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 - TY - CONF A1 - Much, Helmut A1 - Krüger, Ralph-Peter A1 - Schulz, Günter T1 - Investigation of Macromer Heterogeneity by Two-Dimensional HPLC and MALDI-TOF-MS T2 - 19th International Symposium on Column Liquid Chromatography CY - Innsbruck, Austria DA - 1995-05-28 PY - 1995 CY - Innsbruck AN - OPUS4-2204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Reichert, K.H. A1 - Schulz, Günter A1 - Wachsen, O. T1 - Untersuchungen zur Charakterisierung des Polylactidabbaus mittels HPLC und MALDI-TOF-MS T2 - Präsentationsveranstaltung des Instituts für Angewandte Chemie Berlin-Adlershof e.V. CY - Berlin, Germany DA - 1995-09-26 PY - 1995 CY - Berlin AN - OPUS4-2206 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 - Investigation of Macromer Heterogeneity by 2D-HPLC and MALDI-TOF-MS T2 - Präsentationsveranstaltung des Instituts für Angewandte Chemie Berlin-Adlershof e.V. CY - Berlin, Germany DA - 1995-09-26 PY - 1995 CY - Berlin AN - OPUS4-2207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Flatau, S. A1 - Much, Helmut A1 - Schulz, Günter T1 - Hochleistungsflüssigchromatographie T2 - Statusseminar des ACA CY - Berlin, Deutschland DA - 1996-11-05 PY - 1996 AN - OPUS4-2210 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brehme, R. A1 - Gründemann, E. A1 - Schneider, M. A1 - Radeglia, Reiner A1 - Reck, Günter A1 - Schulz, Burkhard T1 - Aza-enamines X - Formylation of Pyrazole-4-carbaldehyde Hydrazones at the Hydrazonoazomethine C-Atom N2 - 1,3-Disubstituted 1H-pyrazole-4-carbaldehyde-N,N-di­methylhydrazones 1 reacted with the Vilsmeier-Haackreagent, corresponding to the aza-enamine concept, in an electrophilicsubstitution reaction at the azomethine C-atom yielding the 1,4,5-triaza-pentadieniumsalts 2. These were hydrolysed to give2-hydrazono-2-(1H-pyrazole-4-yl)ethanals 3. The electrophilic attack did not takeplace at the vinylogous position 5' of the pyrazoles. KW - Aza-enamines KW - Hydrazones KW - Heterocycles KW - Formylation KW - Alpha-oxoethanals PY - 2003 DO - https://doi.org/10.1055/s-2003-40527 SN - 0039-7881 SN - 1437-210X IS - 10 SP - 1615 EP - 1619 PB - Thieme [u.a.] CY - Stuttgart AN - OPUS4-2617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brehme, R. A1 - Reck, Günter A1 - Schulz, Burkhard A1 - Radeglia, Reiner T1 - Synthesis and Reactions of (1E,2Z)-2-N,N-Dialkylhydrazono-2-phenylethanal N,N-Dimethylhydrazones N2 - (1E,2Z)-2-N,N-Dialkylhydrazono-2-phenylethanal N,N-dimethylhydrazones 3a-e weresynthesised by the reaction of 1,4,5-triazapentadienium salts 2 with N,N-dimethylhydrazine. The compounds 3a and 3d didnot react with tosyl isocyanate in an electrophilic substitutionreaction at the azomethine C-1 as aza-enamines, but they reactedat room temperature in benzene in a 1,4-dipolar cycloaddition toyield 1,3,5-triazinan-2,4-diones 5a and 5d, whereas at 70 °Coctahydroimidazoimidazol-2,5-dione 6a wasformed via criss-cross addition reaction. With dimethyl sulfatein DMF, 3a was transformed into the trimethylhydrazoniumsalts 7a and 8a,isolated as co-crystallised perchlorates (molar ratio 1:1). KW - Aza-enamines KW - Heterocycles KW - Hydrazonium salts KW - 1,4-dipolar cycloaddition KW - Criss-cross addition reaction PY - 2003 DO - https://doi.org/10.1055/s-2003-40528 SN - 0039-7881 SN - 1437-210X IS - 10 SP - 1620 EP - 1625 PB - Thieme [u.a.] CY - Stuttgart AN - OPUS4-2618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H.R. A1 - Vakhtangishvili, L. A1 - Schwarz, G. A1 - Schulz, Günter A1 - Krüger, Ralph-Peter T1 - Macrocycles 25. Cyclic poly(ether sulfone)s derived from 4-tert-butylcatechol N2 - Poly(ether sulfone)s were prepared by polycondensation of silylated 4-tert-butylcatechol and 4,4?-difluorodiphenylsulfone in N-methylpyrrolidone. The feed ratio and the reaction time were varied to study the influence of stoichiometry and conversion on molecular weight and extent of cyclization. Molecular weights and molecular weight distributions (MWD)s were characterized by SEC measurements calibrated with polystyrene. Light scattering confirmed that calibration with polystyrene gives reasonable results and revealed a tendency towards a bimodal MWD for the samples rich in cycles. The MALDI-TOF mass spectrometry indicated that the extent of cyclization increased with higher conversion and with optimization of the stoichiometry. This interpretation was confirmed by 1H NMR endgroup analyses. For the samples with the highest molar masses only mass peaks of cycles were found, which were detectable up to 20 000 Da before and up to 27 000 Da after fractionation. Via the pseudo-high dilution method low molar mass poly(ether sulfone) containing more than 95 mol% of cycles were prepared, and even these low molar mass samples had broad MWDs. DSC measurements indicated that the glass transition temperatures depend on the structure of the endgroups and increase with higher fractions of cycles. KW - Poly(ether sulfone)s KW - Polycondensation KW - MALDI-TOF mass spectrometry PY - 2003 DO - https://doi.org/10.1016/S0032-3861(03)00410-5 SN - 0032-3861 SN - 1873-2291 VL - 44 SP - 4471 EP - 4480 PB - Springer CY - Berlin AN - OPUS4-2623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reck, Günter A1 - Orgzall, I. A1 - Schulz, B. T1 - 2,5-Di-p-tolyl-1,3,4-oxa­diazo­le N2 - The mol­ecule of the title compound, C16H14N2O, consists of two equivalent parts related by a twofold axis of the space group. The O atom occupies a special position on this twofold axis. PY - 2003 DO - https://doi.org/10.1107/S1600536803014867 SN - 1600-5368 VL - 59 IS - 8 SP - o1135 EP - o1136 PB - Munksgaard CY - Copenhagen AN - OPUS4-2609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aree, T. A1 - Reck, Günter A1 - Schulz, Burkhard T1 - Crystal Structures of ß-Cyclodextrin Complexes with Formic Acid and Acetic Acid N2 - ß-Cyclodextrin (ߖCD)-formic acid (1) and ß-CD–acetic acid (2) inclusion complexes crystallizeas ß-CD...0.3HCOOH...7.7H2O and ß-CD...0.4CH3COOH...7.7H2O in themonoclinic space group P21 with comparable unit cell constants. Anisotropic refinement of atomic parameters against X-ray diffractiondata with Fo 2 > 2 (Fo 2) (986/8563 and 991/8358) converged at R-factors of 0.051 and 0.054 for 1 and 2,respectively. In both complexes, the ß-CD molecularconformation, hydration pattern and crystal packing are similar,but the inclusion geometries of the guest molecules are different.The ß-CD macrocycles adopt a ``round'' conformationstabilized by intramolecular, interglucose O3(n)...O2(n + 1)hydrogen bonds and their O6–H groups are systematically hydratedby water molecules. In the asymmetric unit, each complex contains one ß-CD, 0.3 formic acid (or 0.4 acetic acid), and 7.7 water moleculesthat are distributed over 9 positions. Water sites located in the ß-CD cavity hydrogen bond to the guest molecule. In thecrystal lattice, ß-CD molecules are packed in a typical ``herringbone'' fashion. In 1, the formic acid (occupancy 0.3) is entirely included in the ß-CD cavity such that its C atom is shifted from the O4-plane center to the ß-CD O6-side by 2.90 Å and C=O, C–-O bonds point to this side. In 2, the acetic acid (occupancy 0.4) is completely embedded in the ß-CD cavity, in which the carboxylic C atom is displaced from the O4-plane centerto the ß-CD O6-side by 0.87 Å; the C=O bond directsto the ß-CD O6-side and makes an angle of 15°to the ß-CD molecular axis. Furthermore, bothdimethyl-ß-CD-acetic acid and ß-CD-acetic acidcomplexes form a cage structure, showing that the small guestsenclosed entirely in the cavity either in ß-CD or indimethyl--CD do not affect the packing of the host macrocycles. KW - Acetic acid KW - Crystal structures KW - Beta-cyclodextrin KW - Formic acid KW - Hydrogen bond KW - Inclusion complex KW - X-ray analysis PY - 2003 DO - https://doi.org/10.1023/B:JIPH.0000003923.92981.0f SN - 1388-3127 SN - 0923-0750 SN - 1573-1111 VL - 47 IS - 1-2 SP - 39 EP - 45 PB - Kluwer Academics Publishers CY - Dordrecht AN - OPUS4-3707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H.R. A1 - Böhme, S. A1 - Schwarz, G. A1 - Krüger, Ralph-Peter A1 - Schulz, Günter T1 - Macrocycles 18. The Role of Cyclization in Syntheses of Poly(ether-sulfone)s N2 - Poly(ether-sulfone)s having an identical backbone were prepared by four different methods. First, silylated bisphenol A (BSBA) was polycondensed with 4,4'-difluorodiphenyl sulfone (DFDPS) and K2CO3 in N-methylpyrrolidone with variation of the temperature. Second, analogous polycondensation were conducted using CsF as catalyst (and no K2CO3). Third, CsF-catalyzed polycondensations BSBA and DFDPS were conducted in bulk up to 290 C. Fourth, free bisphenol was polycondensed with DFDPS or 4,4'-dichlorodiphenyl sulfone and K2CO3 in DMSO with azeotropic removal of water. MALDI-TOF mass spectroscopy revealed that the first method mainly yielded cyclic poly(ether-sulfone)s which were detected up to masses around 13 000 Da. These and other results suggest that these polycondensations take a kinetically kontrolled course at tempeatures 145 C. This interpretation is also valid for the fourth method where high yields of cycles were obtained with DFDPS. With the less reactive 4,4'-dichlorodiphenyl sulfone lower conversions, lower molecular weights and lower fractions of cycles were found. In contrast to KF (resulting from K2CO3) CsF cleaves the poly(ether sulfone) backbone at temperatures > 145 C. Smaller amounts of smaller cycles were found in these CsF-catalyzed polycondensations which were in this case the result of thermodynamically controlled "back-biting degradation". PY - 2001 DO - https://doi.org/10.1021/ma010218l SN - 0024-9297 SN - 1520-5835 VL - 34 SP - 8886 EP - 8893 PB - American Chemical Society CY - Washington, DC AN - OPUS4-2176 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 - Heß, H. A1 - Hübner, H. A1 - Sobisch, T. T1 - Umfassende analytische Charakterisierung handelsüblicher nichtionischer Tenside durch Kopplung von HPLC und MALDI-TOF-MS T2 - Dechema-Jahrestagung 1996 CY - Wiesbaden, Deutschland DA - 1996-05-21 PY - 1996 PB - DECHEMA CY - Frankfurt am Main AN - OPUS4-2220 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter A1 - Frey, H. T1 - Characterization of unusual Silsesquioxane-Based Polymer Architectures Based on the Coupling of Liquid Chromatography and MALDI-TOF-MS T2 - 11th International Symposium on Organosilicon Chemistry CY - Montpellier, France DA - 1996-09-01 PY - 1996 CY - Montpellier AN - OPUS4-2222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Pickard, M. A1 - Schulz, Günter A1 - Wachsen, O. T1 - Characterization of thermal and hydrolytic degradation of polylactides by Liquid Chromatography and MALDI-TOF mass spectrometry T2 - International Symposium on "Biodegradable Materials" and Hamburger Makromolekulares Symposium CY - Hamburg, Germany DA - 1996-10-07 PY - 1996 CY - Hamburg AN - OPUS4-2225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rikowski, E. A1 - Krüger, Ralph-Peter A1 - Much, Helmut A1 - Schulz, Günter T1 - Synthesis of Polyhedral Hexa-, Octa-, Deca- and Dodeca Silsesquioxanes, Separation by NP-HPLC, SEC and LACCC, Characterization by MALDI-TOF-MS T2 - 4. Münchener Silikontage CY - München, Germany DA - 1998-04-07 PY - 1998 VL - 4 AN - OPUS4-2234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -