TY - JOUR A1 - Fink, Friedrich A1 - Emmerling, Franziska A1 - Falkenhagen, Jana T1 - Identification and Classification of Technical Lignins by means of Principle Component Analysis and k-Nearest Neighbor Algorithm N2 - The characterization of technical lignins is a key step for the efficient use and processing of this material into valuable chemicals and for quality control. In this study 31 lignin samples were prepared from different biomass sources (hardwood, softwood, straw, grass) and different pulping processes (sulfite, Kraft, organosolv). Each lignin was analysed by attenuated total reflectance Fourier transform infrared (ATR-FT-IR) spectroscopy. Statistical analysis of the ATR-FT-IR spectra by means of principal component analysis (PCA) showed significant differences between the lignins. Hence, the samples can be separated by PCA according to the original biomass. The differences observed in the ATR-FT-IR spectra result primarily from the relative ratios of the p-hydroxyphenyl, guaiacyl and syringyl units. Only limited influence of the pulping process is reflected by the spectral data. The spectra do not differ between samples processed by Kraft or organosolv processes. Lignosulfonates are clearly distinguishable by ATR-FT-IR from the other samples. For the classification a model was created using the k-nearest neighbor (k NN) algorithm. Different data pretreatment steps were compared for k=1…20. For validation purposes, a 5-fold cross-validation was chosen and the different quality criteria Accuracy (Acc), Error Rate (Err), Sensitivity (TPR) and specificity (TNR) were introduced. The optimized model for k=4 gives values for Acc = 98.9 %, Err = 1.1 %, TPR = 99.2 % and TNR = 99.6 %. KW - Classification KW - PCA KW - K-nearest neighbor KW - FT-IR KW - Technical lignin PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533855 DO - https://doi.org/10.1002/cmtd.202100028 VL - 1 IS - 8 SP - 350 EP - 396 PB - Wiley-VCH GmbH AN - OPUS4-53385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Falkenhagen, Jana A1 - Weidner, Steffen ED - Barner-Kowollik, C. ED - Gründling, T. ED - Falkenhagen, Jana ED - Weidner, Steffen T1 - Hyphenated techniques N2 - Hyphenation of techniques has become a versatile tool in polymer analysis. It has been demonstrated that the complexity and heterogeneity of modern polymers and copolymers, in particular, could only be determined by a combination of several methods. With this regard, a chromatographic separation in various thermodynamic modes combined with mass spectral identification of polymer species provides new insights in polymer synthesis, modification, and degradation. Both methods are widely complementary and can therefore often compensate each other’s drawbacks. The development of suitable coupling interfaces, the introduction of AP devices, and an increasing application of ESI pushed polymer analysis toward new regions. Future developments in the field of MS detectors, lasers and software, as well new pressure-stable stationary chromatographic phases will aid in increasing the importance and acceptance of LC-MS coupling methods and will enable new applications in sophisticated polymer analysis. KW - MALDI KW - Chromatography KW - Coupling techniques PY - 2012 SN - 978-3-527-32924-3 SN - 978-3-527-64182-6 DO - https://doi.org/10.1002/9783527641826.ch7 SP - 209 EP - 235 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Polymer characterisation by multidimensional techniques with focus on LC - MALDI/ESI-TOF-MS N2 - Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development. The lecture will give a general survey of different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry. Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces the polydispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame. On the basis of different examples on- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed. Recently, MALDI imaging techniques in coupling with chromatography have become interesting e.g. for visualization of copolymer composition. T2 - International Symposium GPC/SEC and Related Techniques CY - Amsterdam, The Netherlands DA - 26.09.2016 KW - Polymers KW - Liquid chromatography KW - MALDI-TOF-MS KW - ESI-TOF-MS PY - 2016 AN - OPUS4-37629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Much, Helmut A1 - Krüger, Ralph-Peter A1 - Friedrich, Jörg Florian T1 - Determination of chemical and molecular-weight distributions of heterogeneous polymers by means of MALDI-MS coupled with chromatography T2 - 219th ACS national meeting CY - San Francisco, CA, USA DA - 2000-03-26 PY - 2000 SN - 0032-3934 VL - 41 IS - 1 SP - 655 EP - 656 PB - American Chemical Society CY - Newark, NJ AN - OPUS4-2169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Much, Helmut A1 - Schulz, Günter A1 - Friedrich, Jörg Florian T1 - Beiträge zur Charakterisierung von synthetischen Si-Polymeren durch Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-MS T2 - DFG-Symposium zum Schwerpunktprogramm "Silicium-Chemie" CY - Werfenweng, Österreich DA - 2000-09-27 PY - 2000 AN - OPUS4-2251 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Kombinierte Trenn- und Detektionstechniken: Neue Aspekte und Probleme T2 - Seminar der Abteilung VI "Funktion von Polymeren", BAM CY - Berlin, Germany DA - 2004-06-03 PY - 2004 AN - OPUS4-5531 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupling of chromatographic and spectrometric techniques for polymer characterization N2 - Presentation of coupling of polymer chromatography and polymer mass spectrometry based on different examples. T2 - Kolloquium CY - Universität für Bodenkultur, Wien, Austria DA - 14.06.2019 KW - LCCC KW - Mass spectrometry of polymers KW - LC x MALDI/ESI-TOF-MS KW - Liquid chromatography of polymers PY - 2019 AN - OPUS4-48223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Maier, Bärbel A1 - Much, Helmut A1 - Schulz, Günter T1 - Orthogonal two-dimensional chromatography of poly(ethylene oxid) adducts T2 - HPLC '96 CY - San Francisco, CA, USA DA - 1996-06-16 PY - 1996 CY - San Francisco AN - OPUS4-2221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Synthesis and Characterization of Polyhedral Silsesquioxanes with Nanotubular Structures T2 - DFG-Schwerpunktprogramm "Nanodrähte und Nanoröhren" CY - Bad Honnef, Germany DA - 2004-01-23 PY - 2004 AN - OPUS4-4338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Falkenhagen, Jana T1 - Combined impact of UV radiation and nitric acid (HNO3) on HDPE jerrycans – comparison of outdoor and lab test N2 - A damaging action of HNO3-55% only occurs in combination with its decomposition into nitrous gases, which can be caused by UV radiation. In a laboratory test, transparent HDPE jerrycans have been exposed to both UV radiation and 55 wt-% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The respective damages are compared with FTIR spectroscopy in ATR and HT-gel permeation chromatography (GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. The gradual increase in oxidative damage shows the good reproducibility of the lab exposure. The decomposition of nitric acid into nitrous gases by UV radiation – as well as the jerrycan oxidation – is also observed at lower HNO3 concentration (28 wt- %). Similar results are obtained after outdoor tests. Again, the damage occurs only after combined exposure, in contrast to the exposures to UV only and to HNO3 only, which were conducted in parallel. Outdoor exposures are most readily accepted as they represent possible end-use conditions. However, the reproducibility of these exposures is poor due to the large temporal variations in weather. There are also several safety risks, which is why the number of replicates remains limited. Since the outdoor and lab exposure tests show the same qualitative results, it is appropriate to conduct systematic studies in the laboratory. After 6 days of lab exposure, the oxidation damage is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. It should be noted that this amount can also occur in two sunny weeks. T2 - 24th iapri World Packaging Conference CY - Valencia, Spain DA - 17.06.2024 KW - Ppolyethylene KW - UV exposure KW - Nitric acid KW - Oxidation PY - 2024 VL - 2 SP - 30 EP - 37 PB - ITENE AN - OPUS4-60414 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupling of chromatographic and spectrometric techniques for polymer characterization N2 - Coupling of chromatographic and spectrometric techniques for polymer characterization; focus topics: LCxMALDI-TOF-MS and UPLC x ESI-TOF-MS T2 - 16. Tagung des Arbeitskreises Polymeranalytik CY - Online meeting DA - 22.03.2022 KW - Liquid chromatography KW - Mass spectrometry KW - Polymers KW - Two-dimensional chromatography (2D-LC) PY - 2022 AN - OPUS4-54567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - 70 years size exclusion chromatography - An ongoing challenge N2 - The reason for our current activities is that polymers may also be subject to REACh regulations in the future. In this context, the determination of oligomer content is important. SEC is still the method of choice for determining molar mass distribution. The regulations aim for narrow limits and SEC has rather large error margins, which are well known to all experts. Different polymers need different methods. What to do when samples with a wide range of practical aspects, samples with higher distribution range, reduced solubility, including side components, gel content etc. need be analyzed? A concept for round robin tests and first impressions will be presented. T2 - Analytical Solutions 2025 CY - Ede, Netherlands DA - 04.06.2025 KW - Polymers KW - Size exclusion chromatography KW - REACH KW - Round Robin Tests PY - 2025 AN - OPUS4-63310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization and identification of new polymer structures by optimization and coupling of HPLC and MALDI-TOF-MS T2 - Diskussionstagung der DECHEMA, Neue Methoden der Polymeranalytik CY - Mainz, Germany DA - 2001-04-02 PY - 2001 AN - OPUS4-3366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krüger, Ralph-Peter A1 - Heinemann, M. A1 - Falkenhagen, Jana A1 - Hartmann, A. A1 - Friedrich, Jörg Florian A1 - Fritz, H.-G. ED - Fritz, H. ED - Eisenbach, C. T1 - Charakterisierung biologisch abbaubarer Homo- und Copolyester / Characterisation of biodegradable Homo- and Copolyesters T2 - 19. Stuttgarter Kunststoff-Kolloquium 2005 CY - Stuttgart, Deutschland DA - 2005-03-09 KW - MALDI-TOF-MS KW - Bioabbaubare Polyester KW - Flüssigchromatographie KW - Methodenkopplung KW - Biodegradable polyesters KW - Liquid chromatography KW - Coupling of analytical methods PY - 2005 SN - 3-00-015246-6 SP - 5/P1-1 - 5/P1-9 PB - IKT CY - Stuttgart AN - OPUS4-11767 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of copolyesters by coupling of liquid chromatography with MALDI and ESI mass spectrometry T2 - National Institute of Standards & Technology Polymer Mass Spectrometry Workshop CY - Gaithersburg, MD, USA DA - 2005-11-09 PY - 2005 AN - OPUS4-11544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Polymer characterization by combination of chromatographic techniques coupled with MALDI and ESI mass spectrometry T2 - Analytica Conference 2006 CY - Munich, Germany DA - 2006-04-25 PY - 2006 AN - OPUS4-12384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupling of liquid-chromatographic, spectroscopic and spectrometric techniques for polymer characterization T2 - Polydays CY - Berlin, Germany DA - 2006-10-04 PY - 2006 AN - OPUS4-12377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Friedrich, Jörg Florian A1 - Krüger, Ralph-Peter A1 - Schulz, Günter A1 - Much, Helmut T1 - Liquid Adsorption Chromatography near Critical Conditions of Adsorption coupled with Matrix-assisted Laser/Ionization Mass Spectrometry T2 - 47th ASMS Conference on Mass Spectrometry and Allied Topics CY - Dallas, TX, USA DA - 1999-06-13 PY - 1999 CY - Dallas, Tex AN - OPUS4-2165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Friedrich, Jörg Florian A1 - Much, Helmut A1 - Schulz, Günter A1 - Falkenhagen, Jana T1 - Zur Charakterisierung von Si-Polymeren durch Kopplung flüssigchromatographischer Arbeitsweisen mit der MALDI-TOF-MS T2 - DFG-Symposium zum Schwerpunktprogramm "Silicium-Chemie" CY - Bielefeld, Deutschland DA - 1999-05-09 PY - 1999 AN - OPUS4-2239 LA - deu 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 - 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 - 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 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Much, Helmut A1 - Schulz, Günter A1 - Friedrich, Jörg Florian T1 - Beiträge zur Charakterisierung von synthetischen Si-Polymeren durch Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-MS T2 - Incom 2001 - International Symposium on Instrumentalized Analytical Chemistry and Computer Technology CY - Düsseldorf, Deutschland DA - 2001-03-27 PY - 2001 AN - OPUS4-2254 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Much, Helmut A1 - Schulz, Günter A1 - Weidner, Steffen T1 - Charakterisierung von synthetischen Polymeren durch Kopplung flüssigchromato-graphischer Trennmethoden mit der MALDI-TOF-Massenspektrometrie T2 - 1. Berliner Werkstofftag CY - Berlin, Deutschland DA - 1999-09-16 PY - 1999 AN - OPUS4-2242 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Weidner, Steffen ED - Grellmann, W. T1 - Characterization and identification of new polymer structures by optimization and coupling of HPLC and MALDI-TOF-MS T2 - Polymerwerkstoffe 2000 CY - Halle (Saale), Germany DA - 2000-09-25 PY - 2000 SN - 3-86010-605-8 PB - Martin-Luther-Univ. CY - Halle AN - OPUS4-2250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radke, W. A1 - Falkenhagen, Jana ED - Haddad, P.R. ED - Poole, C.F. ED - Fanali, S. ED - Schoenmakers, P. ED - Lloyd, D. T1 - Liquid interaction chromatography of polymers N2 - In the last decade, the use of interaction chromatography and hyphenated techniques has become increasingly important for the characterization of polymeric materials. Interaction chromatography allows separation by other structural features than molar mass, while hyphenation with mass spectroscopy or spectroscopic techniques provides detailed characterization of the separated chromatographic fractions. This chapter gives an overview of the principles and applications of interaction chromatography and the information that can be determined by hyphenation of polymer chromatography with mass spectrometry and spectroscopic techniques. KW - Polymer chromatography KW - Gradient chromatography KW - Critical chromatography KW - SEC-gradients KW - 2D-chromatography KW - Hyphenation KW - MALDI KW - ESI KW - LC-FTIR KW - LC-NMR PY - 2013 SN - 978-0-12-415806-1 DO - https://doi.org/10.1016/B978-0-12-415806-1.00005-X IS - Chapter 5 SP - 1 EP - 46 PB - Elsevier AN - OPUS4-27909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Weidner, Steffen A1 - Falkenhagen, Jana ED - Li, L. T1 - LC-MALDI MS for polymer characterization KW - Mass spectrometry KW - Polymers PY - 2010 SN - 978-0-471-77579-9 N1 - Serientitel: Chemical analysis: a series of monographs on analytical chemistry and its applications – Series title: Chemical analysis: a series of monographs on analytical chemistry and its applications VL - 175 IS - Chapter 11 SP - 247 EP - 265 PB - John Wiley & Sons AN - OPUS4-26406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gähde, J. A1 - Friedrich, Jörg Florian A1 - Fischer, T. A1 - Unger, Wolfgang A1 - Lippitz, Andreas A1 - Falkenhagen, Jana T1 - Reactions of polymer analogous model substances with metals and oxides KW - Modellverbindung KW - Al202 KW - Chrom KW - Orientierung, molekular KW - Chemical interaction KW - Model compounds KW - Al2O3 and chromium KW - Molecular orientation KW - Formation of complexes KW - Plasma PY - 1996 SN - 0340-255x SN - 1437-8027 VL - 101 SP - 194 EP - 198 PB - Springer CY - Berlin AN - OPUS4-685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Charakterisierung von synthetischen Polymeren mit komplexen Strukturen durch HPLC / MALDI-MS-Kopplung T2 - Makromolekulares Kolloquium, DKI CY - Darmstadt, Germany DA - 2002-07-05 PY - 2002 AN - OPUS4-1799 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Polylactidanalytik T2 - Fachgruppenvollversammlung BAM CY - Berlin, Germany DA - 2002-01-29 PY - 2002 AN - OPUS4-2192 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Möglichkeiten zur Polymercharakterisierung durch die Anwendung verschiedener HPLC-Modi in Kopplung mit der MALDI-TOF-MS T2 - WGE Polymertreffen 1999 CY - Potsdam, Germany DA - 1999-05-06 PY - 1999 AN - OPUS4-11129 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - New Aspects of Characterization of Polymer Structures by Coupling of Different HPLC Modes with MALDI-TOF-MS T2 - Workshop on Mass Spectrometry of Polymers CY - Catania, Italy DA - 1999-12-01 PY - 1999 AN - OPUS4-11132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Investigations of Polymer Structures Using Chromatographic and Spectroscopic Techniques T2 - Esparation and Characterization of Macromolecules CY - Bratislava, Slovakia DA - 1999-07-04 PY - 1999 AN - OPUS4-11131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Falkenhagen, Jana A1 - Panne, Ulrich A1 - Hiller, W. A1 - Gruendling, T. A1 - Staal, B. A1 - Lang, C. A1 - Lamprou, A. T1 - Simultaneous characterization of poly(acrylic acid) andpolysaccharide polymers and copolymers N2 - Copolymer products that result from grafting acrylic acid and other hydrophilicmonomers onto polysaccharides have recently gained significant interest in researchand industry. Originating from renewable sources, these biodegradable, low toxicity,and polar copolymer products exhibit potential to replace polymers from fossil sourcesin several applications and industries. The methods usually employed to character-ize these copolymers are, however, quite limited, especially for the measurement ofbulk properties. With more sophisticated applications, for example, in pharmaceu-tics requiring a more detailed analysis of the chemical structure, we describe a newapproach for this kind of complex polymers. Our approach utilizes chromatographyin combination with several detection methods to separate and characterize reactionproducts of the copolymerization of acrylic acid and chemically hydrolyzed starch.These samples consisted of a mixture of homopolymer poly (acrylic acid), homopoly-mer hydrolyzed starch, and – in a lower amount – the formed copolymers. Several chro-matographic methods exist that are capable of characterizing either poly (acrylic acid)or hydrolyzed starch. In contrast, our approach offers simultaneous characterization ofboth polymers. The combination of LC and UV/RI offered insight into the compositionand copolymer content of the samples. Size exclusion chromatography experimentsrevealed the molar mass distribution of homopolymers and copolymers. FTIR inves-tigations confirmed the formation of copolymers while ESI-MS gave more details onthe end groups of hydrolyzed starches and poly (acrylic acids). Evidence of copolymerstructures was obtained through NMR measurements. Finally, two-dimensional chro-matography led to the separation of the copolymers from both homopolymers as wellas the additional separation of sodium clusters. The methods described in this work area powerful toolset to characterize copolymerization products of hydrolyzed starch andpoly(acrylic acid). Together, our approach successfully correlates the physicochemicalproperties of such complex mixtures with their actual composition. KW - 2D chromatography KW - LC-MS KW - SEC KW - Renewable copolymers KW - Grafting PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508873 DO - https://doi.org/10.1002/ansa.202000044 SP - 1 EP - 12 PB - Wiley-VCH Verlag-GmbH&Co. KGaA CY - Weinheim AN - OPUS4-50887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Barner‐Kowollik, C. A1 - Falkenhagen, Jana A1 - Gründling, T. A1 - Weidner, Steffen ED - Barner-Kowollik, C. ED - Gründling, T. ED - Falkenhagen, Jana ED - Weidner, Steffen T1 - Outlook N2 - The synthesis of macromolecules of an increasing architectural diversity and complexity is the lifeblood of modern macromolecular chemistry, allowing for specialized applications in fields ranging from industrial coatings to medical drug delivery systems. The high complexity of modern polymers with regard to molar mass, chemical functionality, composition, and topology requires a versatile technique for their comprehensive characterization. Today, mass spectrometry, in combination with the soft ionization techniques ESI and MALDI, has been established as an extremely valuable tool for the analysis of polymeric materials. KW - Mass spectrometry KW - Polymers PY - 2012 SN - 978-3-527-32924-3 SN - 978-3-527-64182-6 DO - https://doi.org/10.1002/9783527641826.ch14 SP - 467 EP - 468 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana T1 - Characterization of Polyesters and Copolyesters by Coupled Liquid Chromatographic and Spectroscopic Techniques T2 - Polydays 2004 CY - Potsdam, Germany DA - 2004-10-04 PY - 2004 AN - OPUS4-4341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Falkenhagen, Jana A1 - Beskers, Timo. F. A1 - Myxa, Anett A1 - Pursch, Matthias T1 - Round-robin test for size exclusion chromatography – Data summary N2 - Size exclusion chromatography (SEC or GPC) is one critical component of polymer analysis to meet the increasing requirements in regulatory context – namely, determination of Mn, as well as oligomers of less than 500 g mol-1 and 1000 g mol-1. The underlying test methods (OECD 118/119 and DIN EN ISO 13885 1 to 3) provide a framework for SEC measurements; however, they lack sufficient specificity to obtain accurate results. Previous SEC round robin tests were mostly performed on homopolymers and did not collect data on oligomer contents. A new round robin test was initiated and conceptualized within the Task force “Method Evaluation for Polymer REACh (MeEP)”, an initiative of “Industrieforum Analytik” within the German Chemical Society (GDCh). Samples for this study were selected to represent both easy benchmark polymers as well as real-life, industry-relevant polymer materials. Data collection focused on the regulatory requirements. Distribution of samples, gathering of individual results and evaluation were carried out by BAM. A data summary as initial result is reported here. Further evaluation and interpretation are a part of ongoing research. KW - Size exclusion chromatography KW - Polymers KW - Oligomer content KW - Round-robin test PY - 2026 DO - https://doi.org/10.26272/opus4-65587 SP - 1 EP - 84 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-65587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hoskins, Jessica A1 - Falkenhagen, Jana A1 - Weidner, Steffen ED - Udomkichdecha, W. ED - Böllinghaus, Thomas ED - Manonukul, A. ED - Lexow, J. T1 - Characterization of randomly branched polymers utilizing liquid chromatography and mass spectrometry N2 - Branching in polymers is an important way to modify the materials properties, however the characterization of random branching in polymeric materials is a challenge in polymer analysis. In this work, liquid adsorption chromatography methods are developed for a commercially available hyperbranched polyester (Boltorn™). This Chromatographie techniques was then coupled to offline MALDI-TOF MS analysis, a first in the analysis of randomly branched polymers. The coupling of these two techniques provides superior MALDI-TOF spectra, enabling the easy identification of structural subdistributons based on theoretical molecular weight. Detailed analysis of the MALDI-TOF spectra shows that these Chromatographie conditions separate cyclic Boltorn polymers (with no core molecule) from non-cyclic polymers (with core molecule), and these are the only two architectures observed. MALDI MS also confirms that the Chromatographie Separation mode is adsorption, but further analysis is needed to determine if there is a Separation by degree of branching. KW - Hyperbranched polyesters KW - Polymer mass spectrometry KW - Polymer chromatography KW - Liquid adsorption chromatography KW - MALDI-TOF MS KW - Carbon capture KW - Climate change KW - Lubricant KW - Micro manufacturing KW - Multiphysics simulations KW - WMRIF PY - 2014 SN - 978-3-319-11339-5 SN - 978-3-319-11340-1 SP - 1 EP - 10 PB - Springer AN - OPUS4-32519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska A1 - Michalchuk, Adam A1 - Stolar, Jasna A1 - Falkenhagen, Jana A1 - Bhattacharya, Biswajit A1 - Gugin, Nikita A1 - Casali, Lucia T1 - Mechanochemical pathways to sustainability: from molecular insights to applications N2 - Mechanochemical Innovations for Sustainable Synthesis of Framework Materials and Industrial ScaleUp Mechanochemistry has emerged as a powerful approach for sustainable materials synthesis and processing, with significant potential to meet the UN Sustainable Development Goals. This presentation will highlight our recent advancements in understanding, monitoring, and scaling-up mechanochemical synthesis of framework materials, focusing on the balance between fundamental understanding of reaction mechanisms and its practical applications in energy storage and energy transfer materials. A central focus of our work has been the development and application of time-resolved in situ monitoring techniques for mechanochemical processes. Our research on real-time synchrotron X-ray diffraction has enabled unprecedented insights into reaction pathways and kinetics. Recently, we have successfully applied energy-dispersive X-ray diffraction for time-resolved in situ monitoring of reactive extrusion, marking a significant step towards ‘lighting up’ industrial-scale mechanochemistry. Bridging fundamental understanding with practical applications, we have explored the mechanochemical synthesis of functional materials for energy storage and transfer, making process in the mechanochemical synthesis of highly proton-conductive metal phosphonates, demonstrating the potential of mechanochemistry to manufacture advanced materials for energy applications. T2 - GDCh Universität Marburg CY - Marburg, Germany DA - 10.02.2025 KW - Situ investigation KW - Nanoparticles KW - Metal phosphonates PY - 2025 AN - OPUS4-64844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Microstructure characterization of oligomers by analysis of UPLC / ESI-TOF-MS reconstructed ion chromatograms N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available. The challenge consists in a clever combination of these techniques with a specific approach of data analysis. In this presentation different liquid chromatographic separation modes were combined with Electrospray Time-of-Flight mass spectrometry. The online coupling allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples e.g. the topology elucidation of branched EO-PO copolymers, the possibilities and limitations of this approach were demonstrated. T2 - Analyticon 2020 CY - Online meeting DA - 05.11.2020 KW - Microstructure KW - Copolymer KW - LC-MS PY - 2020 AN - OPUS4-51540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Günter A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter T1 - Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-Massenspektrometrie zur Charakterisierung von Si-haltigen Verbindungen T2 - DFG-Symposium zum Schwerpunktprogramm "Silicium-Chemie" CY - Werfenweng, Österreich DA - 2002-05-02 PY - 2002 AN - OPUS4-1797 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Structure Analysis of Oligomers by Online UHPLC/ ESI-TOF-MS T2 - ANAKON 2015 CY - Graz, Austria DA - 2015-03-23 PY - 2015 AN - OPUS4-32936 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Gerstung, Vanessa A1 - Much, Helmut A1 - Schulz, Günter A1 - Friedrich, Jörg Florian T1 - Beiträge zur Charakterisierung von synthetischen Si-Polymeren durch Kopplung von HPLC-Trennmethoden mit der MALDI-TOF-Massenspektrometrie T2 - Berliner Polymeren-Tage 2000 CY - Berlin, Deutschland DA - 2000-10-09 PY - 2000 CY - Berlin AN - OPUS4-2252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Much, Helmut A1 - Schulz, Günter A1 - Rikowski, E. T1 - Characterization of silicon polymers (silsesquioxanes, dendrimers and copolymers) by means of different modes of Liquid Chromatography and MALDI-TOF-MS PY - 1998 PB - Messe München GmbH CY - München AN - OPUS4-2236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Lösemittelfreie Probenpräparation in der Chromatographie - MALDI Kopplung T2 - 8. Kolloquium "MALDI-TOF-MS und synthetische Polymere", BAM CY - Berlin, Germany DA - 2004-05-11 PY - 2004 AN - OPUS4-4345 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Hyphenated characterization techniques for polymer analysis: from SEC-ESI-MS to 2D HPLC/SEC chromatography T2 - Controlled/Living Radical Polymerizations: Latest Trends in Synthesis, Characterization and Industrial Applications CY - Houffalize, Belgium DA - 2009-09-17 PY - 2009 AN - OPUS4-20000 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Schulz, Günter A1 - Gloede, J. T1 - Charakterisierung von Calixarenen durch Kopplung von Flüssigchromatographie und MALDI-TOF-MS KW - Flüssigchromatographie KW - Kopplung LACCC KW - MALDI-TOF-MS KW - Calixarene KW - Novolake PY - 2001 SN - 0016-3538 VL - 45 IS - 4 SP - 380 EP - 384 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-2177 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schulz, Günter A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Rikowski, E. ED - Cherdron, H. T1 - Nachweis neuer Si-Polymerstrukturen durch die Kopplung der SEC mit der MALDI-TOF-MS T2 - Symposium on Tailormade Polymers CY - Merseburg, Deutschland DA - 2000-03-20 PY - 2000 SN - 3-527-30325-1 SN - 1022-1360 N1 - Serientitel: Macromolecular symposia – Series title: Macromolecular symposia IS - 163 PB - Wiley-VCH CY - Weinheim AN - OPUS4-2244 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -