TY - CONF A1 - Falkenhagen, Jana T1 - Investigation of heterogeneity of polyethers by coupling of liquid chromatographic methods with MALDI-TOF-MS T2 - Berliner Polymerentage 2000 CY - Berlin, Germany DA - 2000-10-09 PY - 2000 AN - OPUS4-3766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Investigation of heterogeneity of polyethers by coupling of liquid chromatographic methods with MALDI-TOF-MS T2 - ISPAC 2000 CY - Pittsburgh, PA, USA DA - 2000-06-19 PY - 2000 AN - OPUS4-3765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of polylactides by coupling of chromatographic methods with MALDI-TOF-MS T2 - Polydays 2002, TU Berlin CY - Berlin, Germany DA - 2002-09-30 PY - 2002 AN - OPUS4-3455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Charakterisierung von Polymeren durch Kopplung von flüssigchromatographischen und spektroskopischen Methoden T2 - HPLC-Tage CY - Mannheim, Germany DA - 2002-11-12 PY - 2002 AN - OPUS4-3549 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupled Separation and Detection Techniques: New Aspects and Problems T2 - 17th International Symposium on Polymer Analysis and Characterization (ISPAC 2004) CY - Heidelberg, Germany DA - 2004-06-07 PY - 2004 AN - OPUS4-5530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupled Separation and Detection Techniques: New Aspects and Problems T2 - 17th International Symposium on Polymer Analysis and Characterization (ISPAC 2004) CY - Heidelberg, Germany DA - 2004-06-06 PY - 2004 AN - OPUS4-4343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Application of Solvent-free Sample Preparation for LC/MALDI-MS Coupling T2 - 52nd ASMS Conference CY - Nashville, TN, USA DA - 2004-05-23 PY - 2004 AN - OPUS4-4344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of polyesters and copolyesters by coupled chromatographic and spectroscopic techniques T2 - 2nd International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules SCM-2 CY - Amsterdam, Netherlands DA - 2005-02-02 PY - 2005 AN - OPUS4-5535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of silicon polymers by coupling of liquid chromatographic methods with MALDI-TOF-MS T2 - ISPAC 2000 CY - Pittsburgh, PA, USA DA - 2000-06-18 PY - 2000 AN - OPUS4-11130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Neue Wege zur analytischen Charakterisierung komplexer Polymersysteme T2 - BAM-Kuratoriumssitzung CY - Berlin, Germany DA - 2000-05-16 PY - 2000 AN - OPUS4-11135 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Charakterisierung strukturheterogener Polymersysteme T2 - BAM-Kolloquium CY - Berlin, Germany DA - 2000-09-07 PY - 2000 AN - OPUS4-11133 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterisierung von Polyvinylpyrollidonen T2 - Fachgruppenvollversammlung VI.3, BAM CY - Berlin, Germany DA - 2004-12-14 PY - 2004 AN - OPUS4-5537 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of Polyacetals by comprehensive 2D liquid chromatography an hyphenated techniques T2 - Separation and Characterization of Natural and Synthectic Macromolecules (SCM-2) CY - Amsterdam, Netherlands DA - 2005-02-02 PY - 2005 AN - OPUS4-11552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of Polymer Heterogeneity by Hyphenated Techniques (Coupling of HPLC and MALDI-TOF-MS) T2 - Polymer Laboratories CY - Church Stretton, England DA - 1996-06-28 PY - 1996 AN - OPUS4-11185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Kang, Nianjun A1 - Wang, De-Yi A1 - Falkenhagen, Jana A1 - Thünemann, Andreas A1 - Schönhals, Andreas T1 - Structure–Property Relationships of Nanocomposites Based on Polylactide and Layered Double Hydroxides – Comparison of MgAl and NiAl LDH as Nanofiller N2 - Nanocomposites based on poly(L-lactide) (PLA) and organically modified Ni/Al layered double hydroxides (NiAl/LDHs) are prepared by melt blending and investigated by a combination of size exclusion chromatography, differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), wide-angle X-ray scattering, and broadband dielectric spectroscopy. A detailed comparison to the behavior of the corresponding MgAl/LDH–PLA nanocomposites is made. SAXS investigations show that the morphology of the NiAl/LDH–PLA nanocomposites is more intercalated compared to the MgAl/LDH based PLA nanocomposite, which is more exfoliated. The DSC investigation gives a different dependence of the degree of crystallization on the concentration of LDH for NiAl/LDH–PLA than for MgAl/LDH–PLA nanocomposite system. These differences are discussed taking the differences of the morphologies of both systems into account. Broadband dielectric spectroscopy reveals information about the molecular dynamics where essential differences are observed for all relaxation processes taking place in both systems which were related to the different morphologies. KW - Nanocomposites KW - Polylactide PY - 2017 DO - https://doi.org/10.1002/macp.201700232 SN - 1022-1352 SN - 1521-3935 VL - 218 IS - 20 SP - Article 1700232, 1 EP - 12 PB - Wiley-VCH Verlag AN - OPUS4-42597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Rikowski, Eckhard A1 - Schulz, Günter A1 - Friedrich, Jörg Florian ED - Grellmann, W. T1 - Synthesis and Characterisation of Polyhedral Silsesquioxanes with Nanotubular Structures T2 - 23. DVM-Vortrags- und Diskussionstagung "Werkstoffprüfung 2005", DA - 2005-12-01 PY - 2005 SP - 25 EP - 30 PB - DVM AN - OPUS4-11947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Charakterisierung strukturheterogener synthetischer Polymere mittels LC / MALDI- und LC / ESI-TOF-MS Kopplung T2 - MC-Kolloquium der Heinrich-Heine-Universität CY - Düsseldorf, Germany DA - 2007-05-03 PY - 2007 AN - OPUS4-14667 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Polymer characterization by hyphenated chromatographic techniques coupled with MALDI and ESI mass spectrometry T2 - Australasian Polymer Symposium (29th APS) CY - Hobart, Australia DA - 2007-02-11 PY - 2007 AN - OPUS4-13820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Hyphenated liquid-chromatographic, spectroscopic and spectrometric techniques for polymer characterization T2 - Fraunhofer & PTS-Seminar CY - Potsdam, Germany DA - 2006-03-22 PY - 2006 AN - OPUS4-12378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - LC / MALDI- und LC / ESI-TOF-MS Kopplung zur Charakterisierung von Polyethern und Polyestern T2 - 11. MALDI-TOF-MS Kolloquium, BAM CY - Berlin, Germany DA - 2007-05-15 PY - 2007 AN - OPUS4-14705 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Charakterisierung von Polyvinylpyrrolidon Homo- und Copolymeren T2 - 9. Kolloquium "MALDI-TOF-MS und synthetische Polymere", BAM CY - Berlin, Germany DA - 2005-05-10 PY - 2005 AN - OPUS4-11557 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 T1 - Characterization of silicon polymers (silsesquioxanes, dendrimers and copolymers) by means of different modes of Liquid Chromatography and MALDI-TOF-MS T2 - 11th International Symposium on Polymer Analysis and Characterization CY - Santa Margherita Ligure, Italien DA - 1998-05-25 PY - 1999 N1 - Serientitel: International journal of polymer analysis and characterization – Series title: International journal of polymer analysis and characterization IS - 5.1999,3 PB - Gordon and Breach CY - St. Helier AN - OPUS4-19053 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Online UP-LACCC / ESI-TOF-MS for characterization of synthetic polymers as complementary tool to LC / MALDI-TOF-MS coupling T2 - 32nd International Symposium on HPLC and Related Techniques CY - Baltimore, MD, USA DA - 2008-05-10 PY - 2008 AN - OPUS4-17897 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - LC - MALDI/ESI-TOF-MS for Charactarization of Complex Polymer Systems T2 - 4th International Symposium on Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 2009-01-27 PY - 2009 AN - OPUS4-19188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Structure and end group analysis of complex polymers by LC/MALDI/ESI-TOF CID MS/MS T2 - 11th Bayreuther Polymer Symposium CY - Bayreuth, Germany DA - 2009-09-13 PY - 2009 AN - OPUS4-19988 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Synthesis and characterization of Polylactides by coupling of liquid chromatographic methods with MALDI-TOF-MS T2 - Kick-Off-Meeting; Bioabbaubare Verpackungen aus Polylactid CY - Darmstadt, Germany DA - 2008-05-08 PY - 2008 AN - OPUS4-17895 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Rapid determination of critical conditions of adsorption of synthetic coplymers by UPLC/ESI-MS T2 - Analytica Conference 2008 CY - Munich, Germany DA - 2008-04-01 PY - 2008 AN - OPUS4-17850 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, M. A1 - Glassner, M. A1 - Gruendling, T. A1 - Schmid, Christina A1 - Falkenhagen, Jana A1 - Barner-Kowollik, C. T1 - Facile conversion of RAFT polymers into hydroxyl functional polymers: a detailed investigation of variable monomer and RAFT agent combinations N2 - We report the systematic investigation of a recently introduced one-pot radical transformation of methacrylate and acrylate-type polymers prepared via reversible addition fragmentation chain transfer (RAFT) polymerization into hydroxyl functional polymers. The simple reaction procedure involves stirring a solution of the RAFT functional polymer and an azo-initiator in tetrahydrofuran at elevated temperatures (T = 60 °C) in the presence of ambient air. Subsequent reduction of the formed hydroperoxide functional polymers to hydroxyl functional polymers is achieved in a one-pot procedure using triphenylphosphine. Polymers investigated in the current study are poly(methyl acrylate) (pMA), poly(butyl acrylate) (pBA), poly(isobornyl acrylate) (piBoA) and poly(tert-butyl acrylate) (ptBA) carrying a dithiobenzoate or phenyldithioacetate end terminius as well as a symmetrical trithiocarbonate mid chain function. Quantitative conversion into the hydroperoxyl and hydroxyl terminated product is observed when trithiocarbonate functional polymers are employed. In the case of dithiobenzoate and phenyldithioacetate functional acrylic polymers, some minor side products due to the oxidation of the RAFT end-group are generated. Size exclusion chromatography (SEC) and size exclusion chromatography–electrospray mass spectrometry (SEC-ESI-MS) were employed to monitor the progress of the reaction and to investigate the proposed reaction mechanism for the model polymers. When trithiocarbonate functional polymers are employed in the transformation reaction, the SEC analysis shows a bisection of the initial Mn. Collision induced dissociation (CID) MS experiments of the intermediate reaction products were conducted to gain in-depth information about the chemical structure. The new backbone linked hydroxyl group provides a versatile anchor for chemical end-group conversions and conjugation reactions with RAFT prepared polymers, alleviating problems with the rather limited ability of the dithioester end-group to undergo non-radical transformations. KW - Polymers KW - RAFT KW - SEC/ESI-mass spectrometry KW - CID-MS PY - 2010 DO - https://doi.org/10.1039/b9py00273a SN - 1759-9954 SN - 1759-9962 VL - 1 IS - 5 SP - 634 EP - 644 AN - OPUS4-21907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Hyphenated Characterization TEchniques for Polymers: From LC/MALDI- and UPLC/ESI-TOF-MS to CID tandem mass spectrometry T2 - 11th Int. Symp. on Hyphenated Techniques in Chromatography CY - Amsterdam, Netherlands DA - 2010-01-27 PY - 2010 AN - OPUS4-21965 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Hyphenated techniques for copolymer characterization with the focus on 2D-LC / mass spectrometry T2 - 5th Int.Symp. on the Separation and Characterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 2011-01-25 PY - 2011 AN - OPUS4-22657 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Copolymer characterization by coupled LC - MS/MS techniques T2 - 2010 International Chemical Congress of Pcific Basin Societies CY - Honolulu, HI, USA DA - 2010-12-15 PY - 2010 AN - OPUS4-22831 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, C. A1 - Falkenhagen, Jana A1 - Beskers, T.F. A1 - Nguyen, L.-T.T. A1 - Wilhelm, M. A1 - Du Prez, F.E. A1 - Barner-Kowollik, C. T1 - Multi-block polyurethanes via RAFT end-group switching and their characterization by advanced hyphenated techniques N2 - The detailed characterization of poly(styrene)-b-poly(tetrahydrofuran) (pS-b-pTHF) multiblock copolymers (17800 g mol-1 ≤ Mn ≤ 46800 g mol-1) generated via urethane linkages is presented. The synthesis of the block copolymers is enabled via a mechanistic switch of the thiocarbonyl thio end group of a poly(styrene) to dihydroxyl terminated polymers that subsequently react with a diisocyanate terminated polytetrahydrofuran based prepolymer to form multiblock copolymer structures. The characterization of the multiblock copolymers and their substructures includes size exclusion chromatography (SEC), liquid chromatography at critical conditions (LCCC), nuclear magnetic resonance (NMR), and infrared (IR) spectroscopy as well as matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. To obtain even further details of the polymer size and its composition, SEC with triple detection as well as newly developed SEC coupled online to IR spectroscopy was carried out. The quantification of the average block fractions via online SEC-IR (41–61 mol % pTHF) is in very good agreement with the results obtained via NMR spectroscopy (39–66 mol % pTHF). PY - 2012 DO - https://doi.org/10.1021/ma301117k SN - 0024-9297 SN - 1520-5835 VL - 45 IS - 16 SP - 6353 EP - 6362 PB - American Chemical Society CY - Washington, DC AN - OPUS4-26942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bahlmann, Arnold A1 - Falkenhagen, Jana A1 - Weller, Michael G. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Cetirizine as pH-dependent cross-reactant in a carbamazepine-specific immunoassay N2 - High performance liquid chromatography (HPLC) was hyphenated with a previously reported carbamazepine-specific enzyme-linked immunosorbent assay (ELISA) as a screening approach to water analysis in order to identify possible interferences from transformation products. Treated wastewater was analysed and three substances were recognized by the antibody besides carbamazepine: the metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 2-hydroxycarbamazepine plus the structurally not obviously related antihistamine cetirizine. The molar cross-reactivity against cetirizine was found to be pH-dependent and assessed to be 400% at pH 4.5 and 22% at pH 10.5. Performing the ELISA at pH 10.5 greatly improved the accuracy when carbamazepine was determined in surface and wastewater samples. KW - Immunoassay KW - ELISA KW - Cetirizin KW - Carbamazepin KW - pH-Abhängigkeit KW - Kreuzreaktivität PY - 2011 DO - https://doi.org/10.1039/c0an00928h SN - 0003-2654 SN - 1364-5528 VL - 136 IS - 7 SP - 1357 EP - 1364 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-23546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Anwendung der LC-MS in der Polymeranalytik T2 - Analytica 2012 CY - Munich, Germany DA - 2012-04-17 PY - 2012 AN - OPUS4-25762 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niehoff, A. A1 - Mantion, Alexandre A1 - McAloney, R. A1 - Huber, Alexandra A1 - Falkenhagen, Jana A1 - Goh, C.M. A1 - Thünemann, Andreas A1 - Winnik, M. A. A1 - Menzel, H. T1 - Elucidation of the structure of poly(gamma-benzyl-L-glutamate) nanofibers and gel networks in a helicogenic solvent N2 - The synthesis, characterization, self-assembly, and gel formation of poly(γ-benzyl-L-glutamate) (PBLG) in a molecular weight range from ca. 7,000–100,000 g/mol and with narrow molecular weight distribution are described. The PBLG is synthesized by the nickel-mediated ring-opening polymerization and is characterized by size-exclusion chromatography coupled with multiple-angle laser light scattering, NMR, and Fourier transform infrared spectroscopy. The self-assembly and thermoreversible gel formation in the helicogenic solvent toluene is investigated by transmission electron microscopy, atomic force microscopy, small-angle X-ray scattering, and synchrotron powder X-ray diffraction. At concentrations significantly below the minimum gelation concentration, spherical aggregates are observed. At higher concentrations, gels are formed, which show a 3D network structure composed of nanofibers. The proposed self-assembly mechanism is based on a distorted hexagonal packing of PBLG helices parallel to the axis of the nanofiber. The gel network forms due to branching and rejoining of bundles of PBLG nanofibers. The network exhibits uniform domains with a length of 200±42 nm composed of densely packed PBLG helices. KW - Poly(gamma-benzyl-L-glutamate) (PBLG) KW - Nickel-mediated NCA polymerization KW - Thermoreversible gel formation KW - Physical/supramolecular organogel KW - Nanofiber KW - Self-assembly KW - Alpha-helix KW - Nanotechnology KW - Small-angle X-ray scatering KW - SAXS PY - 2013 DO - https://doi.org/10.1007/s00396-012-2866-9 SN - 0303-402X SN - 1435-1536 VL - 291 IS - 6 SP - 1353 EP - 1363 PB - Springer CY - Berlin AN - OPUS4-28615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - SURVEY OF COUPLING TECHNIQUES FOR POLYMER CHARACTERIZATION WITH FOCUS ON LC-MS T2 - SCM-6, Separation and Characterization of Macromolecules CY - Dresden, Germany DA - 2013-02-04 PY - 2013 AN - OPUS4-27658 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Shedding Light into Polymer Microstructure 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. 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 coordinated with the heterogeneity to be investigated. A number of applications will be presented from e.g. topology elucidation of branched EO-PO “academic” copolymers to copolymer composition of partially broadly distributed progressively tailored “industrial relevant” copolymers consisting of e.g. polyamides, polycarbonates and polysiloxanes. Multidimensional separation techniques will be demonstrated with focus on mass spectrometric detection techniques (ESI-/MALDI-TOF-MS) coupled online or semi-online to prior separation. T2 - FAST 2019, COAST Community of Innovation CY - Veldhoven, The Netherlands DA - 21.05.2019 KW - LCCC KW - Mass spectrometry of polymers KW - SEC KW - LC x MALDI/ESI-TOF-MS coupling PY - 2019 AN - OPUS4-48222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation 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. This is and will remain a challenge for analysts. First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized. Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures. Subsequently, different examples will be shown how these limitations in some cases could be outsmarted. First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied. Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS. All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra. T2 - SCM-9 CY - Amsterdam, The Netherlands DA - 29.01.2019 KW - Reconstructed ion chromatograms KW - Copolymer KW - Microstructure KW - LC x ESI-TOF-MS PY - 2019 AN - OPUS4-47836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krüger, Ralph-Peter A1 - Falkenhagen, Jana A1 - Schulz, Günter A1 - Heinemann, M. A1 - Weinmann, S. A1 - Friedrich, Jörg Florian A1 - Fritz, H.-G. ED - Fritz, H.-G. ED - Eisenbach, C. D. T1 - Synthese von Polylactiden mittels reaktiver Extrusion und Produktcharakterisierung durch Kopplung von HPLC-Methoden mit der MALDI-TOF-MS T2 - 18. Stuttgarter Kunststoff-Kolloquium CY - Stuttgart, Deutschland DA - 2003-03-19 PY - 2003 SN - 3-00-010663-4 IS - CD-ROM PB - Univ., IKT, IAMC CY - Stuttgart AN - OPUS4-2190 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Panne, Ulrich A1 - Falkenhagen, Jana T1 - Critical conditions for liquid chromatography of statistical copolymers: Functionality type and composition distribution characterization by UP-LCCC/ESI-MS N2 - Statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses additionally containing two kinds of end groups (FTD) were investigated by ultra high pressure liquid chromatography under critical conditions (UP-LCCC) combined with electrospray ionization time-of flight mass spectrometry (ESI-TOFMS). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution1 could be studied and confirmed. A fundamentally new approach to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with mass spectrometric detection, is described. The shift of the critical eluent composition with the monomer composition of the polymers was determined. Due to the broad molar mass distribution (MMD) and the presumed existence of different end group functionalities as well as monomer sequence distribution (MSD), Gradient separation only by CCD was not possible. Therefore, isocratic separation conditions at the CPA of definite CCD fractions were developed. Although the various present distributions partly superimposed the separation process, the goal of separation by end group functionality was still achieved on the basis of the additional dimension of ESI-TOF-MS. The existence of HO-H besides the desired allylO-H end group functionalities was confirmed and their amount estimated. Furthermore, indications for a MSD were found by UPLC/MS/MS measurements. This approach offers for the first time the possibility to obtain a fingerprint of a broad distributed statistical copolymer including MMD, FTD, CCD, and MSD. KW - Polymer KW - Liquid chromatography at critical conditions KW - ESI-TOF-MS PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04064 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 3 SP - 1778 EP - 1786 AN - OPUS4-39240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -