TY - JOUR A1 - Kricheldorf, H.R. A1 - Vakhtangishvili, L. A1 - Schwarz, G. A1 - Krüger, Ralph-Peter T1 - Cyclic Hyperbranched Poly(ether ketone)s Derived from 3,5-Bis(4-fluorobenzoyl)phenol N2 - 3,5-Bis(4-fluorobenzoyl)phenol was polycondensed under various reaction conditions. Low molecular weights were obtained (Mn < 8000 Da), and MALDI-TOF mass spectrometry indicated that the chain growth was limited by cyclization. In the best mass spectra the cyclic, hyperbranched poly(ether ketone)s were detectable up to masses around 14 000 Da. When 4,4'-difluordiphenyl sulfone was added, star-shaped polymers having a diphenyl sulfone star center were formed, but cyclization was not completely suppressed. The results were compared to those obtained from "linear polycondensations" based on 4,4'-difluorobenzophenone (DFBP) and 4-tert-butylcatechol or bisphenol A. The poly(ether ketone)s of DFBP had also low molecular weights and contained high fractions of cycles. It is concluded that also in the case of hyperbranched polymers cyclization competes with propagation at any stage of the polycondensation at any concentration. Therefore, the fundamental trend of any "abn" polycondensation is the formation of star-shaped polymers having a cyclic core and hyperbranched star arms. PY - 2003 DO - https://doi.org/10.1021/ma021799x SN - 0024-9297 SN - 1520-5835 VL - 36 SP - 5551 EP - 5558 PB - American Chemical Society CY - Washington, DC AN - OPUS4-2622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krüger, Ralph-Peter T1 - H. Pasch and W. Schrepp "MALDI-TOF Mass Spectrometry of Synthetic Polymers" (Book review) PY - 2004 DO - https://doi.org/10.1002/macp.200400155 SN - 1022-1352 SN - 1521-3935 VL - 205 SP - 1284 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-3567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Rikowski, E. T1 - Characterization of Silicon-Polymers by Liquid Chromatography and MALDI-TOF-MS T2 - GDCh-Hauptversammlung in Verbindung mit dem 37. IUPAC Congress CY - Berlin, Germany DA - 1999-08-14 PY - 1999 AN - OPUS4-3547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Viala, S. A1 - Tauer, K. A1 - Antonietti, M. A1 - Krüger, Ralph-Peter A1 - Bremser, W. T1 - Structural control in radical polymerization with 1,1-diphenylethylene. 1. Copolymerization of 1,1-diphenylethylene with methyl methacrylate N2 - The role of 1,1-diphenylethylene (DPE) in radical emulsion polymerization of methyl methacrylate is investigated. The presence of DPE causes a strong decrease in both the rate of polymerization and the molecular weight. According to the results of structure analysis by means of MALDI-TOF mass spectrometry, UV–vis spectroscopy, and 1H–NMR spectroscopy, DPE is incorporated in the copolymer chain exclusively as a reactive recombinant ?,p-dimer, underlining the peculiar role of DPE in radical polymerizations. KW - Emulsion polymerization KW - 1,1-Diphenylethylene KW - Copolymer structure PY - 2002 DO - https://doi.org/10.1016/S0032-3861(02)00676-6 SN - 0032-3861 SN - 1873-2291 VL - 43 IS - 26 SP - 7231 EP - 7241 PB - Springer CY - Berlin AN - OPUS4-1919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klapdohr, S. A1 - Moszner, N. A1 - Kickelbick, G. A1 - Krüger, Ralph-Peter T1 - Investigation of the Structure of Polymerizable Silsesquioxanes by GPC and MALDI-TOF-MS in Relation to their Viscosity N2 - Hydrolytic condensation of different methacrylate groups containing alkoxy silanes yielded resins which showed interesting properties as a matrix for dental composites. For this purpose, resins of low viscosity are desired resulting in composites with a high amount of inorganic fillers. Our investigations demonstrated that the viscosity of the obtained polycondensates was predominantly influenced by the kind of organic spacer between the methacrylate group and the silicon atom. In addition, the viscosity also significantly changed in dependence of the kind of structure units built. NMR spectroscopic investigations as well as size exclusion chromatography (SEC) and matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry showed that the formed structures depended both on the kind of catalyst used for hydrolysis/condensation and the bulkiness of the organic substituent at the silicon atom. KW - Nanostructure KW - Sols KW - Polycondensation KW - Silicon compounds KW - Dental PY - 2006 DO - https://doi.org/10.1007/s00706-006-0442-z SN - 0026-9247 SN - 1434-4475 VL - 137 SP - 667 EP - 679 PB - Springer CY - Wien AN - OPUS4-12139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trathnigg, B. A1 - Maier, B. A1 - Schulz, G. A1 - Krüger, Ralph-Peter A1 - Just, Ulrich T1 - Characterization of Polyethers using different methods: SFC, LAC and SEC with different detectors, and MALDI-TOF-MS PY - 1996 SN - 1022-1360 SN - 0258-0322 SN - 1521-3900 VL - 110 SP - 231 EP - 240 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-11332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Chatti, S. A1 - Schwarz, G. A1 - Krüger, Ralph-Peter T1 - Macrocycles 27 - Cyclic Aliphatic Polyesters of Isosorbide N2 - Numerous polycondensations of isosorbide and suberoyl chloride or other aliphatic dicarboxylic acid dichlorides were performed with pyridine as a catalyst and HCl acceptor. The reaction conditions were varied to optimize both the molecular weight and the fraction of cyclic oligo- and polyesters. Furthermore, we attempted to obtain the cyclic monomer by catalyzed back-biting degradation of the molten cyclic polyesters above 220 °C in vacuo. The polyesters were characterized by viscosity and size exclusion chromatographic measurements as well as matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. In selected cases, mixtures of linear and cyclic polyesters were treated with a hot solution of partially methylated ß-cyclodextrin in methanol. This treatment allowed for a selective extraction of the linear chains up to approximately 5000 Da. KW - Polycondensation KW - Cyclization KW - Isosorbide KW - Polyesters KW - MALDI PY - 2003 DO - https://doi.org/10.1002/pola.10933 SN - 0360-6376 SN - 0887-624X VL - 41 IS - 21 SP - 3414 EP - 3424 PB - Wiley CY - Hoboken, NJ AN - OPUS4-12017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Klapdohr, S A1 - Moszner, N. A1 - Kickelbick, G. T1 - Structure and Related Properties of Polymerizable Silsesquioxanes as a Matrix for Dental Composites T2 - 13th International Workshop on Sol-Gel Science and Technology CY - Los Angeles, CA, USA DA - 2005-08-21 PY - 2005 AN - OPUS4-10748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Just, Ulrich T1 - Principle of Two-Dimensional Characterization of Copolymers N2 - Two-dimensional polymer characterization is used for a simultaneous analysis of molar masses and chemical heterogeneities (e.g., end groups, copolymer composition, etc.). This principle is based on coupling of two different chromatographic modes. Liquid adsorption chromatography at critical conditions (LACCC) is applied for a separation according to the chemical heterogeneity, whereas in the second-dimension fractions are analyzed with regard to their molar mass distribution by means of size exclusion chromatography (SEC). Because appropriate standards for a calibration of the SEC are seldom available, matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF MS) was used to substitute the SEC. The LACCC-MALDI MS coupling enables acquiring additional structural information on copolymer composition, which can considerably enhance the performance of this coupled method. KW - MALDI-TOF MS KW - Chromatographie KW - Kopplung PY - 2007 DO - https://doi.org/10.1021/ac062145f SN - 0003-2700 SN - 1520-6882 VL - 79 IS - 13 SP - 4814 EP - 4819 PB - American Chemical Society CY - Washington, DC AN - OPUS4-17722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Schulz, Günter T1 - Characterization of polylactides by coupling of chromatographic methods with MALDI-TOF-MS T2 - Polydays 2002 ; ISPAC 2002 CY - Berlin, Germany DA - 2002-09-30 PY - 2002 AN - OPUS4-1807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Schulz, Günter A1 - Weidner, Steffen T1 - Polymer Characterization by LC / MALDI-MS Coupling T2 - Vortragstagung "Funktionspolymere für Systemlösungen" CY - Darmstadt, Germany DA - 2002-03-18 PY - 2002 AN - OPUS4-1805 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 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Investigations of Polymer Heterogeneity by Two-Dimensional HPLC, MALDI-TOF-MS and FTIR Coupling T2 - ISPAC 8, HPLC ´95 CY - Sanibel Island, FL, USA DA - 1995-05-20 PY - 1995 PB - Gordon and Breach CY - Sant Helier AN - OPUS4-2203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Schulz, Günter ED - Jutzi, P. ED - Schubert, U. T1 - Characterization of Si-polymers by coupling of HPLC-separation methods with MALDI-TOF-MS T2 - Symposium on Silicon Chemistry CY - Werfenweng, Österreich DA - 2002-01-01 PY - 2003 SN - 3-527-30647-1 SP - 406 EP - 418 PB - Wiley-VCH CY - Weinheim AN - OPUS4-2194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Coupling of different modes of liquid chromatography of polymers with spectroscopic methods and MALDI-TOF-MS-key for determination of polymer heterogeneity T2 - 6th SPSJ International Polymer Conference (IPC 97) CY - Kusatsu, Japan DA - 1997-10-20 PY - 1997 VL - 6 AN - OPUS4-2233 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 T1 - Characterization of silicon polymers by means of different liquid chromatographic modes and MALDI-TOF-MS T2 - DFG-Symposium zum Schwerpunktprogramm "Silicium-Chemie" CY - Werfenweng, Austria DA - 1998-06-11 PY - 1998 AN - OPUS4-2237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Schulz, Günter A1 - Weidner, Steffen T1 - Polymer characterization by LC / MALDI-MS coupling T2 - Bayreuther Polymer Symposium 2001 CY - Bayreuth, Germany DA - 2001-09-16 PY - 2001 CY - Bayreuth AN - OPUS4-2256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenhagen, Jana A1 - Jancke, Harald A1 - Krüger, Ralph-Peter A1 - Rikowski, Eckhard A1 - Schulz, Günter T1 - Characterization of Silsesquioxanes by Size-exclusion chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry N2 - Liquid chromatography in combination with spectroscopic methods like matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) or nuclear magnetic resonance (NMR) spectroscopy is a powerful method to characterize silsesquioxanes and silsesquioxane mixtures. As new examples, the formation of silsesquioxyl-substituted silsesquioxanes [(n-octyl)7(SiO1.5)8]2O and [(n-octyl)7(SiO1.5)8O]2[(n-octyl)6(SiO1.5)8] as well as the cage rearrangement of octa-[(n-heptyl)silsesquioxane] to larger structur es [(n-heptyl)SiO1.5)]n up to n=28 are shown. PY - 2003 DO - https://doi.org/10.1002/rcm.911 SN - 0951-4198 SN - 1097-0231 VL - 17 IS - 4 SP - 285 EP - 290 PB - Wiley CY - Chichester AN - OPUS4-2182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter ED - Fell, A. T1 - Two-dimensional chromatography, their optimization and coupling with different detection techniques for investigation of polymer heterogeneity T2 - 21st International Symposium on High Performance Liquid Phase Separations and Related Techniques (HPLC) CY - Birmingham, England, UK DA - 1997-06-22 PY - 1997 SN - 0021-9673 PB - Elsevier CY - Amsterdam AN - OPUS4-2232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenhagen, Jana A1 - Friedrich, Jörg Florian A1 - Schulz, Günter A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Weidner, Steffen T1 - Liquid Adsorption Chromatography near Critical Conditions of Adsorption coupled with Matrix-assisted Laser Desorption/Ionization Mass Spectrometry N2 - Chemical heterogeneities and molecular weight distributions of poly(ethylene oxide) (PEO)-co-polymethylene (PM) model oligomers, which are relevant to the synthesis of commonly used tensides, were investigated. For analytical characterization, the well-known principle of liquid adsorption chromatography at 'critical conditions' (LACCC) was modified. Near the critical conditions of adsorption of the PEO unit, e.g., at slight adsorption conditions of PM, the copolymers could be separated according to their PM chain length. The eluates were separated and single fractions of each peak were continuously transferred onto the MALDI target by means of a commercially available device. Simultaneously, the MALDI matrix solution was continuously added with a second pump. This procedure offers the possibility of the formation of homogeneous matrix-polymer textures. By MALDI-MS a complete characterization of the chemical composition (PEO and PM chain length) of each peak could be achieved. The obtained MALDI mass spectra of the eluates at different retention times could be used for the molecular weight calibration of the LAC system. In this way, an additional application of SEC, as in conventional 2D-chromatography, was avoided by using the MALDI method as quasi chromatographic separation KW - Liquid adsorption chromatography KW - Matrix-assisted laser desorption KW - Ionization mass spectrometry KW - Coupling methods KW - MALDI PY - 2000 DO - https://doi.org/10.1080/10236660008034644 SN - 1023-666X SN - 1563-5341 VL - 5 SP - 549 EP - 562 PB - Gordon and Breach Publ. CY - Amsterdam AN - OPUS4-2168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -