Thermal behavior, structure, and dynamics of low-temperature water confined in mesoporous organosilica by differential scanning calorimetry, X-ray diffraction, and quasi-elastic neutron scattering

2012 ◽  
Vol 85 (1) ◽  
pp. 289-305 ◽  
Author(s):  
Mai Aso ◽  
Kanae Ito ◽  
Hiroaki Sugino ◽  
Koji Yoshida ◽  
Takeshi Yamada ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Water Molecule ◽  
Neutron Scattering ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Elastic Neutron ◽  
X Ray ◽  
Mesoporous Organosilica ◽  
Condensed Water ◽  
Elastic Neutron Scattering

Differential scanning calorimetry (DSC), X-ray diffraction (XRD), and quasi-elastic neutron scattering (QENS) measurements have been made at 200~330 K for capillary-condensed water confined in periodic mesoporous organosilica (PMO) materials with the phenyl groups embedded in silica matrix (Ph-PMO; pore diameter 30 Å). The DSC data showed that the capillary-condensed water in Ph-PMO freezes at 228 K. X-ray radial distribution functions (RDFs) showed that the tetrahedral-like hydrogen-bonded structure of water is distorted in Ph-PMO pores, compared with bulk water; however, with lowering temperature the tetrahedral moiety of water is gradually recovered in the pores. Below the freezing point, cubic ice Ic was formed in the Ph-PMO pores. The QENS data showed that the translational diffusion constant and the residence time and the rotational relaxation time of water molecule in Ph-PMO are comparable with those in bulk. The corresponding activation energies suggested that the more hydrophobic the nature of the wall is, the smaller the activation energy of diffusion and rotation of a water molecule; this implies that water molecules confined in the hydrophobic pores are present in the core of the pores, whereas those in the hydrophilic pores strongly interact with the silanol groups.

Multidisciplinary study on the hydrogelation of digold(I) complex [{Au(9N-adeninate)}2(μ-dmpe)]: optical, rheological, and quasi-elastic neutron scattering perspectives

2021 ◽  
Author(s):  
José Maria López-de-Luzuriaga ◽  
Daniel Blasco ◽  
Miguel Monge ◽  
Maria Elena Olmos ◽  
María Rodríguez-Castillo ◽  
...  
Keyword(s):  
Neutron Scattering ◽  
X Ray Diffraction ◽  
Elastic Neutron ◽  
X Ray ◽  
Multidisciplinary Study ◽  
Elastic Neutron Scattering ◽  
Aurophilic Interaction

Herein, the syntheses of [{Au(9N-adeninate)}2(μ-dmpe)] (2, dmpe = 1,2-bis(dimethylphosphino)ethane) and its chloride precursor [(AuCl)2(μ-dmpe)] (1) are described. X-ray diffraction of 2 reveals a short intramolecular aurophilic interaction (2.9919(8) Å), which...

Research on compatibility and surface of high impact bio-based polyamide

2021 ◽  
pp. 095400832110055
Author(s):  
Yang Wang ◽  
Yuhui Zhang ◽  
Yuhan Xu ◽  
Xiucai Liu ◽  
Weihong Guo
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Scanning Electron Microscopy ◽  
Differential Scanning Calorimetry ◽  
Crystallization Behavior ◽  
High Impact ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Scanning Electron

The super-tough bio-based nylon was prepared by melt extrusion. In order to improve the compatibility between bio-based nylon and elastomer, the elastomer POE was grafted with maleic anhydride. Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA) were used to study the compatibility and micro-distribution between super-tough bio-based nylon and toughened elastomers. The results of mechanical strength experiments show that the 20% content of POE-g-MAH has the best toughening effect. After toughening, the toughness of the super-tough nylon was significantly improved. The notched impact strength was 88 kJ/m2 increasing by 1700%, which was in line with the industrial super-tough nylon. X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were used to study the crystallization behavior of bio-based PA56, and the effect of bio-based PA56 with high crystallinity on mechanical properties was analyzed from the microstructure.

scholarly journals Synthesis and mesomorphic properties of calamitic malonates and cyanoacetates tethered to 4-cyanobiphenyls

2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ambient Temperature ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Cyanoacetic Acid ◽  
Scanning Calorimetry ◽  
Isotropic Liquid ◽  
X Ray ◽  
Nematic Phases ◽  
Mesomorphic Properties

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).

Inosose-Flüssigkristalle / Inosose Liquid Crystals

1990 ◽  
Vol 45 (7) ◽  
pp. 1084-1090 ◽  
Author(s):  
Klaus Praefcke ◽  
Bernd Kohne ◽  
Andreas Eckert ◽  
Joachim Hempel
Keyword(s):  
Differential Scanning Calorimetry ◽  
Liquid Crystal ◽  
High Temperature ◽  
Liquid Crystalline ◽  
Structural Features ◽  
Lyotropic Liquid Crystal ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Alkyl Chains

Six S,S-dialkyl acetals 2a-f of inosose (1), tripodal in structure, have been synthesized, characterized and investigated by optical microscopy and differential scanning calorimetry (d.s.c.). The four S,S-acetals 2c-f with sufficiently long alkyl chains are thermotropic liquid crystalline; 2 e and 2 f are even dithermomesomorphic. Each of these four inosose derivatives 2c-f exhibits monotropically a most likely cubic mesophase (MI); in addition 2e and 2f show enantiotropically a hexagonal mesophase (Hx) with a non-covalent, supramolecular H-bridge architecture. Whereas the nature of the optically isotropic mesophase MI needs further clarification the stable high temperature mesophase Hx of 2 e and 2 f has been established by a miscibility test using a sugar S,S-dialkyl acetal also tripodal in structure and with a Hx phase proved by X-ray diffraction, but in contrast to 2 with an acyclic hydrophilic part. Similarities of structural features between the Hx-phases of 2e and 2f as well as of other thermotropic and lyotropic liquid crystal systems are discussed briefly.

scholarly journals Formation of Pharmaceutical Salts and Cocrystals via Vapour-Assisted Tumbling (VAT) – A Solvent Efficient Process with Potential Industrial Applications

2021 ◽  
Author(s):  
Alexander J. Stirk ◽  
Fabio E. S. Souza ◽  
Jenny Gerster ◽  
Fatemeh M. Mir ◽  
Avedis Karadeolian ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Environmental Impact ◽  
Industrial Applications ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
New Techniques ◽  
X Ray ◽  
Industry Standard ◽  
Pharmaceutical Salts ◽  
Solid Form

Crystallisations on both the academic and industrial scale often use large volumes of solvent. In order decrease the environmental impact of such processes, new techniques must be discovered that increase the efficiency of the solvents used. Introduced here is a process that combines repurposed industry standard hardware and aspects of mechanochemistry to produce a technique we call “Vapour Assisted Tumbling” (VAT). Pharmaceutical and well-known cocrystals and salts were formed by tumbling the coformers in an atmosphere of vaporised solvent, in this study, methanol (MeOH). This was done inside a custom built analogue of an industrial rotary cone dryer (RCD). It was found that a desired solid form could be obtained as monitored by powder X-ray diffraction and differential scanning calorimetry. By repurposing industrial RCDs, it is feasible that solid forms can be crystallised with both minimal and reusable/recyclable solvent – drastically lowering the environmental impact of such transformations.

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