TY - JOUR A1 - Barheine, Sabrina A1 - Hayakawa, S. A1 - Osaka, A. A1 - Jäger, Christian T1 - A NMR investigation of borate incorporation in apatitic biomaterials N2 - The incorporation of ions in the lattice of hydroxyapatite alters significantly its structure. Particularly, if anions such as trigonal borate units are accommodated in the lattice severe distortions must occur around the substitution site because of different geometric shape, electric charge and anion size. Solid-state NMR has been used to investigate this problem in detail for a hydroxyapatite sample synthesized by high temperature solid state reaction. The results clearly verify the existence of network distortions. Indeed, only about 1/3 of the total phosphate content forms crystalline hydroxyapatite (also found in XRD) whereas the residual amount is contained in two different phosphate sites with 31P chemical shifts of 5.5 ppm and 2.3 ppm, but broad resonances lines suggesting disorder. Furthermore, a novel proton signal at -0.6 ppm was found which is directly associated with the borate incorporation. No specific correlation of the two structurally different borate units with the two phosphate groups is found. KW - Apatite KW - Borate KW - Biomaterials KW - Solid-state NMR PY - 2009 UR - http://www.scientific.net/0-87849-353-0/205/ DO - https://doi.org/10.4028/3-908453-07-0.205 SN - 1013-9826 VL - 396-398 SP - 205 EP - 208 PB - Trans Tech Publ. CY - Aedermannsdorf AN - OPUS4-18914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yoneda, Y. A1 - Mereiter, K. A1 - Jäger, Christian A1 - Brecker, L. A1 - Kosma, P. A1 - Rosenau, T. A1 - French, A. T1 - Van der Waals versus Hydrogen-Bonding Forces in a Crystalline Analog of Cellotetraose: Cyclohexyl 4'-O-Cyclohexyl Beta-D-Cellobioside Cyclohexane Solvate KW - Cellobioside KW - Cellotetraose KW - Cellulose KW - Solid state NMR PY - 2008 DO - https://doi.org/10.1021/ja805147t SN - 0002-7863 SN - 1520-5126 VL - 130 SP - 16678 EP - 16690 PB - American Chemical Society CY - Washington, DC AN - OPUS4-18915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jäger, Christian T1 - NMR beyond limits: Surfaces of phosphate nanoparticles and interface in biomaterials T2 - Universität Mainz CY - Mainz, Germany DA - 2007-12-17 PY - 2007 AN - OPUS4-19189 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karrasch, Andrea A1 - Jäger, Christian A1 - Saake, B. A1 - Potthast, A. A1 - Rosenau, T. T1 - Solid-state NMR studies of methyl celluloses. Part 2: Determination of degree of substitution and O-6 vs. O-2/O-3 substituent distribution in commercial methyl cellulose samples N2 - Solid state NMR spectroscopy was applied to determine the overall degree of substitution (DS) and the degrees of substitution at C-6 (DSC-6) and C-2/3 (DSC-2/3). Four commercial methyl cellulose samples were used, having a DS between 0.51 and 1.96 as determined by wet-chemical analysis. The strategy and optimization of the NMR data acquisition as well as the data evaluation procedures are explained in detail. Optimization of the approach mainly comprised (a) maximizing the signal by choice of NMR probe, MAS spinning frequency and B0 field, (b) minimizing the measurement time by a Torchia-type experiment and (c) suppressing probe background by rotor-synchronized echo detection. Data evaluation used simply the integration of three different spectral ranges in the 13C NMR spectrum. The results of the experiments were in good agreement with the wet-chemical data. The NMR approach takes about the same analysis time as the conventional hydrolysis/chromatography analysis. However, it is a generally applicable and simple alternative without need for an extended sample preparation which is most useful if wet-chemical/chromatographic analyses are undesired or unavailable. Further studies have to concentrate on the validation of the analytical method and application to a larger sample array. KW - Methyl cellulose KW - Solid-state NMR KW - 13C CPMAS NMR KW - Rotor-synchronized echo sequence KW - Substituent distribution KW - Substitution pattern KW - Degree of substitution PY - 2009 DO - https://doi.org/10.1007/s10570-009-9304-2 SN - 0969-0239 SN - 1572-882X VL - 16 IS - 6 SP - 1159 EP - 1166 PB - Chapman & Hall CY - London AN - OPUS4-21130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, W. A1 - Kurzhals, R. A1 - Sauerbeck, S. A1 - Toufar, H. A1 - Buhl, J.-C. A1 - Gesing, T. A1 - Altenburg, Wolfgang A1 - Jäger, Christian T1 - Hydrothermal stability of zeolite SAPO-11 N2 - The hydrothermal stability of SAPO-11 was studied in water of autogenous pressure as function of the temperature. SAPO-11 remained crystalline up to 190 °C. Thereby, it was observed, parent as well as hydrothermally treated samples showed similarities to the isotypic structure of zeolite AlPO-11 called here AELdry. After fully hydration of the samples, AELdry changed completely into a hydrated AELwet structure of another framework symmetry. The transition from calcined to hydrated state was reversible for both the parent and the hydrothermally treated samples. 27Al and 31P NMR MAS spectra showed a single resonance typical for AlPO4 type tetrahedra for the calcined parent and hydrothermally treated samples. Upon hydration, the single AlPO4 resonance signal split into three different signals as is the case for the corresponding 31P signals. By means of NH3-TPD measurement a loss of acidity was detected after the hydrothermal treatment as follows from a framework desilication. Nitrogen and water adsorption decreased systematically. At 210 °C a non-zeolitic, non-porous phase was irreversibly formed. The XRD pattern of this phase shows resemblance to a synthetic aluminium phosphate of the tridymite structure type. KW - Zeolite KW - Silicoaluminophosphate KW - SAPO-11 KW - Hydrothermal stability KW - Phase transformation PY - 2010 DO - https://doi.org/10.1016/j.micromeso.2009.08.003 SN - 1387-1811 SN - 1873-3093 VL - 132 IS - 1-2 SP - 31 EP - 36 PB - Elsevier CY - Amsterdam AN - OPUS4-21131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Debatin, F. A1 - Thomas, A. A1 - Kelling, A. A1 - Hedin, N. A1 - Bacsik, Z. A1 - Senkovska, I. A1 - Kaskel, S. A1 - Junginger, M. A1 - Müller, H. A1 - Schilde, U. A1 - Jäger, Christian A1 - Friedrich, A. A1 - Holdt, H.-J. T1 - In situ synthesis of an imidazolate-4-amide-5-imidate ligand and formation of a microporous zinc-organic framework with H2-and CO2-storage ability KW - Metal-organic framework KW - Synthesis KW - XRD KW - FTIR KW - NMR KW - Gas sorption KW - Microporous materials KW - N,O ligands KW - Solvothermal synthesis PY - 2010 DO - https://doi.org/10.1002/anie.200906188 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 49 IS - 7 SP - 1258 EP - 1262 PB - Wiley-VCH CY - Weinheim AN - OPUS4-21132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, G. A1 - Krahl, Thoralf A1 - Ahrens, M. A1 - Martineau, C. A1 - Buzaré, J.Y. A1 - Jäger, Christian A1 - Kemnitz, E. T1 - 115In and 19F MAS NMR study of (NH4)3InF6 phases N2 - This study presents for the first time an NMR spectroscopic characterization of the room and high temperature phases of (NH4)3InF6 using 19F and 115In as probe nuclei. The reversible phase transition to the cubic phase at 353 K was followed by MAS NMR in situ. Static NMR experiments of the room temperature phase and MAS NMR experiments of the high temperature phase allowed the determination of the NMR parameters of both nuclei. Finally, the scalar In–F coupling, rarely observed in solid state NMR, is evidenced in both room and high temperature phases of (NH4)3InF6, and measured in the high temperature phase. KW - (NH4)3InF6 KW - 115In and 19F solid state NMR KW - XRD PY - 2011 DO - https://doi.org/10.1016/j.jfluchem.2011.01.010 SN - 0022-1139 SN - 1873-3328 VL - 132 IS - 4 SP - 244 EP - 249 PB - Elsevier CY - Amsterdam AN - OPUS4-23475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dreßler, Martin A1 - Nofz, Marianne A1 - Pauli, Jutta A1 - Jäger, Christian T1 - Influence of polyvinylpyrrolidone (PVP) on alumina sols prepared by a modified Yoldas procedure N2 - Al13 polycations containing alumina sols, prepared by a modified Yoldas procedure were mixed with polyvinylpyrrolidone (PVP). Although Al speciation in freshly prepared sols was not affected by PVP addition the decay rate of Al13 polycations was slightly decreased in PVP-containing sols. PVP does not show any influence on particle size and particle growth. The influence of PVP addition on viscosity and flow behavior of modified Yoldas sols depends on their solids content and NO3-/Al molar ratio. KW - ModifiedYoldas sols KW - PVP KW - NMR KW - Rheology KW - Particle size KW - Aging PY - 2008 DO - https://doi.org/10.1007/s10971-008-1798-9 SN - 0928-0707 SN - 1573-4846 VL - 47 IS - 3 SP - 260 EP - 267 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-17854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karrasch, Andrea A1 - Jäger, Christian T1 - Thermal decomposition of PDMS in flame-retarded bisphenol-A polycarbonate: A solid-state NMR investigation T2 - GDCh-Tagung Magnetische Resonanz 2008 CY - Regensburg, Germany DA - 2008-09-22 PY - 2008 AN - OPUS4-17831 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jäger, Christian T1 - Bulk and surfaces of nanosized calcium phosphates and their interaction with organic molecules in bone and synthetic biomaterials T2 - The 6th International Symposium on Inorganic Phosphate Materials (ISIPM-6- La Rochelle 2008) CY - La Rochelle, France DA - 2008-08-24 PY - 2008 AN - OPUS4-17883 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jäger, Christian A1 - Barheine, Sabrina T1 - A NMR investigation of borate incorpation in apatitic biomaterials T2 - 21st International Symposium of Ceramics in Medicine - Bioceramics 21 CY - Búzios, Brazil DA - 2008-10-21 PY - 2008 AN - OPUS4-17884 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jäger, Christian T1 - Mission Impossible? Surfaces of phosphate nanoparticles and the mineral-organic interface in biomaterials T2 - Max-Planck-Institut für Chemische Physik Fester Stoffe CY - Dresden, Germany DA - 2008-05-09 PY - 2008 AN - OPUS4-17885 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jäger, Christian T1 - Mission Impossible? Surfaces of phosphate nanoparticles and the mineral-organic interface in biomaterials T2 - Seminar "Festkörper-NMR-Methoden und Anwendungen in der Materialforschung", Universität Tübingen CY - Bad Hindelang, Germany DA - 2008-07-13 PY - 2008 AN - OPUS4-17886 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aguiar, H. A1 - Solla, E.L. A1 - Serra, J. A1 - González, P. A1 - León, B. A1 - Malz, Frank A1 - Jäger, Christian T1 - Raman and NMR study of bioactive Na2O-MgO-CaO-P2O5-SiO2 glasses N2 - The results of a structural study combining NMR and Raman spectroscopy of several melt-derived glasses in the system Na2O–MgO–CaO–P2O5–SiO2 are presented. The Raman spectra show clear changes in the Si–O–Si vibrational modes (related to the bridging oxygen atoms, BO) and also verify the presence of non-bridging oxygen atoms (NBO), also named terminal oxygens. The intensity of the Si–O–NBO stretching mode depends on the cation concentration. It can be concluded from the NMR studies that the MgO-containing samples have orthophosphate units charge-compensated by Ca2+ and Mg2+. The silicate matrix also contains both types of two-valent cations and consists of Q2 and Q1 units. Similarly, the Na2O-containing samples contain isolated orthophosphate units in a silicate matrix (Q2 and Q3 units), both charge-compensated by mixed cations Ca2+ and Na+. These experimental data were compared with theoretical parameters given by the Stevels model, which is a suitable tool for understanding bioactive behavior of these glasses. Furthermore, results of the in vitro tests carried out in simulated body fluids are presented and compared with both Raman and NMR structural data. KW - Raman KW - NMR KW - Solid state KW - Bioactive glasses KW - Glass ceramics PY - 2008 DO - https://doi.org/10.1016/j.jnoncrysol.2008.07.033 SN - 0022-3093 VL - 354 IS - 45-46 SP - 5004 EP - 5008 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-18364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - König, R. A1 - Scholz, G. A1 - Pawlik, Alf A1 - Jäger, Christian A1 - van Rossumm, B. A1 - Oschkinat, H. A1 - Kemnitz, E. T1 - Crystalline Aluminium Hydroxy Fluorides: Structural Insights Obtained by High Field Solid State NMR and Trend Analyses N2 - A series of crystalline aluminum hydroxy fluorides in cubic pyrochlore structure AlFx(OH)3-x·H2O with variable F-content x were investigated by solid-state NMR by applying different magnetic fields up to 21.1 T. Distinguishable octahedral species AlFx(OH)6-x (x = 1-6) were identified in the crystalline aluminum hydroxy fluorides. The subsequent analysis of the highfield 27Al MAS NMR data allows the derivation of the trend analysis graphs giving correlations between the 27Al chemical shifts and the quadrupolar frequencies and the F-content x in AlFx(OH)6-x. Clear trends were obtained for both, which are, along with the 19F MAS chemical-shift trend analysis presented earlier, valuable tools for the interpretation of MAS NMR spectra of amorphous AlFx(OX)3-x compounds (X = H, alkyl). Following the dehydration of the pyrochlores by solid-state NMR eventually reveals a remarkable influence of the incorporated solvent molecules (H2O) on the 19F chemical shift. On that basis, a new chemical-shift trend analysis for 19F chemical shifts in correlation with x in AlFx(OH)6-x units for proton-poor substances (in the Al, F, O, H system) was determined. By using this correlation, high-surface AlF3 has a mean bulk Al:F ratio similar to that found for ACF, namely, AlF2.8(O/OH)0.2. KW - Aluminium-27 KW - Crystalline aluminium hydroxy fluorides KW - Chemical shift trend analysis KW - High field solid state NMR KW - Quadrupolar nuclei PY - 2008 DO - https://doi.org/10.1021/jp804662f SN - 1932-7447 SN - 1089-5639 VL - 112 IS - 40 SP - 15708 EP - 15720 PB - Soc. CY - Washington, DC AN - OPUS4-18365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, T. A1 - Dai, Z. A1 - Drexler, H.-J. A1 - Baumann, W. A1 - Jäger, Christian A1 - Pfeifer, Dietmar A1 - Heller, D. T1 - Novel contributions to the mechanism of the enantioselective hydrogenation of dimethyl itaconate with rhodium complexes KW - Enantioselective Hydrogenation KW - Rhodium-Phosphor-Complex KW - Powder Diffractometry KW - Hr- and Solid State NMR-Spectroscpy KW - Asymmetric catalysis KW - Hydrogenation KW - Kinetics KW - Reaction mechanisms KW - Rhodium PY - 2008 DO - https://doi.org/10.1002/chem.200800389 SN - 0947-6539 SN - 1521-3765 VL - 14 IS - 15 SP - 4469 EP - 4471 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-18368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maltsev, Sergey A1 - Jäger, Christian T1 - Solid-state NMR spectroscopy using the lost I spin magnetization in polarization transfer experiments N2 - A variation of the cross polarization (CP) experiment is discussed. The method requires two scans where the difference signal is equivalent to the I spin magnetization that is transferred to the S spins. The acquired signal is equivalent to F1 sum projection of a two-dimensional (2D) heteronuclear correlation experiment and is obtained by just two scans without the need to increment the indirect time domain t1. Any polarization transfer method and any kind of spin manipulations during the t1 incrementation period of a 2D NMR experiment can be applied. The method allows fast measurements of the CP transfer, particularly if various S spins signal overlap and is good for spectral editing of I spin signals with contact to S spins. Various examples for biomaterials are presented. Most importantly, this novel approach is ideal for detailed investigations of organic–mineral interfaces in bone, here demonstrated for O-phospho-L-serine as simple model compound. KW - NMR KW - Double resonance KW - Cross polarization KW - Heteronuclear correlation KW - Biomaterials KW - Hydroxyapaptite KW - Bone PY - 2008 DO - https://doi.org/10.1016/j.ssnmr.2008.08.001 SN - 0926-2040 SN - 1527-3326 VL - 34 IS - 3 SP - 175 EP - 179 PB - Academ. Press CY - Orlando, Fla. AN - OPUS4-18377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pawlik, Alf A1 - Jäger, Christian T1 - Catalytically active High-Surface Aluminiumfluoride and its Precursor a Solid-State NMR Study. T2 - 6th Alpine Conference on Solid-State NMR CY - Chamonix, France DA - 2009-09-13 PY - 2009 AN - OPUS4-19374 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krahl, Thoralf A1 - Jäger, Christian T1 - Predicting Phase Compositions of CA10(K,Na)(PO4)7 Melts by 31PMAS NMR T2 - 22nd International Symposium of Ceramics in Medicine - Bioceramics 22 CY - Daegu, South Korea DA - 2009-10-26 PY - 2009 AN - OPUS4-19416 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barheine, Sabrina A1 - Jäger, Christian T1 - Surface, interface and bulk structure of borate containing apatitic biomaterials T2 - The Alpine Conference on Solid-State NMR CY - Chamonix, France DA - 2009-09-13 PY - 2009 AN - OPUS4-19370 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karrasch, Andrea A1 - Jäger, Christian T1 - Solid-state NMR Studies of Methyl Celluloses T2 - The Alpine Conference on Solid-State NMR CY - Chamonix, France DA - 2009-09-13 PY - 2009 AN - OPUS4-19372 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -