TY - CONF A1 - Falkenhagen, Jana T1 - Challenges of sec and the necessity of round robin tests N2 - Size exclusion chromatography (SEC) is still the method of choice for determining the molar mass and molar mass distribution of macromolecules. From the distribution curve molar mass averages and the oligomer content (percentage of peak area smaller than 1000 g/mol and 500 g/mol) of polymers can be derived. The determination of oligomer content is important, because it is often used in regulatory contexts as a measure of small, mobile and potentially more toxic parts of the polymer. Polymer regulations are of increasing political and societal importance. Regulations often strive for narrow limits. But SEC has rather large error margins of 10-20% for the molar mass determination performed in different laboratories or on different instruments. These variances are well known to all experts and users and have been investigated in several round robin tests in the past. These resulted in DIN and ISO standards which, in our opinion, no longer meet today's requirements. Gaps have been identified that require further harmonization. Different polymer types or classes require different methods. On the other hand, as far as we know, the margins of error in determining oligomer content have not yet been investigated. It is expected that the variation will be rather high. This is because it depends on many factors related to the experimental conditions (column sets used, solvent, temperatures, sample preparation) on the one hand, and the data evaluation mechanisms (choice of baseline and peak limits) on the other. In order to actually measure the error margins and to support this with actual data a round robin test has been performed from June to November 2024 with approx. 40 participating laboratories. Three different solvents were selected, namely THF, DMAc or DMF and water. The samples were selected taking into account a wide range of practical aspects far from narrowly distributed standards: e.g higher distribution range, reduced solubility, included side components, copolymers and dispersions with gel content. In this contribution we will present the detailed concept of this round robin test and impressions T2 - 2025 Polymer Separations GNT meeting, Dow CY - Online meeting DA - 25.02.2025 KW - Polymers KW - Size exclusion chromatography KW - REACH PY - 2025 AN - OPUS4-63314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Fink, Friedrich T1 - Biobased and biodegradable polymers - sustainability and circular economy N2 - The presentation shows recent results on the synthesis and modification of environmentally relevant polymers based on renewable resources and the associated development of robust, high quality analytical methods. The first topic presents analytical results for star-shaped polylactides with different degrees of functionalisation. It is shown how liquid chromatography and mass spectrometry methods complement each other in a proven way to obtain accurate molar masses and to quantify chemically heterogeneous species. The second part presents an approach to incorporate lignin into epoxy matrices to obtain covalently adaptable epoxy networks that can be reprocessed and reused. T2 - 11th International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 21.01.2025 KW - Polylactides KW - Ligninbased thermosets KW - MALDI-TOF-MS KW - Gradient elution liquid adsorption chromatography KW - Atomic force spectroscopy KW - FT-IR PY - 2025 AN - OPUS4-62532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter T1 - Beiträge zur Charakterisierung von Polylactiden durch Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-MS T2 - Analytica Conference 2002 CY - Munich, Germany DA - 2002-04-23 PY - 2002 AN - OPUS4-3386 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter T1 - Hyphenated liquid-chromatographic, spectroscopic and spectrometric techniques for polymer characterization T2 - Polymerwerkstoffe 2006 CY - Halle (Saale), Germany DA - 2006-09-27 PY - 2006 AN - OPUS4-13808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Sample spot heterogeneity investigated by MALDI-imaging mass spectrometry T2 - 18th International Mass Spectrometry Conference CY - Bremen, Germany DA - 2009-08-30 PY - 2009 AN - OPUS4-19375 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fandrich, Nick T1 - Characterisation of new blocky copolymers of N-vinyl pyrrolidone and vinyl acetate by using of liquid chromatography and hyphenated techniques T2 - ExTech-HTC-Public Safety and Security Symposia CY - Bruges, Belgium DA - 2008-01-30 PY - 2008 AN - OPUS4-16398 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Identification of End Group Heterogeneity of Modified Polyamide 6.6 utilizing Two-Dimensional Chromatography/MALDI-MS T2 - 51st ASMS Conference CY - Montreal, Canada DA - 2003-06-08 PY - 2003 AN - OPUS4-4655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - A new two-dimensional approach for copolymer characterization by LC / MALDI- and LC / ESI-TOF-MS T2 - European Polymer Congress 2007 CY - Portorož, Slovenia DA - 2007-07-02 PY - 2007 AN - OPUS4-14702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - UPLC/ESI-MS and HPLC/MALDI-MS-Complementary devices for copolymer characterization T2 - 20th International Symposium on Polymer Analysis and Characterization CY - Crete, Greece DA - 2007-10-01 PY - 2007 AN - OPUS4-15465 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rittig, F. T1 - Characterization of Polyamides using new combined techniques T2 - Vortragstagung der Fachgruppe Makromolekulare Chemie der GDCh CY - Düsseldorf, Germany DA - 2004-03-15 PY - 2004 AN - OPUS4-11142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - LC / MALDI- and LC / ESI-TOF MS coupling for characterization of synthetic polymers T2 - ANAKON 2007 CY - Jena, Germany DA - 2007-03-27 PY - 2007 AN - OPUS4-14660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kricheldorf, H. R. T1 - Syntheses of Cyclic Polymers via the ROPPOC Approach N2 - Different strategies for the synthesis of polylactides were presented with special focus on Ring-opening Polymerization (ROP) and simultaneous ROP and Polycondensation (ROPPOC) mechanism. The mechanism of the formation of cyclic Polyesters is discussed in detail and established theories about the formation of cycles in polycondensation reactions are critically reviewed. T2 - DSM Competence Meeting CY - Dalfsen, The Netherlands DA - 12.11.2018 KW - Polylactide KW - MALDI-TOF mass spectrometry KW - Polycondensation KW - Cycles PY - 2018 AN - OPUS4-47027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate T1 - Charakterisierung der Umsetzung von OH-terminierten Oligomeren mit 3-(Isocyanatopropyl)trimethoxysilan mittels MALDI-TOF und FTIR T2 - 12. Kolloquium "MALDI und Synthetische Polymere" CY - Berlin, Germany DA - 2008-05-06 PY - 2008 AN - OPUS4-17505 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter T1 - Beiträge zur Charakterisierung von Polyatiden durch Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-MS T2 - Analytica Conference 2002 CY - Munich, Germany DA - 2002-04-23 PY - 2002 AN - OPUS4-3385 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - New approach for copolymer characterization using multidimensional coupling methods T2 - 10th Annual UNESCO / IUPAC Conference on Macromolecules & Materials CY - Mpumalanga, South Africa DA - 2008-09-07 PY - 2008 AN - OPUS4-17887 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abderrazak, H. T1 - Synthesis of new bio based adsorbent phases N2 - Over the years, industrial and human activities and agricultural practices have caused a serious threat to human health and the environment. Indeed, it has been demonstrated that these activities are responsible for the presence of pollutants in the soil, air and water. Water is one of the most strategic issues today, as it is associated with the living world. Therefore, water pollution is becoming a universal scourge that leads to environmental degradation, decrease of water quality and threatens public health. Water pollution is mainly due to the discharge of certain harmful chemical compounds that are not very or not at all biodegradable (phenolic compounds, heavy metals, hydrocarbons, dyes, pesticides, etc.) by various industries: chemical, pharmaceutical, textile, food processing, etc. The impact of these industrial effluents on fauna and flora is very harmful. A sensitization of the socio-economic actors and the public, accompanied by a severe regulation in relation to the discharges, would contribute to fight against this drift, but also, by the development of effective methods allowing to remove these pollutants, not only in an analytical purpose but also of depollution. Thus and within the framework of the preservation of an environment with regard to any anthropogenic activity, our research topic relates to the use of original biosourced polymeric phases for the extraction of the organic compounds and the heavy metals in aqueous mediums. Therefore, we have proceeded to the synthesis and characterization of a large variety of monomers, polymers and cross-linked materials. These products, partially derived from biomass, contain various functional groups with the ability to interact with chemical components without discriminating effect. The developed polymer phases have been successfully used for the adsorption of some organic pollutants and heavy metals in synthetic aqueous solutions. T2 - 12. Journees maghreb-europe. Matériaux et Applications aux Dispositifs et Capteurs CY - Monastir, Tunisia DA - 08.11.2022 KW - Organic-inorganic adsorbents KW - Semi-Interpenetrating Network KW - Poly(ether-sulfone) KW - Reversible adsorption. PY - 2022 AN - OPUS4-56286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Determination of molecular mass and molecular mass distribution of polymers by matrixassisted laser desorption/ionization - time of fightmass spectrometry (MALDI TOF MS) T2 - ISO TC 61/SC 5 Meeting CY - Yokohama, Japan DA - 2006-09-18 PY - 2006 AN - OPUS4-13822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Hyphenated coupling methods for polymer characterization and identification T2 - Dutch Polymer Workshop CY - Jena, Germany DA - 2013-12-09 PY - 2013 AN - OPUS4-30268 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter T1 - Charakterisierung von Si-Polymerarchitekturen durch Kopplung von flüssigchromatographischen Methoden mit der MALDI-TOF-Massenspektrometrie im DFG-Schwerpunktprogramm T2 - DFG-Kolloquium zum Schwerpunktprogramm "Silicium-Chemie" CY - Bielefeld, Germany DA - 1997-05-12 PY - 1997 AN - OPUS4-3443 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MassChrom2D zur Bestimmung der Zusammensetzung von Copolymeren aus MALDI und LC Daten T2 - 16. Kolloquium MALDI und Synthetische Polymere CY - Berlin, Germany DA - 2012-05-08 PY - 2012 AN - OPUS4-26135 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Liquid Adsorption Chromatography near Critical Conditions of Adsorption coupled with Matrix-assisted Laser Desorption / ionization Mass Spectrometry T2 - 47th Conference of The American Society of Mass Spectrometry CY - Dallas, TX, USA DA - 1999-06-11 PY - 1999 AN - OPUS4-2240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Zweidimensionale Charakterisierung von PA 6.6 durch Kopplung von LAC und MALDI-MS T2 - 7. Kolloquium "MALDI und synthetische Polymere" CY - Berlin, Germany DA - 2003-05-13 PY - 2003 AN - OPUS4-3094 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI TOF MS zur Aufklärung von Kristallisationsprozessen in Polyestern N2 - MALDI TOF Massenspektrometrie wurde verwendet, um Kristallisationsprozesse in Polyestern (Polylactide, Polyglycolide) zu untersuchen. Dabei konnte gezeigt werden, dass Zyklen und Linearen simultan, aber in unterschiedlichen Kristalliten, kristallisieren. Die dabei ablaufenden Umesterungen (Transesterifizierungen) konnten mit der MALDI TOF Massenspektrometrie nachgewiesen werden. Damit wurde ein völlig neues Anwendungsgebiet dieser MS Methode demonstriert. T2 - 28. Kolloquium Massenspektrometrie von Polymeren CY - Berlin, Germany DA - 14.05.2024 KW - MALDI TOF MS KW - Bioabbaubare Polymere KW - Crystallinity PY - 2024 AN - OPUS4-60029 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Abbau und Zersetzungsverhalten von Polymeren und Komposit‐ Materialien auf Polyurethanbasis N2 - Polyurethane zeichnen sich durch ihre große Flexibilität des Anwendungsbereiches aus. Im Rahmen dieses Vortrags wird ein neues Themenfeldprojekt der BAM vorgestellt und erste Ergebnisse präsentiert. T2 - Deutsche Gesellschaft für Materialprüfung, Fachausschuss Polymerwerkstoffe CY - Darmstadt, Germany DA - 10.11.2016 KW - Polyurethane KW - Abbauverhalten PY - 2016 AN - OPUS4-38332 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kricheldorf, H. R. T1 - Cyclization and dispersity of polyesters N2 - Starting out from Flory`s most probable Distribution concept, correct and incorrect evaluations of SEC measurements are discussed. Using the correct mode, polyesters prepared by irreversible and reversible polycondensation methods were studied. Polyesters of α,ω−alkanediols and isophthalic acid or polyesters of diphenols and sebacic acid were prepared by three different irreversible polyconcensation methods. Formation of cyclic oligo and polyesters was monitored by MALDI-TOF mass spectrometry and dispersities were measured by SEC. The results are compared with the theories of Flory and Odian. Eqilibrated polyesters were prepared by reversible polycondensation of ethyl 6-hydroxycaproate or by alcohol-initiated ring-opening polymerization of ε-caprolactone. Various catalysts were compared. The influence of dilution and of di- or multifunctional initiators was evaluated. Furthermore, equilibrated polylactides were prepared from L- or meso-lactide at 120, 160 and 180°C. A fast even-odd equilibration was discovered in addition to reversible cyclization and intermolecular transesterification. The influence of these different equilibration mechanisms on the dispersity was investigated. The preparative and theoretical consequences are discussed. T2 - Polycondensation 2016 CY - Moscow, Russia DA - 11.09.2016 KW - Polyester KW - Cyclization KW - MALDI-TOF MS KW - SEC PY - 2016 AN - OPUS4-38365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Entmischungsphänomene in der MALDI dried-droplet Probenpräparation und deren Vermeidung T2 - Anakon 2015 CY - Graz (Österreich) DA - 2015-03-23 PY - 2015 AN - OPUS4-33053 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -