therefore, we wish to establish a certified reference method to provide a method for testing plastics. Aim of this project is the development of fast motion standard reference methods for testing plastics regarding to their environmental compatibility. To establish these testing methods, we use polystyrene (PS) and polypropylene (PP) with environmental relevant brominated flame retardants, known for their persistent bioaccumulative and toxic (PBT) properties. In case of PS the material contains 1 wt% of 1,2,5,6,9,10-hexabromocyclododecan (HBCD) and in case of PP 0.1 wt% bromodiphenylether (BDE-209), which is known as a substance of very high concern (SVHC). Furthermore, we use polycarbonate (PC), which is still used as material in baby flasks and releases Bisphenol A (BPA), an estrogenic active substance. As an additional material PTFE is used for its importance as a source for two ubiquitous environmental substances (PFOS and PFOA), whose toxicological effects are still incompletely known. The focus in this current work is set on the transfer of potential pollutants out of applied materials mentioned above into environmental compartments like water or soil. Here an accelerated aging concept should be developed to shortened time consuming natural processes. For these resulting simulations we use a programmable weathering chamber with dry and wet periods and with high and low temperatures. These programmes run for several weeks and according to a defined sampling schedule we take water samples, run a clean-up procedure by SPE (Molecular imprinted polymers (MiPs) resp. polymer-based cartridges (Waters Oasis HLB)) and analyse them by HPLC-UV resp. LC-MS/MS. Of most interest in case of flame retardants are photocatalytic transformation products. Therefore, we conduct a non-target-screening resp. a suspected target-screening by LC-MS/MS and HRMS. T2 - Project meeting PlasticsEurope - BAM CY - Leverkusen, Germany DA - 06.11.2018 KW - Environmental simulation KW - Pollutants PY - 2018 AN - OPUS4-47026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Kick-off meeting “18NRM01-EDC-WFD” N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD “Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive” aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - EMPIR Kick-off meeting EDC-WFD CY - Paris, France DA - 07.10.2019 KW - Estrogens KW - Reliable measurements KW - Effect based Method KW - Comparability KW - MS based method PY - 2019 AN - OPUS4-49741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - NSO-Heterozyklen – Zwischen Rattengift und Normung N2 - Warfarin als ein Vertreter der NSO-Hetereozyklen, ist seit den 1950er Jahren einer der bekanntesten Gerinnungshemmer. Beim Menschen wird es bis heute zur Vorbeugung von Thrombose und der Behandlung von Vorhofflimmern und Arrhythmie eingesetzt. Doch schon einige Jahre vor der FDA Zulassung als Medikament wurde es zur Bekämpfung von Nagetieren eingesetzt. Bis heute wurde es nur teilweise durch weitaus wirksamere antikoagulante Rodentizide (ARs) der zweiten Generation, sogenannte Superwarfarine, ersetzt. In der Fachliteratur finden sich zahlreiche Beispiele für sekundäre und tertiäre Vergiftung mit ARs bei Wildtieren und anderen Nichtzieltieren. Bisher ist relativ wenig über die Bioakkumulation, Persistenz und Toxizität von ARs und deren Transformationsprodukten (TPs) in der terrestrischen und aquatischen Umwelt, sowie der Nahrungskette bekannt. Um Einblicke in mögliche Transformations- und Abbauprozesse von Warfarin zu erhalten und um Umwelteinflüsse zu simulieren, wurde es in einer elektrochemischen Reaktorzelle oxidativ umgesetzt und mittels Massenspektrometrie analysiert. Hinsichtlich der Wasseraufbereitung in Kläranlagen wurden technisch relevante Simulationsverfahren wie Chlorung, UV-Bestrahlung und Ozonung angewendet um potentielle Eliminierungswege aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt, massenspektrometrisch analysiert und verglichen. T2 - MS-Tage CY - Düsseldorf, Germany DA - 03.12.2019 KW - GC-MS KW - Warfarin KW - NSO-Heterozyklen PY - 2019 AN - OPUS4-49974 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 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit 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. 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 (polybromierte Flammschutzmittel) 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. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - Kolloquium "Aquatische Ökologie" CY - Essen, Germany DA - 27.11.2019 KW - Umweltsimulation KW - PBFSM KW - LA-ICP-MS KW - RFA PY - 2019 AN - OPUS4-49975 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Changes in polymer surface morphology and leaching of brominated flame retardants induced by different weathering scenarios N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt.% hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) 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 raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching 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. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - BFR KW - LA-ICP-MS KW - XRF KW - Polymer PY - 2019 N1 - Folien in deutscher Sprache, Votrag, Titel und Abtract in englischer Sprache AN - OPUS4-49796 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Environmental sustainability and –stability of materials concerning the migration of pollutants N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) 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 raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching 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. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - Goldschmidt 2019 CY - Barcelona, Spain DA - 18.08.2019 KW - Pollutants KW - Environmental simulation KW - Migration PY - 2019 AN - OPUS4-49803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Identification of Transformation Products of Warfarin N2 - Warfarin, also known as Coumadin is one of the most popular anticoagulant drugs used as a therapeutic in humans to prevent thrombosis, atrial fibrosis, and fibrillation since the 1950s. Because of its ability to hinder blood from clotting by blocking vitamin K-depending carboxylation of blood clotting precursors, it is also used as a rodenticide worldwide. Until today it has been partially substituted by far more potent anticoagulant rodenticides (ARs), so-called superwarfarins. There are numerous references confirming secondary and tertiary poisoning in non-target-animals and wildlife like mammals, birds, and fish associated with ARs. Up to now relatively little is known about persistence and toxicity of transformation products of those AR in the environment and food chain. Herein, warfarin was chosen as a model compound to determine andelucidate TPs which are generated technically and under environment-like conditions. Such as the simulation of the oxidative phase I metabolism by implementing electrochemical flow cells coupled to mass spectrometry (MS). Obtained results are being compared to TPs generated by UVB-irradiation and ozonation. Analysis and separation of degradation products and TPs were achieved by a variety of gas- and liquid chromatographic techniques coupled to (high resolution) MS. T2 - Goldschmidt 2019 CY - Barcelona, Spain DA - 18.08.2019 KW - GC-MS KW - Warfarin KW - Transformations products PY - 2019 AN - OPUS4-49795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Beschreibung des Verhaltens von organischen Schadstoffen unter umweltrelevanten Bedingungen N2 - Zu den letzten beiden Jahrestagungen der GUS wurden Verfahren und Methoden vorgestellt, die es gestatten, den Transfer von Schadstoffen aus Materialien und Produkten in die Umwelt unter umweltrelevanten Bedingungen beschreiben zu können. Dabei lag der Fokus auf den Materialien und der eingesetzten Umweltsimulationen. In einem sich anschließenden Schritt soll nun das Verhalten der freigesetzten organischen Schadstoffe unter den Bedingungen von realen und simulierten Umwelteinflüssen charakterisiert und beschrieben werden. Hier werden im Detail drei potentielle Schadstoffe betrachtet, die Inhaltsstoffe bzw. Additive in den jeweils eingesetzten Materialien sind. Im Falle von Polypropylen (PP) und Polystyrol (PS) handelt es sich um polybromierte Flammschutzmittel BDE 209 (Decabrom-diphenylether, als Einzelsubstanz) und HBCD (Hexabromcyclododecan, als technische Formulierung). Für das eingesetzte Polycarbonat ist BPA (Bisphenol A) als Schadstoff zu definieren, welcher unter umweltrelevanten Bedingungen freigesetzt wird. Im Rahmen der durchzuführenden Arbeiten sollen die aufgeführten prioritären Schadstoffe hinsichtlich möglicher Transformationsprozesse in Umwelt und Klärwerk charakterisiert werden. Die unter den Bedingungen der Ozonung, Chlorierung und UV-Bestrahlung erhaltenen Transformationsprodukte (TPs) sollen im Sinne einer Non-Target-Analytik identifiziert und eindeutig charakterisiert werden. Die Ergebnisse sollen mittels vorhandener Analysenverfahren, wie GC-EI-MS, HPLC-ESI-IT-MSn bzw. LC-MS/MS erzeugt bzw. abgesichert werden. Anhand der in der Struktur eindeutig zu beschreibenden Transformationsprodukte und der Charakterisierung von potentiellen Intermediaten sollen belastbare Reaktionswege und –mechanismen abgeleitet werden. T2 - 48. Jahrestagung der GUS CY - Blankenloch-Stutensee, Germany DA - 27.03.2019 KW - Transformationsprodukte KW - Schadstoffe KW - Umweltverhalten PY - 2019 AN - OPUS4-49799 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Weathering of flame-protected polymers and monitoring of the release of brominated flame retardants under different scenarios N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt.% hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) 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 raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching 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. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - SETAC Glb 2019 CY - Landau, Germany DA - 04.09.2019 KW - Polymer KW - XRF KW - LA-ICP-MS KW - BFR PY - 2019 AN - OPUS4-49797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. D. A1 - Choteau, T. A1 - Martos, G. A1 - Wielgosz, R. A1 - Sarzuri, Y. A. A1 - Mendoza, E. A1 - do Rego, E. C. P. A1 - Violante, F. G. M. A1 - da Silva Souza, W. A1 - de Carvalho, L. J. A1 - Fernandes, J. L. N. A1 - Bates, J. A1 - Rajotte, I. A1 - Melanson, J. E. A1 - Li, H. A1 - Guo, Z. A1 - Su, F. A1 - Wang, S. A1 - Huang, T. A1 - Lalerle, B. A1 - Gantois, F. A1 - Piechotta, Christian A1 - Philipp, Rosemarie A1 - Kaminski, Katja A1 - Klyk-Seitz, Urzsula-Anna A1 - Giannikopoulou, P. A1 - Skotidaki, E. A1 - Kakoulides, E. A1 - Pui-Kwan, C. A1 - Kuroe, M. A1 - Itoh, N. A1 - Calderón, M. A. A. A1 - Contreras, L. R. A1 - Osuna, M. A. A1 - Alrashed, M. A1 - Ting, L. A1 - Mei, G. E. A1 - Juan, W. A1 - Sze, C. P. A1 - Lin, T. T. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Ahn, S. A1 - Chaiphet, T. A1 - Sudsiri, N. A1 - Bellazreg, W. A1 - Bilsel, M. A1 - Colombo, G. T1 - Key comparison CCQM-K78.b - non-polar analytes in organic solvent: methoxychlor and trifluralin in acetonitrile N2 - The CCQM-K78.b key comparison was coordinated by the Bureau International des Poids et Mesures (BIPM) on behalf of the CCQM Organic Analysis Working Group (OAWG) of the 'Comité Consultatif pour la Quantité de Matière' (CCQM), for National Measurement Institutes (NMIs) and Designated Institutes (DIs) providing measurement services in organic analysis under the 'Comité International des Poids et Mesures' (CIPM) Mutual Recognition Arrangement (MRA). This key comparison was conducted as a 'Track A' comparison within the OAWG's 10-year strategic plan. The goal of CCQM-K78.b was to underpin capabilities for the value assignment of calibration solutions containing low polarity/non-polar organic analytes in organic solvents. The selected model system consisted of a two-component pesticide solution in acetonitrile, comprising methoxychlor and trifluralin. Participants were tasked with assigning the mass fractions, in units of μg/g, of methoxychlor and trifluralin in acetonitrile solution. The mass fraction levels and analytical challenges of the selected analytes were representative of those encountered for calibration solutions of non-polar organic analytes. Participation in CCQM-K78.b allowed for the benchmarking of capabilities for assigning the mass fraction of non-polar organic compounds (pKow < -2) in solution, at mass fractions above 5 μg/g, in an organic solvent. Additionally, the comparison assessed the capabilities for the quantitative assignment of thermally labile compounds. Participants were provided by the BIPM with ampoules containing methoxychlor and trifluralin in acetonitrile. Each participant reported the mass fraction content of each analyte in μg/g. All participants ensured the metrological traceability of their results through the use of a Primary Reference Material (PRM), which was used to prepare a primary calibrator solution for each analyte using a gravimetric procedure. The twenty participating institutes primarily used analysis procedures based on GC-MS, -IDMS, -MS/MS, -ECD, and -FID, with some participants also using LC-UV for the value assignment. The analysis of methoxychlor and trifluralin in acetonitrile solution presented several challenges, including the thermal stability of the analytes under selected analytical techniques, control of solvent volatility, and considerable variation in some results using MS-based quantification methods. The mass fraction assignments for methoxychlor and trifluralin, consistent with the key comparison reference values (KCRVs), were achieved with associated relative standard uncertainties of (0.38 - 2.9) % for methoxychlor and (0.35 - 2.5) % for trifluralin. 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 - Methoxychlor KW - Trifluralin KW - CCQM KW - Key comparison PY - 2025 DO - https://doi.org/10.1088/0026-1394/62/1A/08010 SN - 0026-1394 VL - 62 IS - 1A SP - 1 EP - 37 PB - IOP Publishing AN - OPUS4-64691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhlich, Paul A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Nehls, Irene A1 - Piechotta, Christian T1 - 1-(4-bromo-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one: a precursor for phase-I metabolite of AHTN N2 - The title compound, C18H25BrO, crystallized as a racemate with four independent molecules in the asymmetric unit. In the crystal, three of these four molecules are linked via C-Br...Br-C halogen bonds [Br...Br = 3.662 (2) and 3.652 (2) Å], forming dimers. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-279935 DO - https://doi.org/10.1107/S1600536813006934 SN - 1600-5368 VL - 69 IS - 4 SP - o545, sup-1 EP - sup-17 PB - Munksgaard CY - Copenhagen AN - OPUS4-27993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhlich, Paul A1 - Emmerling, Franziska A1 - Piechotta, Christian A1 - Nehls, Irene T1 - Methyl 3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalene-2-carboxylate (AHTN-COOMe) N2 - Crystals of the title compound, C18H26O2, were grown from ethyl acetate. Due to the racemic precursor, the title compound is also obtained as a racemate. Disorder was observed during structure refinement, originating from two possible half-chair conformations of the non-aromatic ring. The disorder was refined by introducing split positions in the cyclo-hexane ring regarding the two possible R and S-enantiomers at the chiral CH group [ratio 0.744 (3):0.256 (3)]. The crystal structure features pairs of inversion-related molecules connected by pairs of non-classical C–H···O hydrogen bonds. KW - AHTN KW - Tonalide KW - Cyclic musk KW - AHTN-COOMe KW - Disinfection by-product KW - Esterification PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-232769 DO - https://doi.org/10.1107/S1600536811002601 SN - 1600-5368 VL - E67 IS - 2 SP - o485, sup-1 EP - sup-11 PB - Munksgaard CY - Copenhagen AN - OPUS4-23276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bandow, N. A1 - Aitken, M. D. A1 - Geburtig, Anja A1 - Kalbe, Ute A1 - Piechotta, Christian A1 - Schoknecht, Ute A1 - Simon, Franz-Georg A1 - Stephan, Ina T1 - Using Environmental Simulations to Test the Release of Hazardous Substances from Polymer-Based Products: Are Realism and Pragmatism Mutually Exclusive Objectives? N2 - The potential release of hazardous substances from polymer-based products is currently in the focus of environmental policy. Environmental simulations are applied to expose such products to selected aging conditions and to investigate release processes. Commonly applied aging exposure types such as solar and UV radiation in combination with water contact, corrosive gases, and soil contact as well as expected general effects on polymers and additional ingredients of polymer-based products are described. The release of substances is based on mass-transfer processes to the material surfaces. Experimental approaches to investigate transport processes that are caused by water contact are presented. For tailoring the tests, relevant aging exposure types and release quantification methods must be combined appropriately. Several studies on the release of hazardous substances such as metals, polyaromatic hydrocarbons, flame retardants, antioxidants, and carbon nanotubes from polymers are summarized exemplarily. Differences between natural and artificial exposure tests are discussed and demonstrated for the release of flame retardants from several polymers and for biocides from paints. Requirements and limitations to apply results from short-term artificial environmental exposure tests to predict long-term environmental behavior of polymers are presented. KW - Environmental simulations KW - Polymer-based products KW - Artificial weathering KW - Degradation KW - Leaching KW - Soil contact PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509310 DO - https://doi.org/10.3390/ma13122709 SN - 1996-1944 VL - 13 IS - 12 SP - Paper 2709, 22 PB - MDPI CY - Basel, Switzerland AN - OPUS4-50931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Entwicklung, Validierung und Anwendung eines beschleunigten Bewitterungsprotokolls zur Bewertung der Freisetzung von Bisphenol A (BPA) aus Polycarbonat (PC)-Materialien in die Umwelt N2 - BPA unterliegt einer kontinuierlichen behördlichen Kontrolle und ist als besonders besorgniserregender Stoff (SVHC) gelistet. Besondere Besorgnis besteht hinsichtlich seines häufigen Nachweises in Oberflächengewässern, obwohl es leicht biologisch abbaubar ist. In mehreren Studien wurden die Quellen und Wege von BPA in die Umwelt untersucht, wobei festgestellt wurde, dass seine Hauptverwendung als Monomer in PC nur marginal zu den BPA-Freisetzungen in die Umwelt über seinen Lebenszyklus beiträgt. Um die tatsächlichen Freisetzungen von BPA aus PC unter umweltrelevanten Bedingungen besser zu verstehen, wurde eine neu entwickelte Methodik (Bundesanstalt für Materialforschung und -prüfung, BAM) angewendet, die ein neuartiges beschleunigtes Bewitterungsprotokoll für Polycarbonat-Materialien in Kombination mit einem sensitiven Analysenverfahren umfasst, welches eine Bestimmung von BPA im Ultraspurenbereich ermöglicht. Das Bewitterungsprotokoll erreicht eine 13,6-fache Beschleunigung im Vergleich zu mitteleuropäischen Wetterbedingungen und simuliert Umweltstressoren (globale Strahlung, Regen, Temperaturschwankungen) in einer Bewitterungskammer, wobei gleichzeitig die BPA-Freisetzung mit einem validierten LC-MS/MS-Verfahren unter Verwendung einer organischen Isotopenverdünnungskalibrierung bestimmt wird. In parallelen Freilandversuchen wurden die Trübung und die Vergilbung („Yellowness-Index“) der zu untersuchenden Proben als Referenzparameter untersucht. T2 - 54. Jahrestagung der GUS 2026 CY - Blankenloch-Stutensee, Germany DA - 25.03.2026 KW - Bewitterung KW - Bisphenol A KW - Polycarbonat PY - 2026 AN - OPUS4-65794 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -