Polyethersulfone polymers and oligomers — Morphology and crystallization

2012 ◽  
Vol 90 (10) ◽  
pp. 880-890 ◽  
Author(s):  
Abdelkader Benhalima ◽  
François Hudon ◽  
Finda Koulibaly ◽  
Christian Tessier ◽  
Josée Brisson

Crystal forms of polyethersulfones (PES) were investigated by using a model compound and a low molecular weight oligomer. These are amorphous as-synthesized, and can undergo solvent-induced crystallization under the appropriate conditions. The model compound, 4,4′-bis(p-methoxyphenoxy)diphenyl sulfone, yielded monocrystals, and its structure was solved using X-ray diffraction. Conformational disorder is present, two conformers cohabiting in 55:45 proportions. This model compound, combined to previous structural studies published in the literature, served as a basis for conformational studies of polyethersulfone. Low molecular weight polymers submitted to solvent-induced crystallization resulted in a PES crystal form different from that previously published in the literature, as shown by powder X-ray diffraction.

2017 ◽  
Vol 54 (4) ◽  
pp. 655-658
Author(s):  
Andrei Bejan ◽  
Dragos Peptanariu ◽  
Bogdan Chiricuta ◽  
Elena Bicu ◽  
Dalila Belei

Microfibers were obtained from organic low molecular weight compounds based on heteroaromatic and aromatic rings connected by aliphatic spacers. The obtaining of microfibers was proved by scanning electron microscopy. The deciphering of the mechanism of microfiber formation has been elucidated by X-ray diffraction, infrared spectroscopy, and atomic force microscopy measurements. By exciting with light of different wavelength, florescence microscopy revealed a specific optical response, recommending these materials for light sensing applications.


Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.


CrystEngComm ◽  
2015 ◽  
Vol 17 (42) ◽  
pp. 8047-8057 ◽  
Author(s):  
Emily R. Draper ◽  
Kyle L. Morris ◽  
Marc A. Little ◽  
Jaclyn Raeburn ◽  
Catherine Colquhoun ◽  
...  

A number of Fmoc amino acids can be effective low molecular weight hydrogelators; we compare single crystal structures to fibre X-ray diffraction data.


2005 ◽  
Vol 3 (8) ◽  
pp. 441-451 ◽  
Author(s):  
N.W Rizzo ◽  
K.H Gardner ◽  
D.J Walls ◽  
N.M Keiper-Hrynko ◽  
T.S Ganzke ◽  
...  

The ability of certain reptiles to adhere to vertical (and hang from horizontal) surfaces has been attributed to the presence of specialized adhesive setae on their feet. Structural and compositional studies of such adhesive setae will contribute significantly towards the design of biomimetic fibrillar adhesive materials. The results of electron microscopy analyses of the structure of such setae are presented, indicating their formation from aggregates of proteinaceous fibrils held together by a matrix and potentially surrounded by a limiting proteinaceous sheath. Microbeam X-ray diffraction analysis has shown conclusively that the only ordered protein constituent in these structures exhibits a diffraction pattern characteristic of β-keratin. Raman microscopy of individual setae, however, clearly shows the presence of additional protein constituents, some of which may be identified as α-keratins. Electrophoretic analysis of solubilized setal proteins supports these conclusions, indicating the presence of a group of low-molecular-weight β-keratins (14–20 kDa), together with α-keratins, and this interpretation is supported by immunological analyses.


1943 ◽  
Vol 21b (10) ◽  
pp. 219-223 ◽  
Author(s):  
E. B. Paul ◽  
A. L. Blakers ◽  
R. W. Watson

Milkweed latex collected in mid-July was coagulated in acetone, the coagulum purified, and the rubber examined by chemical and X-ray diffraction methods. Chromic acid oxidation analyses indicate that the monomer is isoprene. The X-ray evidence verifies these results and, further, fixes the polymer as the cis-configuration (rubber) as opposed to the trans-configuration (gutta-percha) of polyisoprene.The solvent-extracted rubber from the leaves appears from the chromic acid oxidation results to be isoprene, but so far no polyisoprene diffraction diagram has been obtained. It is therefore likely that the solvent-extracted leaf rubber is an isoprene polymer of low molecular weight.


1979 ◽  
Vol 52 (5) ◽  
pp. 920-948 ◽  
Author(s):  
Yuji Minoura ◽  
Shinzo Yamashita ◽  
Hiroshi Okamoto ◽  
Tadao Matsuo ◽  
Michiaki Izawa ◽  
...  

Abstract The structure-property relationships of polyurethane elastomers derived from a liquid hydroxyl-terminated polybutadiene/low molecular weight aliphatic diol/diisocyanate system were studied. The effects of the amount of low molecular weight diol on the mechanical properties of the elastomer were discussed on the basis of the results of stress-strain, swelling, dynamic viscoelasticity, x-ray diffraction, etc. It was found that some particular combinations of low molecular weight diol and diisocyanate specifically affect the properties of elastomers. When the mechanical properties of the elastomers were plotted against the number of methylene carbons in the low molecular weight diol, characteristic zigzag patterns were obtained. These patterns were explained by the difference in the packing and the dependence of the strength of intermolecular hydrogen bonding on whether the number of the methylene carbons was even or odd. This assumption was confirmed by x-ray diffraction.


2017 ◽  
Vol 8 (41) ◽  
pp. 6443-6454 ◽  
Author(s):  
Ilaria D'Auria ◽  
Stefano Milione ◽  
Tonino Caruso ◽  
Gabriele Balducci ◽  
Claudio Pellecchia

A 6-(2,6-dimethylphenyl)-2-(2,6-diisopropylphenyl)iminopyridine dibromo nickel(ii) complex was synthesized, characterized by X-ray diffraction analysis and tested in ethylene polymerization using diethylaluminumchloride as the cocatalyst.


1995 ◽  
Vol 50 (4) ◽  
pp. 469-475 ◽  
Author(s):  
Gerhard Erker ◽  
Christian Psiorz ◽  
Roland Fröhlich

2,5-Hexanedione was converted into the bisfulvene 2, then treated with two molar equivalents of methyllithium to yield the [4-cyclopentadienylidene-4,7,7-trimethyl-4,5,6,7-tetrahydroindenyl] dilithio compound 4. Hydrolysis, followed by treatment with acetone/pyrrolidine, gave the corresponding fulvene system 5. Reaction of 5 with methyllithium followed by treatment with ZrCl4 furnished the ring-annulated C1-bridged ansa-metallocene 8, bearing a tert-butyl substituent at the Cp ring, as a 1:1 mixture of two diastereoisomers. Treatment of the fulvene 5 with LiAlH4 followed by ZrCl4 yielded the respective isopropyl-substituted ansa-metallocene diastereomers 9a and 9b. Complex 9b was separated by fractional crystallization and characterized by X-ray diffraction. Complexes 8 and 9 provide active homogeneous Ziegler-type catalyst systems upon activation with excess methylalumoxane producing low molecular weight isotactic polypropylene with high catalyst activities.


Sensors ◽  
2020 ◽  
Vol 20 (5) ◽  
pp. 1385 ◽  
Author(s):  
Andrés Rodríguez ◽  
Elio Rico ◽  
Cesar Sierra ◽  
Oscar Rodríguez

Two Covalent Organic Frameworks (COF), named TFP-BZ and TFP-DMBZ, were synthesized using the imine condensation between 1,3,5-triformylphloroglucinol (TFP) with benzidine (BZ) or 3,3-dimethylbenzidine (DMBZ). These materials were deposited, such as films over interdigitated electrodes (IDE), by chemical bath deposition, giving rise to TFP-BZ-IDE and TFP-DMBZ-IDE systems. The synthesized COFs powders were characterized by Powder X-Ray Diffraction (PXRD), Fourier Transform Infrared spectroscopy (FT-IR), solid-state Nuclear Magnetic Resonance (ssNMR), nitrogen adsorption isotherms, Scanning Electron Microscopy (SEM), and Raman spectroscopy, while the films were characterized by SEM and Raman. Ammonia and low molecular weight amine sensing were developed with the COF film systems using the impedance electrochemical spectroscopy (EIS). Results showed that the systems TFP-BZ-IDE and TFP-DMBZ-IDE detect low molecular weight amines selectively by impedimetric analysis. Remarkably, with no significant interference by other atmospheric gas compounds such as nitrogen, carbon dioxide, and methane. Additionally, both COF films presented a range of sensitivity at low amine concentrations below two ppm at room temperature.


2016 ◽  
Vol 8 (7) ◽  
pp. 1637-1645 ◽  
Author(s):  
Nati Salvadó ◽  
Salvador Butí ◽  
Trinitat Pradell ◽  
Victòria Beltran ◽  
Gianfelice Cinque ◽  
...  

Micro-Infrared Spectroscopy (μSR-FTIR) and X-ray diffraction (μSR-XRD) with synchrotron light, Gas Chromatography/Mass Spectrometry (CG/MS), Optical Microscopy (OM) and Scanning Electron Microscopy (SEM/EDS) were used to obtain the distribution of calcium salts of low molecular weight organic acids (LMWOA) in micro-layered micro-samples.


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