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 - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Rikowski, E. T1 - Zur Charakterisierung von Si-Polymeren durch flüssigchromatographische Verfahren in Kopplung mit der MALDI-TOF-MS N2 - Summary. The coupling of the three liquid chromatographic modes with MALDI-TOF mass spectrometry is suitable for the determination of the molecular, functional, and chemical heterogeneities of Si polymers. Silsesquioxanes and siloxanes serve as examples for this method of structure identification. The substance specific construction of the SEC calibration curve by means of MALDI-MS is shown. Zusammenfassung. Die Kopplung der drei flüssigchromatographischen Modi mit MALDI-TOF-Massenspektrometrie ist zur Bestimmung der molekularen, funktionalen und chemischen Verteilungen von Si-Polymeren geeignet. Silsesquioxane und Siloxane dienen als Beispiele für diese Art der Strukturerkennung. Die substanzspezifische Konstruktion einer SEC-Eichkurve mit Hilfe der MALDI-MS wird gezeigt. KW - Si polymer characterization KW - LC/MALDI-TOF-MS PY - 1999 DO - https://doi.org/10.1007/PL00010162 SN - 0026-9247 SN - 1434-4475 VL - 130 IS - 1 SP - 163 EP - 174 PB - Springer CY - Wien AN - OPUS4-2163 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Hauser, K. A1 - Krüger, Ralph-Peter A1 - Schulz, Günter T1 - Macrocycles 12. Ring-Opening Polycondensations of Tin-Containing Macrocycles with Bis(Thioarylester)s N2 - 2,2-Dibutyl-2-stanna-1,3-dioxepane (DSDOP) was polycondensed with bis(4-chlorothiophenyl) suberat under various reaction conditions, but only moderate molecular weights (Mn 10000) were obtained. The MALDI-TOF mass spectrosmetry revealed the formation of cyclic oligo- and polyesters in addition to linear species having OH, CO2H, and unreacted 4-chlorothiophenyl ester endgroups. Furthermore, -Caprolactone (-CL) was polymerized with DSDOP as the initiator at monomer/initiator (M/I) ratios of 20 and 50. The resulting tin-containing macrocyclic polylactones were reacted with sebacic acid bis(4-thiocresyl)ester at three different temperatures and with different reaction times. Analogous polycondensations were conducted with suberic acid bis(4-chlorothiophenyl) ester. The presence of thioarylester endgroups in the isolated polyesters was checked by 1H NMR spectroscopy. The highest conversions were found at long reaction times (24 or 72 hours), or after the addition of pyridine and N,N-dimethylaminopyridine as catalysts. Despite high conversions, the number average molecular weights (Mn's) did not exceed values around 20000. Even in the samples having the highest molecular weights, unreacted 4-chlorothiophenylester endgroups were detected by GPC measurements evaluated with a UV-detector. It is concluded that both factors, cyclization and incomplete conversion, contribute to the limitation of the chain growth. KW - Ring-Opening Polycondensations KW - Macrocycles KW - Polyesters PY - 2000 DO - https://doi.org/10.1081/MA-100101099 SN - 1060-1325 SN - 1520-5738 VL - 37 IS - 4 SP - 379 EP - 394 PB - Taylor & Francis CY - Philadelphia, PA AN - OPUS4-2167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Probst, N. A1 - Schwarz, G. A1 - Schulz, Günter A1 - Krüger, Ralph-Peter T1 - New Polymer Syntheses - 107. Aliphatic Poly(thio ester)s by Ring-Opening Polycondensation of 2-Stanna-1,3-Dithiacycloalkanes N2 - We prepared 2,2-dibutyl-2-stanna-1,3-dithiacycloalkanes from dibutyltin oxide and ,-dimercaptoalkanes. Heterocycles with five-, six-, seven-, or nine-ring members were used as bifunctional monomers for polycondensations with aliphatic dicarboxylic acid chlorides. These polycondensations conducted in bulk were highly exothermic and yielded poly(thio ester)s with number average molecular weights (Mn's) in the range of 5000-30,000 Da. These poly(thio ester)s proved to be rapidly crystallizing materials with melting temperatures in the range of 90-150 °C. In addition to the success of the new synthetic approach, two interesting and unpredictable results were obtained. All volatile species detectable by matrix assisted laser desorption induced-time of flight (MALDI-TOF) mass spectrometry were cyclic oligo- and poly(thio ester)s. Second, several polyesters showed a reversible first-order change of the crystal modification as identified by differential scanning calorimetry measurements and X-ray scattering with variation of the temperature. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 3656-3664, 2000 KW - Poly(thio-ester)s KW - Ring-opening polycondensation KW - Macrocycles KW - Change of crystal structure PY - 2000 DO - https://doi.org/10.1002/1099-0518(20001001)38:19<3656::AID-POLA190>3.0.CO;2-M SN - 0360-6376 SN - 0887-624X VL - 38 IS - 19 SP - 3656 EP - 3664 PB - Wiley CY - Hoboken, NJ AN - OPUS4-2170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reuther, F. A1 - Krüger, Ralph-Peter A1 - Schulz, Günter A1 - Baehr, G. A1 - Westerwelle, U. A1 - Gruetzner, G. ED - Houlihan, F. M. T1 - Tailored novolak resins for advanced photoresists by a two-step procedure - new insight into the molecular structure by coupling GPC and MALDI-TOF-MS T2 - 17th Annual SPIE Conference on Advances in Resist Technology and Processing CY - Santa Clara, CA, USA DA - 2000-02-28 KW - Novolak KW - Structure KW - Synthesis KW - Gel permeation KW - Chromatography KW - MALDI-TOF-MS PY - 2000 SN - 0-8194-3617-8 SN - 1605-7422 N1 - Serientitel: SPIE proceedings series – Series title: SPIE proceedings series IS - 3999 SP - 464 EP - 471 PB - SPIE CY - Bellingham AN - OPUS4-2171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Determination of functionality and molar mass distribution of aliphatic polyesters by orthogonal liquid chromatography, Part I: Off-line investigation of poly-(1,6-hexanediol adipates) PY - 1994 SN - 0148-3919 VL - 17 SP - 3069 EP - 3090 PB - Dekker CY - New York, NY AN - OPUS4-2139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - New Results of Determination of Polymer Heterogeneity by Two-Dimensional Orthogonal Liquid Chromatography T2 - International GPC Symposium CY - Lake Buena Vista, FL, USA DA - 1994-06-05 PY - 1994 SP - 273 EP - 275 PB - Gordon and Breach CY - St. Helier, Jersey AN - OPUS4-2140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachsen, O. A1 - Reichert, K.H. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Thermal decomposition of biodegradable polyesters - III. Studies on the mechanisms of thermal degradation of oligo-L-lactide using SEC, LACCC and MALDI-TOF-MS PY - 1997 SN - 0141-3910 SN - 1873-2321 VL - 55 SP - 225 EP - 231 PB - Applied Science Publ. CY - London AN - OPUS4-2154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Determination of polymer heterogeneity by two-dimensional orthogonal liquid chromatography KW - Orthogonal chromatography KW - Size exclusion chromatography KW - Liquid adsorption chromatography at critical conditions KW - Matrix-assisted laser desorption ionization time-of-flight mass spectrometry KW - Polyester KW - Polyether PY - 1996 SN - 1023-666X SN - 1563-5341 VL - 2 SP - 221 EP - 235 PB - Gordon and Breach Publ. CY - Amsterdam AN - OPUS4-2146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leukel, J. A1 - Burchard, W. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Mechanism of the anionic copolymerization of anhydride- cured epoxies-analysisted by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) PY - 1996 SN - 1022-1336 SN - 1521-3927 VL - 17 SP - 359 EP - 366 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Bestimmung der Polymerheterogenität durch Kopplung von HPLC und MALDI-TOF-MS KW - Zweidimensionale Flüssigchromatographie KW - Flugzeit-Massenspektrometrie KW - Synthetische Polymere PY - 1996 SN - 0016-3538 VL - 40 IS - 4 SP - 398 EP - 402 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-2149 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Wachsen, O. T1 - New aspects of determination of polymer heterogeneity by 2-dimensional orthogonal liquid chromatography and MALDI-TOF-MS PY - 1996 SN - 1022-1360 SN - 0258-0322 SN - 1521-3900 VL - 110 SP - 155 EP - 176 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2150 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 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter ED - Günther, W. T1 - Strukturaufklärung von heterogenen Polymeren durch zweidimensionale Flüssigchromatographie und MALDI-TOF-Massenspektrometrie T2 - InCom '94 - International Symposium on Instrumentalized Analytical Chemistry and Computer Technology CY - Düsseldorf, Deutschland DA - 1994-03-14 PY - 1994 VL - 94 PB - InCom-Bureau CY - Düsseldorf AN - OPUS4-2195 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Polymer Characterization by Two-Dimensional HPLC and MALDI-TOF-MS T2 - 7th International Symposium on Polymer Analysis and Characterization (ISPAC) CY - Les Diablerets, Switzerland DA - 1994-05-24 PY - 1994 PB - Gordon and Breach CY - St. Helier, Jersey AN - OPUS4-2196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Paulus, G. A1 - Resch, M. A1 - Schulz, Günter ED - Darms, R. ED - Suter, U. T1 - Polymer Characterization by MALDI-TOF-MS and Combination with HPLC T2 - 5th European Polymer Federation Symposium on Polymeric Materials (EPF) CY - Basel, Switzerland DA - 1994-10-09 PY - 1994 SN - 3-85739-297-5 SN - 0258-0322 VL - 5 PB - Hüthig & Wepf CY - Zug AN - OPUS4-2200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, Günter A1 - Krüger, Ralph-Peter A1 - Much, Helmut ED - Günther, W. T1 - Polymercharakterisierung durch MALDI-TOF-MS und Kopplung mit der HPLC T2 - InCom '95 - International Symposium on Instrumentalized Analytical Chemistry and Computer Technology CY - Düsseldorf, Germany DA - 1995-03-20 PY - 1995 CY - Moers AN - OPUS4-2201 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachsen, O. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Reichert, K.H. T1 - Untersuchungen zur Charakterisierung des Abbaus von Polylactiden mittels 2D-HPLC und MALDI-TOF-MS T2 - Sitznung des Berliner Verband für Polymerforschung e.V. CY - Berlin DA - 1995-05-18 PY - 1995 CY - Berlin AN - OPUS4-2202 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kilz, P. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter ED - Provder, T. T1 - Two-dimensional chromatography for the deformulation of complex copolymers PY - 1995 SN - 0-8412-3132-X N1 - Serientitel: Advances in chemistry series – Series title: Advances in chemistry series IS - 247 SP - 223 EP - 241 PB - American Chemical Society CY - Washington AN - OPUS4-2185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Rikowski, E. ED - Auner, N. T1 - Synthesis of Polyhedral Hexa-, Octa-, Deca- and Dodeca-Silsesquioxanes, Separation by NP-HPLC, SEC and LAC, Characterization by MALDI-TOF-MS KW - Silsesquioxanes KW - NP-HPLC KW - LAC KW - SEC KW - MALDI-TOF-MS PY - 2000 SN - 3-527-29854-1 SP - 545 ff. PB - Wiley-VCH CY - Weinheim AN - OPUS4-2187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -