TY - JOUR A1 - Pawlik, Alf A1 - König, R. A1 - Scholz, G. A1 - Kemnitz, E. A1 - Brunklaus, G. A1 - Bertmer, M. A1 - Jäger, Christian T1 - Access to local structures of HS-AIF3 and its precursor determined by high-resolution solid-state NMR KW - Aluminium fluoride KW - 27Al NMR KW - MQMAS KW - Amorphous materials KW - Catalysts PY - 2009 DO - https://doi.org/10.1021/jp904626k SN - 1932-7447 SN - 1089-5639 VL - 113 IS - 38 SP - 16674 EP - 16680 PB - Soc. CY - Washington, DC AN - OPUS4-20463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzaré, J.Y. A1 - Silly, G. A1 - Klein, J. A1 - Scholz, G. A1 - Stösser, R. A1 - Nofz, Marianne T1 - Electron paramagnetic resonance investigations of alpha-Al2O3 powders doped with Fe3+ ions: experiments and simulations N2 - Electron paramagnetic resonance (EPR) of Fe3+ ions in Al2O3 is studied in powder samples prepared by different routes and/or modified by thermal or mechanical treatments, with different doping levels and grain sizes. The measurements are performed in various frequency bands (S, X, K, Q and W) and with bimodal detection in X-band. Simulations of the spectra are achieved with a code designed for computing EPR powder spectra described by any spin Hamiltonian including second-, fourth-and sixth-order ZFS terms (S ? 7/2). The linewidths, intensities and lineshapes are accounted for. The lineshape is Gaussian at low Fe3+ concentration whereas it is Lorentzian for higher concentration. The linewidths are interpreted as the superimposition of three main contributions: intrinsic linewidth, dipolar broadening and broadening due to lattice imperfections. The latter is tentatively interpreted in terms of quadrupolar spin Hamiltonian parameter distributions treated using first-order perturbation theory. Whatever the sample, only the b22 spin Hamiltonian parameter is found to be distributed around a mean zero value which corresponds to rhombic distortions. Angle and bond length distributions are tentatively extracted from the b22 distributions which gives some insight into the local order around the spin probe in relation to the preparation and treatment of the samples. PY - 2002 DO - https://doi.org/10.1088/0953-8984/14/43/329 SN - 0953-8984 SN - 1361-648X VL - 14 SP - 10331 EP - 10348 PB - IOP Publ. Ltd. CY - Bristol AN - OPUS4-2261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stösser, R. A1 - Scholz, G. A1 - Buzaré, J.-Y. A1 - Silly, G. A1 - Nofz, Marianne A1 - Schultze, Dietrich T1 - A magnetic resonance investigation of the process of corundum formation starting from sol-gel precursors PY - 2005 SN - 0002-7820 SN - 1551-2916 VL - 88 IS - 10 SP - 2913 EP - 2922 PB - Blackwell Publishing CY - Malden AN - OPUS4-11888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nofz, Marianne A1 - Stößer, R. A1 - Sebastian, S. A1 - Scholz, G. A1 - Willer, M. A1 - Jeschke, G. A1 - Schweiger, A. T1 - Pulse EPR Spectroscopy of Cu2+ - Doped Inorganic Glasses KW - EPR Spectroscopy KW - Inorganic glasses PY - 1999 SN - 0937-9347 SN - 1613-7507 IS - 16 SP - 507 EP - 528 PB - Springer CY - Wien AN - OPUS4-760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Burgbacher, G. A1 - Kafka, P. A1 - Klein, G. A1 - Konersmann, Rainer A1 - Loock, J. A1 - Rupp, M. A1 - Scholz, A. A1 - Seel, H. A1 - Spitzer, C. T1 - Risikoabschätzung Chlorlagerung/Chlortransport unter Einbeziehung der Seveso II-Richtlinie und der Störfallverordnung (2000) N2 - Die BAM, Berlin, die Gesellschaft für Anlagen- und Reaktorsicherheit (GRS), Köln, und der TÜV Süd, München, erarbeiteten eine vergleichende Untersuchung (Risikostudie) an einer realen Anlage zur Lagerung - einschließlich des Transports - von Chlor als für die Studie geeigneten gefährlichen Stoff. T3 - BAM Forschungsberichtreihe - 269 PY - 2005 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-1820 SN - 978-3-86509-319-1 SN - 0938-5533 VL - 269 SP - 1 EP - 240 PB - Wirtschaftsverlag NW CY - Bremerhaven AN - OPUS4-182 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Vogel, Christian A1 - Schuck, G. A1 - Simon, Franz-Georg T1 - Speciation of copper and zinc compounds relevant for the hazard property (HP) 14 classification of municipal solid waste incineration bottom and fly ashes N2 - The analysis of the presence and content of substances that are toxic to aquatic life in waste is essential for classification of waste with regard to hazard property (HP) 14 ‘ecotoxic’. For the determination of HP14 classified copper (Cu) and zinc (Zn) compounds in various municipal solid waste incineration bottom ashes (IBA) and one fly ash (FA) from Germany we applied X-ray absorption near-edge structure (XANES) spectroscopy in combination with linear combination fitting. The analysis showed that approx. 50–70% of Cu in the IBA are Cu(I) compounds and elemental Cu(0), but these compounds were not equally distributed in the different IBA. In contrast, the majority (approx. 50–70%) of Zn in all IBA is elemental zinc, which originates from brass or other alloys and galvanized metals with a large content of zinc in the waste. The FA contain higher mass fraction on Zn and other toxic elements, but similar Cu and Zn species. Additional performed selective extraction at a pH of 4 with an organic acid of some IBA showed that the ecotoxic Zn fraction is mainly elemental zinc and zinc oxide. In contrast, for the ecotoxic Cu fraction within the IBA no specific compound could be identified. Furthermore, the XANES analysis showed that the HP14 properties of especially Cu in IBA is overestimated with current best-practice guidelines for sample processing for the current substance-related approach with the 0.1% cut-off rule for each substance. However, it should be considered whether it would not be better from an environmental point of view to take the ecotoxicologically leachable copper and zinc as a reference value. KW - Thermal waste treatment KW - XANES spectroscopy KW - Ecotoxicity KW - Incineration bottom ash PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609584 DO - https://doi.org/10.1016/j.wasman.2024.09.001 VL - 189 SP - 421 EP - 426 PB - Elsevier Ltd. AN - OPUS4-60958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breitfeld, Steffen A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - BaF-benzenedicarboxylate: the first mechanochemical N2 - Anewbariumcoordination polymer, BaF-benzenedicarboxylate (BaF(p-BDC)0.5), with fluorine directly coordinated to the metal cation, was prepared by mechanochemical synthesis routes. Phase-pure BaF-benzenedicarboxylate was synthesized by milling starting either from barium hydroxide or from Barium acetate as sources for barium cations. In both cases, the second reactant was 1,4-benzenedicarboxylic acid (H2(p-BDC)). Ammonium fluoride was used as fluorinating agent directly at milling. This is the first mechanochemical synthesis of coordination polymers where fluorine is directly coordinated to the metal cation. Following the second possibility, barium acetate fluoride (Ba(OAc)F) is formed as ntermediate product after milling, and the new coordination polymer is accessible only after washing with water and dimethyl sulfoxide. The new compound BaF(p-BDC)0.5 was characterized by X-ray powder diffraction, FTIR-, and 19F, 1H-13C CP MAS NMR spectroscopies, DTA-TG, and elemental Analysis. KW - Milling KW - MOF PY - 2018 DO - https://doi.org/10.1007/s10853-018-2331-3 SN - 0022-2461 VL - 53 IS - 19 SP - 13682 EP - 13689 PB - Springer AN - OPUS4-45677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jentsch, H. A1 - Schwartz, A. A1 - Basedau, Frank A1 - Bazrafshan, K. A1 - Döring, H. A1 - Großwig, S. A1 - Hofmann, Detlef A1 - Kowalle, G. A1 - Kusche, Nadine A1 - Lorenz, R. A1 - Pfeiffer, T. A1 - Sadaghiani, M.R.S. A1 - Scholz, E. A1 - Senze, A. A1 - Tkachenko, Viktoriya A1 - Witt, K. J. ED - Xu, Y. L. ED - Zhu, S. ED - Xia, Y. ED - Ni, Y.Q. ED - Law, S.S. ED - Yin, J. H. ED - Su, Z.Q. T1 - Detection of slipping soil areas with embedded tiny vertical sensing rods N2 - Critical soil zones where large areas along a shear joint might begin to slip should be recognized. In order to avoid damage, monitoring of such unstable zones is necessary. First, soil movements must be detected as early as possible, second, the amount of deformation should be estimated. Because geodetical methods do not provide information about deformation in the underground in different depths, the only way to come to information from possible shear zones is the installation of deformation measurement systems. A special installation method was developed to bring a long-gauge length measurement system into a borehole and transfer data of soil deformations into an installed sensing rod. The mostly vertically installed sensing rod has an outer diameter of 3 mm to 6 mm and contains several optical fibres. One fibre provides integral strain information along the whole length of the rod. To get this information, the phase difference between the fibre input and output is measured and the change of the total length of the fibre can be derived. This easy and cheap online sensing system delivers an early warning of soil deformations respectively possible slip as well as landslides. In case of warning, the second sensing system based on Fibre Bragg Grating sensors located close to the expected shear zone purposefully. It records resulting deformations in detail. In this study, three main objectives were achieved: a) development of tiny pultruded sensing rods with integrated optical sensor fibres, b) installation technology which enables the integration of the sensing rod during drilling and pile driving, and c) development of a stiff but elastic racking material to fix the rod in the soil and to transfer soil deformation into the stiffer sensing rod. These three aspects including the fibre optical measurement systems are described; results from Press Deformation Test (PDT) are presented. Test results of the fibre optical online system are compared and evaluated with the results of conventional inclinometer measurements as well as numerical modelling. An outlook for further possibilities of usage of this monitoring system is given. T2 - SHMII-6 - 6th International conference on structural health monitoring of intelligent infrastructure CY - Hong Kong, China DA - 09.12.2013 KW - Structural health monitoring KW - Soil stability monitoring KW - Optical fibre strain-sensor KW - Geotechnical soil stability KW - Soil deformation modelling PY - 2013 SN - 978-962-367-768-4 SP - 1 EP - 9 AN - OPUS4-29915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - König, R. A1 - Scholz, G. A1 - Kemnitz, E. T1 - Crystalline aluminium hydroxy fluorides: Structural insights obtained by high field solid state NMR and 27Al chemical shift trend analysis T2 - Gesellschaft Deutscher Chemiker CY - Regensburg, Germany DA - 2008-09-22 PY - 2008 AN - OPUS4-17956 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - König, R. A1 - Scholz, G. A1 - Kemnitz, E. T1 - Crystalline aluminium hydroxyl fluorides: Structural insights obtained by high-field solid state NMR and 27Al chemical shift trend analysis T2 - Gesellschaft Deutscher Chemiker CY - Regensburg, Germany DA - 2008-09-22 PY - 2008 AN - OPUS4-17957 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - König, R. A1 - Scholz, G. A1 - Scheurell, K. A1 - Heidemann, D. A1 - Buchem, I. A1 - Unger, Wolfgang A1 - Kemnitz, E. T1 - Spectroscopic characterization of crystalline AIF3 phases N2 - A comprehensive spectroscopic characterization of all known crystalline AlF3 phases (α-, β-, η-, κ-, θ-AlF3) is presented for the first time in this study. Beside their X-ray diffraction powder patterns, which were already published in the literature, 27Al and 19F MAS NMR, FT IR and XPS spectroscopic techniques were applied for all phases in a consistent manner. For all phases prepared the utilization of 27Al satellite transition (SATRAS) NMR allowed to determine the quadrupolar parameters of the aluminium sites including their distributions. In addition, η-AlF3 was isolated with high phase purity and characterized following a new preparation path different from those known so far in the literature. KW - Crystalline aluminium fluorides KW - Solid state NMR KW - FT IR KW - XPS PY - 2010 DO - https://doi.org/10.1016/j.jfluchem.2009.10.015 SN - 0022-1139 SN - 1873-3328 VL - 131 IS - 1 SP - 91 EP - 97 PB - Elsevier CY - Amsterdam AN - OPUS4-20991 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 - 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 - König, R. A1 - Scholz, G. A1 - Pawlik, Alf A1 - Jäger, Christian A1 - Rossum, B. van A1 - Kemnitz, E. T1 - Identification of AIFx(OR)y species in strongly disordered aluminium isopropoxide fluoride solids: a field-dependent MAS NMR study KW - Ultra high-field MAS NMR (21.1T) KW - 27 Al MAS solid state NMR KW - Fluoride xerogels KW - Sol-gel process KW - Fluorolysis KW - Quadrupolar nuclei PY - 2009 DO - https://doi.org/10.1021/jp9066795 SN - 1932-7447 SN - 1089-5639 VL - 113 IS - 35 SP - 15576 EP - 15585 PB - Soc. CY - Washington, DC AN - OPUS4-20461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan A1 - Dreßler, Martin A1 - Nofz, Marianne A1 - Pauli, Jutta A1 - Jäger, Christian A1 - Scholz, G. ED - Krämer, V. T1 - Phasentransformationen von anorganisch modifizierten Alumo-Xerogelen T2 - Jahrestagung der Gesellschaft für Thermische Analyse e.V. CY - Augsburg, Deutschland DA - 2003-09-15 PY - 2003 SP - 1 EP - 2 AN - OPUS4-2668 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nofz, Marianne A1 - Stösser, R. A1 - Scholz, G. A1 - Dörfel, Ilona A1 - Schultze, Dietrich T1 - The thermally induced transformation of pseudoboehmite gels - a comparison of the effects of corundum seeding and iron doping N2 - The transformation of doped or seeded pseudoboehmite to corundum was studied by combining thermal analysis, X-ray diffraction, transmission electron microscopy, and electron paramagnetic resonance spectroscopy. The temperature of phase transformation to corundum was lowered by about 130 °C when Fe3+ or corundum seeds were added to the sols. Action of Fe3+ ions depends on the actual degree of thermally induced transformation of pseudoboehmite via transition aluminas to corundum and the ability of these alumina phases to incorporate Fe3+ ions. These ions tend to aggregate with increasing iron concentration of the alumina phases and can work as nucleation centers. Small (not, vert, similar20 nm) corundum particles act as active nucleation sites whereas larger grains (200–400 nm) also present in the samples are less effective. For the first time trapping and stabilization of NO2 molecules in transition aluminas formed by a sol–gel route was shown. KW - Grain size KW - Sol-gel processes KW - Electron microscopy KW - X-ray methods KW - Al2O3 PY - 2005 DO - https://doi.org/10.1016/j.jeurceramsoc.2004.04.014 SN - 0955-2219 SN - 1873-619X VL - 25 IS - 7 SP - 1095 EP - 1107 PB - Elsevier CY - Oxford AN - OPUS4-7455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Nofz, Marianne A1 - Feist, M. A1 - Scholz, G. T1 - Fe3+-assisted formation of alpha-Al2O3, starting from sol-gel precursors N2 - The role of Fe3+ ions in the transformations from boehmites and pseudoboehmite xerogels via transition aluminas to corundum was studied here. Especially, the active iron species responsible for the decrease of the temperature of transformation to corundum were looked for. To enable the formation of various Fe3+ and Fe2+ species, samples were subjected to thermal treatments in different atmospheres as well as mechanically activated. Thermal analysis and ESR spectroscopy served to follow the processes and to characterise the resulting products. It was found that (i) isolated Fe3+ ions can indicate local structural changes but have (almost) no influence on the temperature of corundum formation, (ii) the temperature of corundum formation decreases in the result of action of small α-Fe2O3 particles and (iii) during thermal treatments Fe3+ ions are distributed between different phases or precursors thereof: transition aluminas, corundum, Fe2O3, and a Fe3+ pool. KW - Redox process KW - ESR spectroscopy KW - Thermal analysis KW - Sol-gel process KW - Boehmite KW - Corundum PY - 2006 DO - https://doi.org/10.1016/j.jssc.2005.11.026 SN - 0022-4596 SN - 1095-726X VL - 179 IS - 3 SP - 645 EP - 657 PB - Elsevier CY - San Diego, Calif. AN - OPUS4-11889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholz, G. T1 - Solid state MAS NMR and solid state EPR investigations of nanostructured AIF3 powders obtained by mechanical milling T2 - Tag der Chemie an der FU CY - Berlin, Germany DA - 2005-06-08 PY - 2005 AN - OPUS4-12189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholz, G. T1 - A magnetic resonance investigation of nanostructured solid fluorides obtained by high-energy ball milling T2 - Magnetresonanztagung GdCh CY - Davos, Switzerland DA - 2005-08-28 PY - 2005 AN - OPUS4-12191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholz, G. T1 - A magnetic resonance investigation of nanostructured solid fluorides obtained by high-energy ball-milling T2 - Magnetresonanztagung GdCh CY - Davos, Switzerland DA - 2005-08-28 PY - 2005 AN - OPUS4-12192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -