TY - JOUR
A1 - Schiffmann, J.
A1 - Emmerling, Franziska
A1 - Martins, Ines
A1 - Van Wüllen, L.
T1 - In-situ reaction monitoring of a mechanochemical ball mill reaction with solid state NMR
JF - Solid State Nuclear Magnetic Resonance
N2 - We present an approach towards the in situ solid state NMR monitoring of mechanochemical reactions in a ball mill. A miniaturized vibration ball mill is integrated into the measuring coil of a home-built solid state NMR probe, allowing for static solid state NMR measurements during the mechanochemical reaction within the vessel. The setup allows to quantitatively follow the product evolution of a prototypical mechanochemical reaction, the formation of zinc phenylphosphonate from zinc acetate and phenylphosphonic acid. MAS NMR investigations on the final reaction mixture confirmed a reaction yield of 89% in a typical example. Thus, NMR spectroscopy may in the future provide complementary information about reaction mechanisms of mechanochemical reactions and team up with other analytical methods which have been employed to follow reactions in situ, such as Raman spectroscopy or X-ray diffraction.
KW - Mechanochemistry
KW - Solid state NMR
KW - NMR probe Development
PY - 2020
DO - https://doi.org/10.1016/j.ssnmr.2020.101687
VL - 109
SP - 101687
PB - Elsevier Inc.
AN - OPUS4-51283
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, M.C.
A1 - Stroh, Julia
A1 - Malaga, K.
A1 - Meng, Birgit
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - Pathway of a damaging mechanism - Analyzing chloride attack by synchrotron based X-ray diffraction
JF - Solid state sciences
N2 - Typically, the changes of the phase compositions due to the chemical attack are studied in-situ only by chemical analysis or microscopy. In this study, the chloride transport and binding in the cement matrix in different cementitious materials was analyzed by synchrotron based X-ray diffraction (SyXRD) and energy dispersive X-ray spectroscopy (EDX). Sample materials consisting of cement paste were embedded in high concentrated sodium chloride solution over different time spans. Afterwards, the phase and chemical compositions were determined. The high spatial resolution and the information about the chloride distribution offer a detailed view of chloride binding in the cement matrix and allow the conclusions about the degradation mechanisms. The results are discussed related to the influence of different supplementary cementitious materials on the damaging mechanism.
KW - Portland cement
KW - In-situ
KW - X-Ray diffraction
KW - EDX
KW - Durability
KW - Chloride attack
PY - 2015
DO - https://doi.org/10.1016/j.solidstatesciences.2015.03.021
SN - 1293-2558
SN - 1873-3085
VL - 44
SP - 45
EP - 54
PB - Elsevier Masson SAS
CY - Amsterdam
AN - OPUS4-33171
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, Moritz-Caspar
A1 - Müller, Urs
A1 - Malaga, Katarina
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - Spatially resolved investigation of complex multi-phase systems using muXRF, SEM-EDX and high resolution SyXRD
JF - Cement & concrete composites
N2 - Spatially resolved analysis of complex multi-phase systems can be validated through different analytical methods. This study compares investigations by scanning electron microscopy coupled with energy dispersive X-ray fluorescence analysis and high resolution X-ray diffraction. The studied sulfate attacked cement paste containing fly ashes consists of different interacting crystalline and amorphous phases. The complementary methods revealed in detail changes in phase composition due to the chemical attack. The advantages and disadvantages of both methods are discussed and suggestions are given for combining them with additional methods to maximize the information content.
KW - EDX-SEM
KW - SyXRD
KW - Spatial investigations
KW - Comparison
KW - High resolution
KW - Cement paste
KW - Sulfate attack
KW - Damaging mechanism
PY - 2013
DO - https://doi.org/10.1016/j.cemconcomp.2012.08.018
SN - 0958-9465
SN - 1873-393X
VL - 37
SP - 241
EP - 245
PB - Elsevier Ltd.
CY - Barking, Essex
AN - OPUS4-29111
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, Moritz-Caspar
A1 - Müller, Urs
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - Deciphering the sulfate attack of cementitious materials by high-resolution micro-x-ray diffraction
JF - Analytical chemistry
N2 - The durability of cementitious materials depends, among others, on their resistance against chemical attack during the service life of a building. Here, we present an approach to analyze changes in the phase composition due to chemical attack in the form of sulfate ingress within the microstructure. Micro-X-ray (µX-ray) diffraction using synchrotron radiation in Debye–Scherrer (transmission) geometry allowed a spatial resolution of 10 µm. Phase transformations in the wake of damaging processes were observed in a detailed high-resolution imaging study. In comparison, samples containing supplementary cementitious materials were investigated and used to reconstruct the influence of different degeneration processes in detail. Additionally, reaction fronts within the bulk were localized by micro-X-ray fluorescence analysis. The experimental setup provided the possibility for analyzing the phase assemblage of a given sample without destroying the microstructure. The specimens for phase analysis are thick sections of the primary material and can be used for further microscopic analysis of the microstructure and microchemistry, e.g., scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDX) or Raman spectroscopy.
PY - 2011
DO - https://doi.org/10.1021/ac200181g
SN - 0003-2700
SN - 1520-6882
VL - 83
IS - 10
SP - 3744
EP - 3749
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-23669
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, Moritz-Caspar
A1 - Sarfraz, Adnan
A1 - Müller, Urs
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - Erste Sekunden im Leben eines Bauwerks - In-situ-Synchrotron-Röntgenbeugungsuntersuchungen der Zementhydratation mit Millisekunden-Auflösung
JF - Angewandte Chemie
N2 - Höchst dynamische Hydratationsprozesse in den ersten Sekunden bei der Entstehung eines Bauwerkes lassen sich mithilfe von Synchrotron-Röntgenbeugung mit einer sehr hohen Zeitauflösung nachverfolgen. Der Schwerpunkt lag dabei auf der Beeinflussung der Bildung erster kristalliner Hydratationsprodukte während des Frühstadiums der Zementhydratation.
KW - SyXRD
KW - High resolution
KW - In-situ
KW - Colloidal suspension
KW - Cement hydration
KW - In-situ-Analyse
KW - Kolloidale Suspensionen
KW - Röntgenbeugung
KW - Zementhydratation
PY - 2012
DO - https://doi.org/10.1002/ange.201200993
SN - 0044-8249
SN - 0932-2140
SN - 1521-3757
VL - 124
IS - 20
SP - 5078
EP - 5081
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-26284
LA - deu
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, Moritz-Caspar
A1 - Sarfraz, Adnan
A1 - Müller, Urs
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - First seconds in a building's life - In situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale
JF - Angewandte Chemie / International Edition
N2 - Setting cement: Highly dynamic hydration processes that occur during the first seconds of cement hydration were studied by time-resolved synchrotron X-ray diffraction. Polycarboxylate ether additives were found to influence the formation of the initial crystalline hydration products on a molecular level.
KW - Cement hydration
KW - Colloidal suspensions
KW - In situ analysis
KW - X-ray diffraction
KW - SyXRD
KW - High resolution
KW - In-situ
PY - 2012
DO - https://doi.org/10.1002/anie.201200993
SN - 1433-7851
SN - 1521-3773
SN - 0570-0833
VL - 51
IS - 20
SP - 4993
EP - 4996
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-26287
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlegel, Moritz-Caspar
A1 - Wenzel, Klaus-Jürgen
A1 - Sarfraz, Adnan
A1 - Panne, Ulrich
A1 - Emmerling, Franziska
T1 - A wall-free climate unit for acoustic levitators
JF - Review of scientific instruments
N2 - Acoustic levitation represents the physical background of trapping a sample in a standing acoustic wave with no contact to the wave generating device. For the last three decades, sample holders based on this effect have been commonly used for contact free handling of samples coupled with a number of analytical techniques. In this study, a wall-free climate unit is presented, which allows the control of the environmental conditions of suspended samples. The insulation is based on a continuous cold/hot gas flow around the sample and thus does not require any additional isolation material. This provides a direct access to the levitated sample and circumvents any influence of the climate unit material to the running analyses.
KW - Acoustic levition
PY - 2012
DO - https://doi.org/10.1063/1.4705968
SN - 0034-6748
SN - 1089-7623
VL - 83
IS - 5
SP - 055101-1 - 055101-3
PB - American Institute of Physics
CY - Melville, NY
AN - OPUS4-25881
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlögl, Johanna
A1 - Goldammer, Ole
A1 - Bader, Julia
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Introducing AFS ([Al(SO3F)3]x) – a thermally stable, readily available, and catalytically active solid Lewis superacid
JF - Chemical Science
N2 - This paper introduces the thermally stable, solid Lewis superacid aluminium tris(fluorosulfate) (AFS), that is easy-to-synthesize from commercially available starting materials. Its applicability, e.g. in catalytic C–F bond activations, is shown.
KW - Lewis Acid
KW - C-F activation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601001
DO - https://doi.org/10.1039/D4SC01753F
SN - 2041-6520
SP - 1
EP - 7
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60100
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Scholz, G.
A1 - Emmerling, Franziska
A1 - Dreger, M.
A1 - Kemnitz, E.
T1 - Mechanochemical synthesis and characterization of hydrated and dehydrated crystalline strontium terephtalates
JF - Zeitschrift für anorganische und allgemeine Chemie = Journal of inorganic and general chemistry
N2 - A successful mechanochemical synthesis of strontium terephthalate trihydrate is described for the first time. The dehydration of Sr(C8H4O4)·3H2O occurs at about 100 °C and results in a well-defined strontium terephtalate, Sr(C8H4O4), thermally stable up to 550 °C. Both compounds are not described so far in the literature. Their structures were solved by ab initio structure determination and subsequent Rietveld refinement of the powder diffraction data. Further methods like DTA-TG, MAS NMR and FT-IR spectroscopy, and BET measurements were used to characterize these compounds.
KW - Mechanochemical synthesis
KW - Ab initio structure determination
KW - MAS NMR spectroscopy
KW - Strontium
PY - 2013
DO - https://doi.org/10.1002/zaac.201200550
SN - 0044-2313
SN - 1521-3749
SN - 0372-7874
SN - 0863-1786
SN - 0863-1778
VL - 639
IS - 5
SP - 689
EP - 693
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-29117
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schulz, K.
A1 - Schmack, R.
A1 - Klemm, H. W.
A1 - Kabelitz, Anke
A1 - Schmidt, T.
A1 - Emmerling, Franziska
A1 - Kraehnert, R.
T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure
JF - Chemistry of Materials
N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content.
KW - Iron oxide
KW - Crystallization
KW - Mesoporous films
KW - Nanostructure
PY - 2017
DO - https://doi.org/10.1021/acs.chemmater.6b05185
SN - 0897-4756
SN - 1520-5002
VL - 29
IS - 4
SP - 1724
EP - 1734
AN - OPUS4-39690
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Seidel, R.
A1 - Kraffert, K.
A1 - Kabelitz, Anke
A1 - Pohl, M.N.
A1 - Kraehnert, R.
A1 - Emmerling, Franziska
A1 - Winter, B.
T1 - Detection of the electronic structure of iron-(III)-oxo oligomers forming in aqueous solutions
JF - Physical Chemistry Chemical Physics
N2 - The nature of the small iron-oxo oligomers in iron-(III) aqueous solutions has a determining effect on the chemical processes that govern the formation of nanoparticles in aqueous phase. Here we report on a liquid-Jet photoelectron-spectroscopy experiment for the investigation of the electronic structure of the occurring iron-oxo oligomers in FeCl3 aqueous solutions. The only iron species in the as-prepared 0.75 M solution are Fe3+ monomers. Addition of NaOH initiates Fe3+ hydrolysis which is followed by the formation of iron-oxo oligomers. At small enough NaOH concentrations, corresponding to approximately [OH]/[Fe] = 0.2–0.25 ratio, the iron oligomers can be stabilized for several hours without engaging in further aggregation. Here, we apply a combination of non-resonant as well as iron 2p and Oxygen 1s resonant photoelectron spectroscopy from a liquid microjet to detect the electronic structure of the occurring species. Specifically, the oxygen 1s partial electron yield X-ray absorption (PEY-XA) spectra are found to exhibit a peak well below the onset of liquid water and OH (aq) absorption. The iron 2p absorption gives rise to signal centered between the main absorption bands typical for aqueous Fe3+. Absorption bands in both PEY-XA spectra are found to correlate with an enhanced photoelectron Peak near 20 eV binding energy, which demonstrates the sensitivity of resonant photoelectron (RPE) spectroscopy to mixing between iron and ligand orbitals. These various signals from the iron-oxo oligomers exhibit Maximum intensity at [OH]/[Fe] = 0.25 ratio. For the same ratio, we observe changes in the pH as well as in complementary Raman spectra, which can be assigned to the Transition from monomeric to oligomeric species. At approximately [OH]/[Fe] = 0.3 we begin to observe particles larger than 1 nm in radius, detected by small-angle X-ray scattering.
KW - Iron-oxo oligomers
KW - XPS
KW - Electronic structure
PY - 2017
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-433468
DO - https://doi.org/10.1039/c7cp06945f
SN - 1463-9076
SN - 1463-9084
VL - 19
IS - 48
SP - 32226
EP - 32234
AN - OPUS4-43346
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Siegel, David
A1 - Blaske, Franziska
A1 - Koch, Matthias
A1 - Emmerling, Franziska
A1 - Nehls, Irene
T1 - Deacetyl tenuazonic acid p-toluenesulfonylhydrazone
JF - Acta crystallographica E
KW - Deacetyl tenuazonic acid
KW - Toluenesulfonylhydrazine
KW - Hydrazone
KW - Crystal structure
PY - 2009
DO - https://doi.org/10.1107/S1600536809048958
SN - 1600-5368
VL - E65
IS - 12
SP - o3136 Sup-1 - o3136 Sup-8
PB - Munksgaard
CY - Copenhagen
AN - OPUS4-20608
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Siegel, David
A1 - Koch, Matthias
A1 - Emmerling, Franziska
A1 - Nehls, Irene
T1 - Deacetyl tenuazonic acid
JF - Acta crystallographica E
KW - Deacetyl tenuazonic acid
KW - X-ray single crystal diffraction
KW - Crystal structure
PY - 2009
DO - https://doi.org/10.1107/S1600536809015372
SN - 1600-5368
VL - 65
IS - 6
SP - o1201
PB - Munksgaard
CY - Copenhagen
AN - OPUS4-19429
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Siegel, David
A1 - Merkel, Stefan
A1 - Koch, Matthias
A1 - Emmerling, Franziska
A1 - Nehls, Irene
T1 - 3-{1-[(2,4-Dinitrophenyl)hydrazino]ethylidene}-5-(1-methylpropyl)pyrrolidine-2,4-dione
JF - Acta crystallographica E
KW - Tenuazonic acid 2,4-dinitrophenylhydrazone
KW - X-ray single crystal diffraction
KW - Crystal structure
PY - 2009
DO - https://doi.org/10.1107/S1600536809012458
SN - 1600-5368
VL - 65
IS - 5
SP - o988
EP - o989
PB - Munksgaard
CY - Copenhagen
AN - OPUS4-19736
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Siegel, David
A1 - Troyanov, S.
A1 - Noack, J.
A1 - Emmerling, Franziska
A1 - Nehls, Irene
T1 - Alternariol
JF - Acta crystallographica E
N2 - In the title compound (systematic name: 3,7,9-trihydroxy-1-methyl-6H-benzo[c]chromen-6-one), C14H10O5, the methyl group is shifted out of the molecular plane due to a steric collision, thus causing a slight twist of the benzene rings. The molecular structure is stabilized by an intramolecular O-H...O hydrogen bond, generating an S(6) ring. In the crystal, molecules are connected by intermolecular O-H...O hydrogen bonds into a three-dimensional network.
KW - Alternariol
KW - Kristallstruktur
PY - 2010
DO - https://doi.org/10.1107/S1600536810017502
SN - 1600-5368
VL - 66
IS - 6
SP - o1366
PB - Munksgaard
CY - Copenhagen
AN - OPUS4-21400
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Simo, A.
A1 - Polte, Jörg
A1 - Pfänder, N.
A1 - Vainio, U.
A1 - Emmerling, Franziska
A1 - Rademann, K.
T1 - Formation mechanism of silver nanoparticles stabilized in glassy matrices
JF - Journal of the American chemical society
N2 - In any given matrix control over the final particle size distribution requires a constitutive understanding of the mechanisms and kinetics of the particle evolution. In this contribution we report on the formation mechanism of silver nanoparticles embedded in a soda-lime silicate glass matrix. For the silver ion-exchanged glass it is shown that at temperatures below 410 °C only molecular clusters (diameter <1 nm) are forming which are most likely silver dimers. These clusters grow to nanoparticles (diameter >1 nm) by annealing above this threshold temperature of 410 °C. It is evidenced that the growth and thus the final silver nanoparticle size are determined by matrix-assisted reduction mechanisms. As a consequence, particle growth proceeds after the initial formation of stable clusters by addition of silver monomers which diffuse from the glass matrix. This is in contrast to the widely accepted concept of particle growth in metal–glass systems, in which it is assumed that the nanoparticle formation is predominantly governed by Ostwald ripening processes.
PY - 2012
DO - https://doi.org/10.1021/ja309034n
SN - 0002-7863
SN - 1520-5126
VL - 134
IS - 45
SP - 18824
EP - 18833
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-27539
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Simoes, R.
A1 - Bernades, C.
A1 - Joseph, A.
A1 - Piedade, F.
A1 - Kraus, Werner
A1 - Emmerling, Franziska
A1 - Diogo, H.
A1 - da Piedade, M.
T1 - Polymorphism in simvastatin: Twinning, disorder, and enantiotropic phase transitions
JF - Molecular pharmaceutics
N2 - : Simvastatin is one of the most widely used active pharmaceutical ingredients for the treatment of hyperlipidemias. Because the compound is employed as a solid in drug formulations, particular attention should be given to the characterization of different polymorphs, their stability domains, and the nature of the phase transitions that relate them. In this work, the phase transitions delimiting the stability domains of three previously reported simvastatin forms were investigated from structural, energetics, and dynamical points of view based on single crystal X-ray diffraction (SCXRD), hot stage microscopy (HSM), and differential scanning calorimetry (DSC) experiments (conventional scans and heat capacity measurements), complemented with molecular dynamics (MD) simulations. Previous assignments of the crystal forms were confirmed by SCXRD: forms I and II were found to be orthorhombic (P212121, Z′/Z = 1/4) and form III was monoclinic (P21, Z′/Z = 2/4). The obtained results further indicated that (i) the transitions between different forms are observed at 235.9 ± 0.1 K (form III → form II) and at 275.2 ± 0.2 K (form II → form I) in DSC runs carried out at 10 K min−1 and close to these values when other types of techniques are used (e.g., HSM). (ii) They are enantiotropic (i.e., there is a transition temperature relating the two phases before fusion at which the stability order is reversed), fast, reversible, with very little hysteresis between heating and cooling modes, and occur under single crystal to single crystal conditions. (iii) A nucleation and growth mechanism seems to be followed since HSM experiments on single crystals evidenced the propagation of an interface, accompanied by a change of birefringence and crystal contraction or expansion (more subtle in the case of form III → form II), when the phase transitions are triggered. (iv) Consistent with the reversible and small hysteresis nature of the phase transitions, the SCXRD results indicated that the molecular packing is very similar in all forms and the main structural differences are associated with conformational changes of the “ester tail”. (v) The MD simulations further suggested that the tail is essentially “frozen” in two conformations below the III → II transition temperature, becomes progressively less hindered throughout the stability domain of form II, and acquires a large conformational freedom above the II → I transition. Finally, the fact that these transitions were found to be fast and reversible suggests that polymorphism is unlikely to be a problem for pharmaceutical formulations employing crystalline simvastatin because, if present, the III and II forms will readily convert to form I at ambient temperature.
KW - Polymorphism
KW - Twinning
KW - Disorder
KW - Simvastatine
PY - 2018
DO - https://doi.org/10.1021/acs.molpharmaceut.8b00818
SN - 1543-8384
SN - 1543-8392
VL - 15
IS - 11
SP - 5349
EP - 5360
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-46927
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Simões, R. G.
A1 - Melo, P. L. T.
A1 - Bernardes, C. E. S.
A1 - Heilmann, Maria
A1 - Emmerling, Franziska
A1 - Minas da Piedade, M. E.
T1 - Linking Aggregation in Solution, Solvation, and Solubility of Simvastatin: An Experimental and MD Simulation Study
JF - Crystal Growth & Design
N2 - The solubility is generally thought to be higher if the solvent effectively solvates solute molecules that are well-separated from each other. The present work suggests, however, that the formation of large solute aggregates does not necessarily imply less effective solvation and lower solubility. Measurements of the solubility of simvastatin (one of the most commonly prescribed antihyperlipidemic drugs) in three solvents with different polarities and protic characters, led to the solubility order acetone > ethyl acetate > ethanol, in the full temperature range covered by the experiments (283–308 K). An analysis of the structures of the different solutions on the basis of molecular dynamics simulation results indicated that this trend seems to be determined by a balance between the solute tendency toward aggregation and the ability of the solvent to efficiently solvate it, by integrating the cluster structures, regardless of their size, and effectively establishing solvent–solute interactions.
KW - Simvastatin
KW - Solubility
KW - API
KW - Aggregation
PY - 2021
DO - https://doi.org/10.1021/acs.cgd.0c01325
VL - 21
IS - 1
SP - 544
EP - 551
AN - OPUS4-52185
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sobina, E.
A1 - Zimathies, Annett
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - de Santis Neves, R.
A1 - Wang, H.
A1 - Mizuno, K.
A1 - Devoille, L.
A1 - Steel, E.
A1 - Ceyhan, A.
A1 - Sadak, E.
ED - Sobina, E.
T1 - Final report of CCQM-K153 Measurement of Specific Adsorption A [mol/kg] of N-2 and Kr on nonporous SiO2 at LN temperature (to enable a traceable determination of the Specific Surface Area (BET) following ISO 9277)
JF - Metrologia
N2 - CCQM key comparison K-153 Measurement of Specific Adsorption A [mol/kg] of N-2 and Kr on nonporous SiO2 at LN temperature (to enable a traceable determination of the Specific Surface Area (BET) following ISO 9277) has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of specific adsorption, BET specific surface area) of nonporous substances (sorbents, ceramics, catalytic agents, etc) used in advanced technology.
In this key comparison, a commercial nonporous silicon dioxide was supplied as a sample. Eight NMIs participated in this key comparison, but only five NMI's have reported in time. All participants used a gas adsorption method, here nitrogen and (or) krypton adsorption at 77.3 K, for analysis according to the international standards ISO 15901-2 and 9277.
In this key comparison, the degrees of equivalence uncertainties for specific adsorption nitrogen and krypton, BET specific surface area were established.
KW - Nonporous SiO2
KW - Specific Adsorption of N-2 and Kr
KW - BET specific surface area
PY - 2019
DO - https://doi.org/10.1088/0026-1394/56/1A/08013
VL - 56
IS - 1A
SP - 08013
PB - IOP publishing Ltd
CY - Bristol, UK
AN - OPUS4-50358
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sobina, E.
A1 - Zimathis, Anett
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - de Santis Neves, R.
A1 - Galhardo, C. E.
A1 - De Robertis, E.
A1 - WANG, H.
A1 - Mizuno, K.
A1 - Kurokawa, A.
A1 - Unger, Wolfgang
T1 - Final report of CCQM-K136 measurement of porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3
JF - Metrologia
N2 - The CCQM-K136 key comparison for determination of the porosity properties of aluminum oxide has been organized jointly by the surface and micro/nano analysis working groups of CCQM to test the abilities of the metrology institutes to measure the porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3.
Ural Scientific Research Institute for Metrology (UNIIM) acted as the coordinating laboratory for this comparison with BAM Federal Institute for Materials Research and Testing (BAM) as co-coordinating laboratory. Five NMIs and one DI participated in this key comparison. All participants used a gas adsorption method, here nitrogen adsorption at 77.3 K, for analysis according to the international standards ISO 15901-2 and 9277.
KW - BET specific surface area
KW - Specific adsorption
KW - Pore diameter
KW - Specific pore volume
KW - Nanoporous Al2O3
PY - 2016
UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08014
DO - https://doi.org/10.1088/0026-1394/53/1A/08014
SN - 0026-1394
SN - 1681-7575
VL - 2016
IS - 53 Technical Supplement
SP - Article 08014, 1
EP - 39
PB - IOPscience
AN - OPUS4-38282
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Sobisch, T.
A1 - Emmerling, Franziska
A1 - Girod, Matthias
A1 - Menzel, Michael
A1 - Lerche, D.
T1 - Advantages of dual wavelength detection for size determination of nanoparticles with analytical centrifugation
JF - Dispersion Letters
KW - Particle size distributions
KW - Dual wavelength detection
KW - Analytical centrifugation
KW - Nanoparticle separation
PY - 2013
SN - 978-3-944261-28-7
SN - 978-3-944261-36-2
SN - 978-3-944261-52-2
VL - 4
SP - 9
EP - 11
AN - OPUS4-30802
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Som, T.
A1 - Simo, A.
A1 - Fenger, R.
A1 - Troppenz, G.V.
A1 - Bansen, R.
A1 - Pfänder, N.
A1 - Emmerling, Franziska
A1 - Rappich, J.
A1 - Boeck, T.
A1 - Rademann, K.
T1 - Bismuth hexagons: facile mass synthesis, stability and applications
JF - ChemPhysChem
N2 - A unique direct electrodeposition technique involving very high current densities, high voltages and high electrolyte concentrations is applied for highly selective mass synthesis of stable, isolable, surfactant-free, single-crystalline Bi hexagons on a Cu wire at room temperature. A formation mechanism of the hexagons is proposed. The morphology, phase purity, and crystallinity of the material are well characterized by FESEM, AFM, TEM, SAED, EDX, XRD, and Raman spectroscopy. The thermal stability of the material under intense electron beam and intense laser light irradiation is studied. The chemical stability of elemental Bi in nitric acid shows different dissolution rates for different morphologies. This effect enables a second way for the selective fabrication of Bi hexagons. Bi hexagons can be oxidized exclusively to α-Bi2O3 hexagons. The Bi hexagons are found to be promising for thermoelectric applications. They are also catalytically active, inducing the reduction of 4-nitrophenol to 4-aminophenol. This electrodeposition methodology has also been demonstrated to be applicable for synthesis of bismuth-based bimetallic hybrid composites for advanced applications.
KW - Bismuth
KW - Hexagons
KW - Dendrites
KW - Single-crystal
KW - Thermoelectric applications
KW - Catalytic applications
PY - 2012
DO - https://doi.org/10.1002/cphc.201101009
SN - 1439-4235
VL - 13
IS - 8
SP - 2162
EP - 2169
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-26278
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Som, Tirtha
A1 - Troppenz, G.V.
A1 - Wendt, R. R.
A1 - Wollgarten, M.
A1 - Rappich, J.
A1 - Emmerling, Franziska
A1 - Rademann, Klaus
T1 - Graphene oxide/alpha-Bi2O3 composites for visible-light photocatalysis, chemical catalysis, and solar energy conversion
JF - ChemSusChem
N2 - The growing challenges of environmental purification by solar photocatalysis, precious-metal-free catalysis, and photocurrent generation in photovoltaic cells receive the utmost global attention. Here we demonstrate a one-pot, green chemical synthesis of a new stable heterostructured, ecofriendly, multifunctional microcomposite that consists of α-Bi2O3 microneedles intercalated with anchored graphene oxide (GO) microsheets (1.0 wt?%) for the above-mentioned applications on a large economical scale. The bare α-Bi2O3 microneedles display two times better photocatalytic activities than commercial TiO2 (Degussa-P25), whereas the GO-hybridized composite exhibits approximately four to six times enhanced photocatalytic activities than the neat TiO2 photocatalyst in the degradation of colored aromatic organic dyes (crystal violet and rhodamine 6G) under visible-light irradiation (300 W tungsten lamp). The highly efficient activity is associated with the strong surface adsorption ability of GO for aromatic dye molecules, the high carrier acceptability, and the efficient electron–hole pair separation in Bi2O3 by individual adjoining GO sheets. The introduction of Ag nanoparticles (2.0 wt?%) further enhances the photocatalytic performance of the composite over eightfold because of a plasmon-induced electron-transfer process from Ag nanoparticles through the GO sheets into the conduction band of Bi2O3. The new composites are also catalytically active and catalyze the reduction of 4-nitrophenol to 4-aminophenol in the presence of borohydride ions. Photoanodes assembled from GO/α-Bi2O3 and Ag/GO/α-Bi2O3 composites display an improved photocurrent response (power conversion efficiency ~20?% higher) over those prepared without GO in dye-sensitized solar cells.
KW - Bismuth
KW - Dyes/pigments
KW - Environmental chemistry
KW - Graphene
KW - Photochemistry
PY - 2014
DO - https://doi.org/10.1002/cssc.201300990
SN - 1864-5631
SN - 1864-564X
VL - 7
IS - 3
SP - 854
EP - 865
PB - Wiley-VCH
CY - Weinheim
AN - OPUS4-30390
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Somasundaram, S. K.
A1 - Buzanich, Ana
A1 - Emmerling, Franziska
A1 - Krishnan, S.
A1 - Senthilkumar, K.
A1 - Joseyphus, R.J.
T1 - New insights into pertinent Fe-complexes for the synthesis of iron via the instant polyol process
JF - Physical Chemistry Chemical Physics
N2 - Chemically synthesized iron is in demand for biomedical applications due to its large saturation magnetization compared to iron oxides. The polyol process, suitable for obtaining Co and Ni particles and their alloys, is laborious in synthesizing Fe. The reaction yields iron oxides, and the reaction pathway remains unexplored. This study shows that a vicinal polyol, such as 1,2-propanediol, is suitable for obtaining Fe rather than 1,3-propanediol owing to the formation of a reducible Fe intermediate complex. X-ray absorption spectroscopy analysis reveals the ferric octahedral geometry and tetrahedral geometry in the ferrous state of the reaction intermediates in 1,2-propanediol and 1,3-propanediol, respectively. The final product obtained using a vicinal polyol is Fe with a γ-Fe2O3 shell, while the terminal polyol is favourable for Fe3O4. The distinct Fe–Fe and Fe–O bond lengths suggest the presence of a carboxylate group and a terminal alkoxide ligand in the intermediate of 1,2-propanediol. A large Fe–Fe bond distance suggests diiron complexes with bidentate carboxylate bridges. Prominent high-spin and low-spin states indicate the possibility of transition, which favors the reduction of iron ions in the reaction using 1,2-propanediol.
KW - XAS
KW - Nanoparticle
PY - 2023
DO - https://doi.org/10.1039/D3CP01969A
SN - 1463-9076
VL - 25
IS - 33
SP - 21970
EP - 21980
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58073
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Souza, B.
A1 - Chauque, S.
A1 - de Oliveira, P.
A1 - Emmerling, Franziska
A1 - Torresi, R.
T1 - Mechanochemical optimization of ZIF-8/Carbon/S8 composites for lithium-sulfur batteries positive electrodes
JF - Journal of Electroanalytical Chemistry
N2 - The application of lithium-sulfur (Li-S) batteries is still limited by their rapid capacity fading. The pulverization of the sulfur positive electrode after the lithiation and the consequence dissolution of long chain polysulfides in organic solvents lead to the shuttle effect. To address these issues, here we report the mechanochemical preparation of ZIF-8 (Zeolitic Imidazole Framework-8)-based composites as sulfur hosts for positive electrodes in Li-S batteries. We studied different methods for the incorporation of conductive carbon. Also, the replacement of Zn2+ metal centers by other bivalent metals (Cu2+, Co2+ and Ni2+), enabled the preparation of other ZIF-8-based materials. The positive electrode ZIF-8/C/S8 showed initial discharges of 772 mA h g−1 while the pristine one, ZIF-8/S8, displayed 502 mA h g−1. The enhanced performance of 54% for ZIF-8/C/S8 indicates that the direct mechanochemical synthesis of ZIF-8 with conductive carbon is beneficial at initials charge/discharge process in comparison to traditional slurry preparation (ZIF-8/S8). Also, the Li2S6 absorption tests shows 87% of discoloration with ZIF-8/C/S8, confirming the better polysulfides absorption.
KW - Lithium-sulfur battery
KW - Metal organic frameworks
KW - ZIF-8
KW - Mechanochemistry
PY - 2021
DO - https://doi.org/10.1016/j.jelechem.2021.115459
VL - 896
SP - 115459
PB - Elsevier B.V.
AN - OPUS4-53542
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Karafiludis, Stephanos
A1 - Pimentel, Carlos
A1 - Montes-Hernández, German
A1 - Kochovski, Zdravko
A1 - Bienert, Ralf
A1 - Weimann, Karin
A1 - Emmerling, Franziska
A1 - Scoppola, Ernesto
A1 - Van Driessche, Alexander E.S.
T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines
JF - Journal of Cleaner Production
N2 - Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
KW - Industrial and Manufacturing Engineering
KW - Strategy and Management
KW - General Environmental Science
KW - Renewable Energy, Sustainability and the Environment
KW - Building and Construction
KW - Calcium sulfate
KW - Gypsum
KW - Bassanite
KW - Scattering
KW - Raman
KW - In situ
KW - Synchrotron
KW - BESSY
KW - MySpot
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698
UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1
DO - https://doi.org/10.1016/j.jclepro.2024.141012
SN - 0959-6526
VL - 440
SP - 1
EP - 12
PB - Elsevier B.V.
AN - OPUS4-59469
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Smales, Glen Jacob
A1 - Scoppola, E.
A1 - Jha, D.
A1 - Morales, L. F. G.
A1 - Moya, A.
A1 - Wirth, R.
A1 - Pauw, Brian Richard
A1 - Emmerling, Franziska
A1 - Van Driessche, A. E. S.
T1 - Seeds of imperfection rule the mesocrystalline disorder in natural anhydrite single crystals
JF - Proceedings of the National Academy of Sciences of the United States of America (PNAS)
N2 - In recent years, we have come to appreciate the astounding intricacies associated with the formation of minerals from ions in aqueous solutions. In this context, a number of studies have revealed that the nucleation of calcium sulfate systems occurs nonclassically, involving the aggregation and reorganization of nanosized prenucleation species. In recent work, we have shown that this particle-mediated nucleation pathway is actually imprinted in the resultant micrometer-sized CaSO4 crystals. This property of CaSO4 minerals provides us with the unique opportunity to search for evidence of nonclassical nucleation pathways in geological environments.
In particular, we focused on large anhydrite Crystals extracted from the Naica Mine in Mexico. We were able to shed light on this mineral's growth history by mapping defects at different length scales. Based on this, we argue that the nanoscale misalignment of the structural subunits, observed in the initial calcium sulfate crystal seeds, propagates through different length scales both in morphological, as well as in strictly crystallographic aspects, eventually causing the formation of large mesostructured single crystals of anhydrite. Hence, the nonclassical nucleation mechanism introduces a “seed of imperfection,” which leads to a macroscopic “single” crystal whose fragments do not fit together at different length scales in a self-similar manner. Consequently, anisotropic voids of various sizes are formed with very welldefined walls/edges. However, at the same time, the material retains in part its single crystal nature.
KW - Calcium sulfate
KW - Anhydrite
KW - Mesocrystal
KW - Nucleation
KW - Naica
PY - 2021
DO - https://doi.org/10.1073/pnas.2111213118
SN - 0027-8424
VL - 118
IS - 48
SP - 1
EP - 11
PB - National Academy of Sciences (USA)
CY - Washington
AN - OPUS4-53820
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stephan, H.
A1 - Kubeil, M.
A1 - Emmerling, Franziska
A1 - Müller, C.E.
T1 - Polyoxometalates as versatile enzyme inhibitors
JF - European journal of inorganic chemistry
N2 - Polyoxometalates (POMs) are inorganic cluster compounds that have been shown to possess a number of pharmacological properties, including antidiabetic, antibacterial, antiprotozoal, antiviral and anticancer activities. Their molecular mechanism of action is largely unknown. However, several studies indicate that many of their activities may be due to the inhibition of enzymes, in particular, of those enzymes that are accessible from the extracellular space and do not require the penetration of cell membranes. In this review, we describe the recent progress in the preparation and optimization of POMs, and an evaluation of their use as inhibitors of different families of enzymes. The next important steps in this area of research will be to gain a better understanding of the interactions of POMs with enzymes on a structural level through an X-ray crystallographic study of enzyme–POM complexes and the analysis of structure–activity relationships. Furthermore, POMs with increased stability and in vivo half-lives have to be prepared. Surface modification may allow the targeting of POM drugs at their sites of action.
KW - Cluster compounds
KW - Polyoxometalates
KW - Metalloprotein mimics
KW - Enzymes
KW - Inhibitors
KW - Bioinorganic chemistry
PY - 2013
DO - https://doi.org/10.1002/ejic.201201224
SN - 1434-1948
SN - 1099-0682
VL - 2013
IS - 10-11
SP - 1585
EP - 1594
PB - Wiley-VCH Verl.
CY - Weinheim
AN - OPUS4-28076
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Ali, Naveed Zafar
A1 - Maierhofer, Christiane
A1 - Emmerling, Franziska
T1 - Ettringite via Mechanochemistry: A Green and Rapid Approach for Industrial Application
JF - ACS Omega
N2 - Here, we report on a first mechanochemical synthesis of ettringite, an important cement hydrate phase. The mineral compound ettringite ([Ca3Al(OH)6]2·(SO4)3·26H2O) occurs rarely in nature, but is common for cement-based materials. Ettringite has wide technical application in the ceramic and paper industry. However, its typical wet-chemical synthesis is cumbersome and produces waste water and CO2 emissions. Here, we investigate the first mechanochemical synthesis of ettringite for developing an easy and sustainable alternative for industrial application. The mechanosynthesis was monitored in situ by coupled synchrotron X-ray diffraction (XRD) and infrared thermography (IRT). The consumption of the reactants and the formation of the reaction product were monitored with time-resolved XRD. IRT showed the temperature increase based on the exothermic reaction. The reaction conversion was significantly improved changing the strategy of the mechanosynthesis from a one- to a two-step process. The latter included neat pregrinding of solid reactants followed by a delayed addition of the stoichiometric amount of water. Thus, an increase of reaction conversion from 34 to 94% of ettringite could be achieved.
KW - XRD
KW - Mechanochemistry
KW - Ettringite
KW - In situ
PY - 2019
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479016
DO - https://doi.org/10.1021/acsomega.9b00560
SN - 2470-1343
VL - 4
IS - 4
SP - 7734
EP - 7737
PB - ACS Publications
CY - Washington, DC
AN - OPUS4-47901
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Feiler, Torvid
A1 - Ali, N. Z.
A1 - Minas da Piedade, M. E.
A1 - Emmerling, Franziska
T1 - Mechanistic Insights into a Sustainable Mechanochemical Synthesis of Ettringite
JF - ChemistryOpen
N2 - Mechanochemistry offers an environmentally benign and facile synthesis method for a variety of cement paste constituents. In addition, these methods can be used to selectively tune the properties of cement components. The mineral ettringite is an important component of cementitious materials and has additional technological potential due to its ion exchange properties.
Synthesis of ettringite via mechanochemistry is an environmentally friendly alternative to conventional wet-chemical synthesis established in industry. This contribution explores the mechanism of a two-step mechanochemical synthesis of ettringite, which was previously found to greatly improve the reaction conversion as compared with one-pot synthesis. The crystallinity of Al(OH)3 was found to decrease during the first stage of this mechanochemical synthesis. This was correlated to a significant decrease in the particle size of Al(OH)3 in this stage. No other significant changes were found for the other components, suggesting that mechanochemical activation of Al(OH)3 is responsible for the enhanced formation of ettringite by the two-step approach. The environmentally friendly approach developed for ettringite synthesis offers a versatile synthetic strategy, which can be applied to synthesise further cementitious materials.
KW - Ettringite
KW - Mechanochemistry
KW - Sustainability
KW - X-ray diffraction
PY - 2019
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489172
DO - https://doi.org/10.1002/open.201900215
VL - 8
IS - 7
SP - 1012
EP - 1019
PB - ChemPubSoc
AN - OPUS4-48917
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Meng, Birgit
A1 - Emmerling, Franziska
T1 - Monitoring of sulphate attack on hardened cement paste studied by synchrotron XRD
JF - Solid state sciences
N2 - The complex matter of external sulphate attack on cement-based construction materials is still not completely understood. The concentration of sulphate is a crucial factor for the formation of secondary phases and phase transitions of cement hydrates due to sulphate ingress into the microstructure. The sulphate attack on building materials for high and low sulphate concentrations was monitored by laboratory experiments. Hardened cement paste consisting of ordinary Portland cement (CEM I) were exposed to aqueous solutions of sodium sulphate for 18 months. Three sample compositions were used for this research, including different supplementary cementitious materials (SCM). The phase composition was determined for different time spans by high resolution synchrotron X-ray diffraction. Cross sections of exposed cement prisms were investigated as a representation of the microstructural profile. Based on the data, a temporal and spatial determination of the stages of the sulphate attack and the deterioration course was possible. Cement matrices blended with slag showed the highest resistance against sulphate attack.
KW - Cement paste
KW - Sulphate attack
KW - Mineral additions
KW - Concentration
KW - Monitoring
PY - 2015
DO - https://doi.org/10.1016/j.solidstatesciences.2015.08.006
SN - 1293-2558
SN - 1873-3085
VL - 48
SP - 278
EP - 285
PB - Elsevier Masson SAS
CY - Amsterdam
AN - OPUS4-34281
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Meng, Birgit
A1 - Emmerling, Franziska
T1 - Deterioration of hardened cement paste under combined sulphatechloride attack investigated by synchrotron XRD
JF - Solid State Sciences
N2 - The exact mechanisms of the phase transitions caused by a combined sulphate-chloride attack are discussed controversially. The main points concern the mutual influences of sulphate and chloride ions during the secondary binding processes of these anions within cement hydrate phases. We simulated combined sulphate-chloride attack under laboratory conditions using solutions containing NaCl and Na2SO4 in different concentrations. Three sample compositions were used for the preparation of the specimens. In two of them, 30% of Portland cement was replaced by supplementary cementitious materials (fly ash, slag). The phase distribution in the samples was determined using synchrotron X-ray diffraction. The analysis with high spatial resolution allows the localisation of the secondary phase formation in the microstructural profile of the sample. A mechanism of the phase developments under combined sulphate-chloride attack is derived.
KW - Cement paste
KW - Sulphate-chloride attack
KW - Portland cement
KW - Mineral additions
PY - 2016
DO - https://doi.org/10.1016/j.solidstatesciences.2016.04.002
IS - 56
SP - 29
EP - 44
PB - Elsevier Masson SAS
CY - Issy les Moulineaux cedex; France
AN - OPUS4-35936
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Schlegel, Moritz-Caspar
A1 - Irassar, E.F.
A1 - Meng, Birgit
A1 - Emmerling, Franziska
T1 - Applying high resolution SyXRD analysis on sulfate attacked concrete field samples
JF - Cement and concrete research
N2 - High resolution synchrotron X-ray diffraction (SyXRD) was applied for a microstructural profile analysis of concrete deterioration after sulfate attack. The cement matrices consist of ordinary Portland cement and different amounts of supplementary cementitious materials, such as fly ash, natural pozzolana and granulated blast furnace slag. The changes of the phase composition were determined along the direction of sulfate ingress. This approach allows the identification of reaction fronts and zones of different phase compositions and conclusions about the mechanisms of sulfate attack. Two reaction fronts were localized in the initial 4 mm from the sample surface. The mechanism of deterioration caused by the exposition in the sulfate-bearing soil is discussed. SyXRD is shown to be a reliable method for investigation of cementitious materials with aggregates embedded in natural environments.
KW - X-ray diffraction (B)
KW - High resolution
KW - Degradation (C)
KW - Sulfate attack (C)
KW - Concrete (E)
PY - 2014
DO - https://doi.org/10.1016/j.cemconres.2014.07.015
SN - 0008-8846
SN - 1873-3948
VL - 66
SP - 19
EP - 26
PB - Pergamon Press
CY - New York, NY
AN - OPUS4-31253
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stroh, Julia
A1 - Schlegel, Moritz-Caspar
A1 - Schmidt, Wolfram
A1 - Nguyen, Thi Yen
A1 - Meng, Birgit
A1 - Emmerling, Franziska
T1 - Time-resolved in situ investigation of Portland cement hydration influenced by chemical admixtures
JF - Construction and Building Materials
N2 - Numerous admixtures are used in the building practice to customize the properties of the cement paste during application. The influences of admixtures on the course of cement hydration and formation of hydrate phases have to be considered. Polycarboxylate ether (PCE) based polymeric superplasticizers (SPs) are known to retard the setting of the cement paste. The extent of the retardation differs depending on the molecular structure of the SP. Additionally, the presence of a stabilizing agent (SA) in the cement paste has a retarding side effect on the setting. The initial cement hydration processes and the detailed mechanisms of the retardation influenced by PCEs, as well as their interactions with particular SAs, are insufficiently understood. Up to now, only the results of phenomenological studies were taken into account to describe this retardation process. A detailed structure analysis monitoring the change of the phase composition during the hydration was never applied. Both SP and SA affect the adsorption of the sulphate ions on the clinker particles, causing changes in the formation of ettringite during the initial hydration, and are therefore a crucial part of the setting process itself. Here, the initial hydration of cement influenced by the interaction of SP and SA was monitored in situ by synchrotron X-ray diffraction. The high time resolution of the measurements allowed a continuous detection of the hydrates formed. The hydration was followed from the starting point of water addition and for couple of hours afterwards. The hydration of the levitated cement pellets containing starch as SA was initialized by adding aqueous solutions of different commercial SPs. Changes in the ettringite formation were detected in comparison to the reference hydration of pure cement.
KW - Synchrotron
KW - Portland cement Initial hydration
KW - Superplasticizer
KW - Stabilizer
KW - XRD
PY - 2016
DO - https://doi.org/http://dx.doi.org/10.1016/j.conbuildmat.2015.12.097
IS - 106
SP - 18
EP - 26
PB - Elsevier
AN - OPUS4-35467
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stößer, R.
A1 - Feist, M.
A1 - Patzwaldt, K.
A1 - Menzel, Michael
A1 - Emmerling, Franziska
ED - Brooks, H.
T1 - Redox reactions of K3[Fe(CN)6] during mechanochemically stimulated phase transitions of AlOOH
JF - Journal of physics and chemistry of solids
N2 - Thermally induced redox reactions of K3[Fe(CN)6] (1) were investigated for a broad temperature range by thermal methods and structure analytical methods (ESR and Mößbauer spectroscopy, X-ray Powder diffraction and XANES). Based on the influence of the mechanically activated and transforming matrices 2 and 3, redox processes can be tuned to form doped Al2O3 systems which contain either isolated Fe3+ centres or redox active phases and precursors like (Al1-xFex)2O3 (4), (Al3-xFex)O4 (5), Fe3O4, Fe2O3 and Fe0. The phase Fe3C and the chemically reactive C-species were detected during the reaction of 1. The final composition of the doped products of α-Al2O3 is mainly influenced by the chemical nature of the Fe doping component, the applied temperature and time regime, and the composition of the gas phase (N2, N2/O2 or N2/H2). From the solid state chemistry point of view it is interesting that the transforming matrix (2 and 3) possesses both oxidative and protective properties and that the incorporation of the Fe species can be performed systematically.
KW - A. Inorganic compounds
KW - C. Mössbauer spectroscopy
KW - C. Thermogravimetric analysis
KW - D. Electron paramagnetic resonance
KW - ESR-Spektroskopie
KW - Kaliumhexacyanoferrat(III)
KW - Mechanische Aktivierung
KW - Mößbauer-Spektroskopie
KW - Redoxreaktionen
KW - TA-MS-Messungen
PY - 2011
DO - https://doi.org/10.1016/j.jpcs.2011.03.016
SN - 0022-3697
VL - 72
IS - 6
SP - 794
EP - 799
PB - Pergamon Press
CY - New York, NY
AN - OPUS4-23685
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stößer, R.
A1 - Feist, M.
A1 - Willgeroth, Carola
A1 - Emmerling, Franziska
A1 - Menzel, Michael
A1 - Reuther, H.
T1 - The 'quiet Goldschmidt' - a mechanochemical, thermoanalytical, and spectroscopic study of selected steps of the aluminothermic reaction
JF - Journal of solid state chemistry
N2 - The Goldschmidt reaction (2Al+α-Fe2O3) was investigated both under mechanical and thermal activation by employing a combination of analytical methods such as ESR and Mössbauer spectroscopy, magnetic susceptibility, X-ray powder diffraction, and thermal analysis (TA). Both the mechanical treatment and the TA runs under air caused the reaction conditions of 'quiet redox reactions' due to a retarding effect and enabled a reaction study in a 'slow motion mode'. This allowed to establish distinct partial steps of the integral reaction process depending on the intensity of the mechanical impact, the educt composition, the gas phase composition, and, finally, the thermal excitation in the TA runs. Particular attention was payed to the role of the gas phase and to the reaction of aluminum with differently activated oxygen species. The phlegmatizing effect was traced back to the formation of Al2O3 coverages of the Al particles.
KW - Thermite reaction
KW - Iron ESR and Mössbauer spectroscopy
KW - Mechanochemical activation
KW - Magnetic moments
KW - DTA-TG
KW - XRD
PY - 2013
DO - https://doi.org/10.1016/j.jssc.2013.02.032
SN - 0022-4596
SN - 1095-726X
VL - 202
SP - 173
EP - 190
PB - Elsevier
CY - San Diego, Calif.
AN - OPUS4-29528
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Surov, A.
A1 - Vasilev, N.
A1 - Voronin, A.
A1 - Churakov, A.
A1 - Emmerling, Franziska
A1 - Perlovich, G.
T1 - Ciprofloxacin salts with benzoic acid derivatives: structural aspects, solid-state properties and solubility performance
JF - Crystengcomm
N2 - n this work, three new pharmaceutical hydrated salts of ciprofloxacin with selected derivatives of benzoic acid, namely 4-hydroxybenzoic acid, 4-aminobenzoic acid and gallic acid, were obtained and systematically investigated by several solid-state analytical techniques. In situ Raman spectroscopy was applied to elucidate the alternative pathways of the solid forms' formation under mechanochemical conditions. Crystal structure analysis and a CSD survey allowed us to establish a distinct supramolecular motif formed by infinite columnar stacks of ciprofloxacin dimers arranged in the “head-to-tail” manner. An alternative “head-to-head” packing arrangement was only observed in the crystal of the hydrated ciprofloxacin salt with 4-aminobenzoic acid. In addition, the pH-solubility behavior of the solid forms was thoroughly investigated. Furthermore, a distinct structure–property relationship between the specific features of the supramolecular organization of the hydrated salts and their solubility was observed and discussed.
KW - Mechanochemistry
KW - XRD
PY - 2020
DO - https://doi.org/10.1039/D0CE00514B
VL - 22
IS - 25
SP - 4238
EP - 4249
AN - OPUS4-51818
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Surov, Artem O.
A1 - Vasilev, Nikita A.
A1 - Churakov, Andrei V.
A1 - Stroh, Julia
A1 - Emmerling, Franziska
A1 - Perlovich, German L.
T1 - Solid Forms of Ciprofloxacin Salicylate: Polymorphism, Formation Pathways, and Thermodynamic Stability
JF - Crystal Growth & Design
N2 - The crystallization of ciprofloxacin - an antibacterial fluoroquinolone compound - with salicylic acid resulted in the isolation of five distinct solid forms of the drug, namely, an anhydrous salt, two polymorphic forms of the salt monohydrate, methanol and acetonitrile solvates, and the salt-cocrystal hydrate. The salicylate salts were investigated by different analytical techniques ranging from powder and single crystal X-ray diffractometry, differential scanning calorimetry, thermogravimetric analysis, variable temperature powder X-ray diffraction, dynamic vapor sorption analysis, dissolution, and solubility investigations. Real-time in situ Raman spectroscopy was used to investigate the mechanochemical formation pathways of the different solid polymorphs of ciprofloxacin salicylate. The mechanism of the phase transformation between the crystalline forms was evaluated under mechanochemical conditions. It was found that the formation pathway and kinetics of the grinding process depend on the form of the starting material and reaction conditions. The analysis of the solid-state thermal evolution of the hydrated salts revealed the two-step mechanism of dehydration process, which proceeds through a formation of the distinct intermediate crystalline products.
KW - Cocrystal
KW - Polymorphism
KW - Ciprofloxacin
KW - XRD
KW - DSC
PY - 2019
DO - https://doi.org/10.1021/acs.cgd.9b00185
SN - 1528-7483
VL - 19
IS - 5
SP - 2979
EP - 2990
PB - American Chemical Society
AN - OPUS4-47903
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Takao, S.
A1 - Takao, K.
A1 - Kraus, Werner
A1 - Emmerling, Franziska
A1 - Scheinost, A.C.
A1 - Bernhard, G.
A1 - Hennig, C.
T1 - First hexanuclear U IV and Th IV formate complexes - Structure and stability range in aqueous solution
JF - European journal of inorganic chemistry
KW - Actinides
KW - Polynuclear species
KW - Formic acid
KW - Bridging ligands
PY - 2009
DO - https://doi.org/10.1002/ejic.200900899
SN - 1434-1948
SN - 1099-0682
VL - 2009
IS - 32
SP - 4771
EP - 4775
PB - Wiley-VCH Verl.
CY - Weinheim
AN - OPUS4-20329
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Thünemann, Andreas
A1 - Kegel, Jenny
A1 - Polte, Jörg
A1 - Emmerling, Franziska
T1 - Superparamagnetic Maghemite Nanorods: Analysis by Coupling Field-Flow Fractionation and Small-Angle X-ray Scattering
JF - Analytical chemistry
N2 - We report on the online coupling of asymmetrical flow field-flow fractionation (A4F) with small-angle X-ray scattering (SAXS) for the detection of nanoparticles. The A4F was used to fractionate superparamagnetic maghemite nanoparticles, which were prepared continuously with a micromixer. The outlet of the A4F was directly coupled to a flow capillary of a SAXSess instrument (Kratky type of camera). SAXS curves were recorded in a 1 s time interval. This was possible by using intense synchrotron radiation. The radii of gyration of the nanoparticles, as determined from Guinier plots, increased from 2 to 6 nm with increasing fractionation time of the A4F. A more detailed analysis of the scattering curves revealed that the particles were cylindrical in shape (nanorods), which we attributed to the micromixing preparation technique. The radii of the nanorods increased only slightly from 1.2 to 1.7 nm with increasing fractionation time, while the lengths increased strongly from 7.0 to 30.0 nm. The volume distribution of the nanorods was determined and described by Schultz-Zimm and log-normal distributions. Nanorod volumes increased from 45 to 263 nm³, corresponding to molar masses of 140 × 10³ to 820 × 10³ g mol-1. We propose A4F-SAXS coupling as a new method for analysis of nanoparticles of complex composition in solution. It allows precise online determination of the particles shape and size distributions. This method can be applied to mixtures of nanoparticles of arbitrary shapes and sizes (1-100 nm). Moreover, the total time needed for fractionation and online SAXS data recording is usually only 20 min.
PY - 2008
DO - https://doi.org/10.1021/ac8004814
SN - 0003-2700
SN - 1520-6882
VL - 80
IS - 15
SP - 5905
EP - 5911
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-17813
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Trowitzsch-Kienast, W.
A1 - Rühl, M.
A1 - Kim, K.Y.
A1 - Emmerling, Franziska
A1 - Erben, U.
A1 - Somasundaram, R.
A1 - Freise, C.
T1 - Absolute configuration of antifibrotic (+)-episesamin isolated from Lindera obtusiloba BLUME
JF - Zeitschrift für Naturforschung
N2 - Fractionation of a 70% ethanolic extract from twigs of Lindera obtusiloba BLUME (Japanese spicebush, Tohaku) yielded fi ve fractions of different polarity. The antifi brotic activity within the chloroform phase was best assessed by an in vitro bioassay using rat hepatic stellate cell (HSC) proliferation and their autocrine transforming growth factor beta (TGF-β) expression as sensitive fibrosis-associated read out. Chromatography of the chloroform extract on Sephadex LH-20 or liquid-liquid extractions yielded a crystalline compound as an active principle, which was identifi ed from NMR and ESI-MS analyses, its melting point, and its optical rotation as (7S,7'S,8S,8'S)-3,4:3',4'-bis(methylenedioxy) -7,9':7',9-diepoxy-lignane [(+)-episesamin]. X-Ray diffraction confirmed the structure and provided, for the fi rst time, directly its absolute confi guration. (+)-Episesamin blocked proliferation and the profi brotic autocrine TGF-β expression HSC without signifi cant cytotoxicity.
KW - TGF-beta
KW - Liver Fibrosis
KW - X-Ray Structure
PY - 2011
SN - 0939-5075
SN - 0341-0382
SN - 0341-0471
VL - 66c
IS - 9/10
SP - 460
EP - 464
PB - Verl. d. Zeitschrift für Naturforschung
CY - Tübingen
AN - OPUS4-24716
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tuchalski, G.
A1 - Emmerling, Franziska
A1 - Gröger, K.
A1 - Hänsicke, A.
A1 - Nagel, T.
A1 - Reck, Günter
T1 - X-ray investigations of nebivolol and its isomers
JF - Journal of molecular structure
N2 - The molecular and crystal structures of the hydrochlorides of d-nebivolol, dl-nebivolol, and seven nebivolol isomers have been determined by X-ray structure analysis. The absolute configuration of all the compounds could be determined unambiguously using anomal dispersion effects. Two compounds, dl-nebivolol (NEB-1d,l) and the (S,R,S,R) nebivolol isomer (NEB-6), crystallize as racemic mixtures in the centrosymmetric space group P-1. d-Nebivolol and six nebivolol isomers crystallize in space group P212121. The d- and l-nebivolol molecules in NEB-1d and NEB-1d,l adopt a conformation which is significantly different compared with that of all nebivolol isomers. With the exception of dl-nebivolol (NEB-1d,l) numerous intermolecular hydrogen bonds connect the molecules forming molecular layers.
KW - X-ray crystal structure
KW - Nebivolol
PY - 2006
DO - https://doi.org/10.1016/j.molstruc.2006.03.086
SN - 0022-2860
SN - 1872-8014
SN - 0377-046X
VL - 800
IS - 1-3
SP - 28
EP - 44
PB - Elsevier
CY - Amsterdam
AN - OPUS4-13800
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Tumanova, N.
A1 - Tumanov, N.
A1 - Robeyns, K.
A1 - Fischer, Franziska
A1 - Fusaro, L.
A1 - Morelle, F.
A1 - Ban, V.
A1 - Hautier, G.
A1 - Filinchuk, Y.
A1 - Wouters, J.
A1 - Leyssens, T.
A1 - Emmerling, Franziska
T1 - Opening Pandora’s Box: Chirality, Polymorphism, and Stoichiometric Diversity in Flurbiprofen/Proline Cocrystals
JF - Crystal Growth & Design
N2 - Proline has been widely used for various cocrystallization applications, including pharmaceutical cocrystals. Combining enantiopure and racemic flurbiprofen and proline, we discovered 18 new crystal structures. Liquid-assisted grinding proved highly efficient to explore all the variety of crystal forms. A unique combination of stateof-the-art characterization techniques, comprising variable temperature in situ X-ray diffraction and in situ ball-milling, along with other physicochemical methods and density functional theory calculations, was indispensable for identifying all the phases. Analyzing the results of in situ ball-milling, we established a stepwise mechanism for the formation of several 1:1 cocrystals via an intermediate 2:1 phase. The nature of the solvent in liquidassisted grinding was found to significantly affect the reaction rate and, in some cases, the reaction pathway.
KW - Mechanochemistry
KW - Polymorphs
KW - In situ
PY - 2018
UR - https://pubs.acs.org/doi/abs/10.1021/acs.cgd.7b01436
DO - https://doi.org/10.1021/acs.cgd.7b01436
VL - 18
IS - 2
SP - 954
EP - 961
PB - American Chemical Society
AN - OPUS4-44365
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Unterlass, M.M.
A1 - Emmerling, Franziska
A1 - Antonietti, M.
A1 - Weber, J.
T1 - From dense monomer salt crystals to CO2 selective microporous polyimides via solid-state polymerization
JF - Chemical communications
N2 - Fully aromatic polyimides are synthesized via solid-state polymerization of the corresponding monomer salts. The crystal structure of salts shows strong hydrogen bonding of the reactive groups and thereby paves the way for solid-state transformations. The polycondensation yields copies of the initial salt crystallite habits, accompanied by the development of a porosity especially suited for CO2.
PY - 2014
DO - https://doi.org/10.1039/c3cc47674j
SN - 0022-4936
SN - 0009-241x
SN - 1359-7345
SN - 1364-548x
VL - 50
IS - 4
SP - 430
EP - 432
PB - Royal Society of Chemistry
CY - Cambridge
AN - OPUS4-29813
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Villajos Collado, José Antonio
A1 - Bienert, M.
A1 - Gugin, Nikita
A1 - Emmerling, Franziska
A1 - Maiwald, Michael
T1 - A database to select affordable MOFs for volumetric hydrogen cryoadsorption considering the cost of their linkers
JF - Materials advances
N2 - Physical adsorption at cryogenic temperature (cryoadsorption) is a reversible mechanism that can reduce the pressure of conventional compressed gas storage systems. Metal–organic framework (MOF) materials are remarkable candidates due to the combination of high specific surface area and density which, in some cases, provide a high volumetric storage capacity. However, such extensive use of MOFs for this application requires the selection of affordable structures, easy to produce and made from feasible metallic and organic components. Herein, we introduce a MOF database detailing the crystallographic and porous properties of 3600 existing MOFs made from industrially relevant metals and their organic composition. The comparison of the available minimum costs of linkers allowed the creation of a database to select affordable structures with high potential for volumetric hydrogen storage by cryoadsorption, considering their composition based on individual or mixed building blocks. A user inter� face, available online, facilitates the selection of MOFs based on the properties or names of structures and linkers.
KW - MOF´s
PY - 2023
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583619
DO - https://doi.org/10.1039/d3ma00315a
VL - 4
IS - 18
SP - 4226
EP - 4237
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-58361
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Walter, Astrid
A1 - Pfeifer, Dietmar
A1 - Kraus, Werner
A1 - Emmerling, Franziska
A1 - Schneider, Rudolf
A1 - Panne, Ulrich
A1 - Weller, Michael G.
T1 - Triacetone Triperoxide (TATP): Hapten design and development of antibodies
JF - Langmuir
N2 - Triacetone triperoxide (TATP), an improvised explosive, is a potential security threat because of its cost-efficient synthesis and the difficulty in detecting it. A highly selective antibody could provide the necessary specificity to the detection process. To obtain antibodies, a hapten made from acetone, hydrogen peroxide, and 7-oxooctanoic acid has been designed, synthesized, and confirmed by NMR that displays the utmost similarity to the analyte. The single-crystal X-ray structures of the solvated species TATP·methanol (1:1) and the TATP derivate were determined. In both compounds, the molecules exhibit D3 symmetry and adopt a twisted boat-chair conformation. The hapten was coupled to bovine serum albumin, and mice were immunized. An immune response against TATP was elicited, and selective antibodies were detected in the mouse serum, which should be very useful for the development of a TATP biosensor system. An ELISA with a limit of detection for TATP of 65 µg L-1 is shown.
KW - TATP
KW - Triacetone triperoxide
KW - Explosive
KW - Antibody
KW - Hapten immunoassay
KW - Structure
PY - 2010
DO - https://doi.org/10.1021/la1018339
SN - 0743-7463
SN - 1520-5827
VL - 26
IS - 19
SP - 15418
EP - 15423
PB - American Chemical Society
CY - Washington, DC
AN - OPUS4-22469
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Walther, M.
A1 - Matterna, M.
A1 - Juran, S.
A1 - Fähnemann, S.
A1 - Stephan, H.
A1 - Kraus, Werner
A1 - Emmerling, Franziska
T1 - Imidazole-containing bispidine ligands: synthesis, structure and Cu(II) complexation
JF - Zeitschrift für Naturforschung B
N2 - The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine Skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, Crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state.
KW - Piperidone
KW - Bispidine
KW - Copper(II)
KW - Configuration isomerism
PY - 2011
SN - 0932-0776
SN - 0340-5087
SN - 0044-3174
VL - 66b
SP - 721
EP - 728
PB - Verl. d. Zeitschrift für Naturforschung
CY - Tübingen
AN - OPUS4-24091
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wegner, Karl David
A1 - Häusler, I.
A1 - Knigge, Xenia
A1 - Hodoroaba, Vasile-Dan
A1 - Emmerling, Franziska
A1 - Reiss, P.
A1 - Resch-Genger, Ute
T1 - One-Pot Heat-Up Synthesis of ZnSe Magic-Sized Clusters Using Thiol Ligands
JF - Inorganic Chemistry
N2 - The synthesis of two new families of ZnSe magic-sized clusters (MSCs) is achieved using the thiol ligand 1-dodecanethiol in a simple one-pot heat-up approach. The sizes of the MSCs are controlled with the thiol ligand concentration and reaction temperature.
KW - ZnSe
KW - Magic-sized cluster
KW - Dodecanethiol
KW - Semiconductor nanocrystals
KW - One-pot synthesis
PY - 2022
DO - https://doi.org/10.1021/acs.inorgchem.2c00041
VL - 61
IS - 19
SP - 7207
EP - 7211
PB - ACS Publications
CY - Washington, DC (USA)
AN - OPUS4-54880
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - Akhemtova, Irina
A1 - Rademann, K.
A1 - Emmerling, Franziska
T1 - Mechanochemical synthesis of cerium(IV)-phosphonates
JF - Journal of materials science
N2 - The syntheses and crystal structures of two cerium(IV) phosphonates are presented. Cerium(IV) bis(phenylphosphonate) Ce(O3PC6H5)2 1 can be formed from precipitation and mechanochemical reaction, whereas cerium(IV) bis(carboxymethylphosphonate) monohydrate Ce(O3PCH2COOH)2 H2O 2 is only accessible via ball milling. All reactions proceed very fast and are completed within a short time span. In situ measurements for the syntheses of 1 show that the product occurs within seconds or a few minutes, respectively. The structures were solved from powder X-ray diffraction data.
KW - In situ studies
KW - Mechanochemistry
KW - XRD
PY - 2018
DO - https://doi.org/10.1007/s10853-018-2507-x
SN - 0022-2461
SN - 1573-4803
VL - 53
IS - 19
SP - 13733
EP - 13741
PB - Springer Science + Business Media B.V.
AN - OPUS4-45672
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Wilke, Manuel
A1 - Bach, S.
A1 - Gorelik, T.
A1 - Kolb, U.
A1 - Tremel, W.
A1 - Emmerling, Franziska
T1 - Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution
JF - Zeitschrift für Kristallographie - Crystalline Materials
N2 - Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry of the phosphonate linkers enables the formation of structures with different dimensionalities ranging from isolated complexes and layered structures to porous frameworks incorporating various functionalities through the choice of the building blocks.
In brief, metal phosphonates offer an interesting opportunity for the design of multifunctional materials. Here, we provide a short review on the class of divalent metal phosphonates discussing their syntheses, structures, and applications. We present the advantages of the recently introduced mechanochemical pathway for the Synthesis of divalent phosphonates as a possibility to generate new, in certain cases metastable compounds. The benefits of in situ investigation of synthesis mechanisms as well as the implementation of sophisticated methods for the structure analysis of the resulting compounds are discussed.
KW - Metal phosphonate
KW - Mechanochemistry
PY - 2017
DO - https://doi.org/10.1515/zkri-2016-1971
SN - 2194-4946
SN - 2196-7105
VL - 232
IS - 1-3
SP - 209
EP - 222
PB - De Gruyter
AN - OPUS4-40003
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -