scholarly journals Microstructural Changes during Degradation of Biobased Poly(4-hydroxybutyrate) Sutures

Polymers ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 2024
Author(s):  
Ina Keridou ◽  
Lourdes Franco ◽  
Luis J. del Valle ◽  
Juan C. Martínez ◽  
Lutz Funk ◽  
...  

Fibers of poly(4-hydroxybutyrate) (P4HB) have been submitted to both hydrolytic and enzymatic degradation media in order to generate samples with different types and degrees of chain breakage. Random chain hydrolysis is clearly enhanced by varying temperatures from 37 to 55 °C and is slightly dependent on the pH of the medium. Enzymatic attack is a surface erosion process with significant solubilization as a consequence of a preferent stepwise degradation. Small angle X-ray diffraction studies revealed a peculiar supramolecular structure with two different types of lamellar stacks. These were caused by the distinct shear stresses that the core and the shell of the fiber suffered during the severe annealing process. External lamellae were characterized by surfaces tilted 45° with respect to the stretching direction and a higher thickness, while the inner lamellae were more imperfect and had their surfaces perpendicularly oriented to the fiber axis. In all cases, WAXD data indicated that the chain molecular axis was aligned with the fiber axis and molecules were arranged according to a single orthorhombic structure. A gradual change of the microstructure was observed as a function of the progress of hydrolysis while changes were not evident under an enzymatic attack. Hydrolysis mainly affected the inner lamellar stacks as revealed by the direct SAXS patterns and the analysis of correlation functions. Both lamellar crystalline and amorphous thicknesses slightly increased as well as the electronic contrast between amorphous and crystalline regions. Thermal treatments of samples exposed to the hydrolytic media revealed microstructural changes caused by degradation, with the inner lamellae being those that melted faster.

Polymers ◽  
2019 ◽  
Vol 11 (4) ◽  
pp. 721 ◽  
Author(s):  
Jorge A. Ramírez-Gómez ◽  
Javier Illescas ◽  
María del Carmen Díaz-Nava ◽  
Claudia Muro-Urista ◽  
Sonia Martínez-Gallegos ◽  
...  

Atrazine (ATZ) is an herbicide which is applied to the soil, and its mechanism of action involves the inhibition of photosynthesis. One of its main functions is to control the appearance of weeds in crops, primarily in corn, sorghum, sugar cane, and wheat; however, it is very toxic for numerous species, including humans. Therefore, this work deals with the adsorption of ATZ from aqueous solutions using nanocomposite materials, synthesized with two different types of organo-modified clays. Those were obtained by the free radical polymerization of 4-vinylpyridine (4VP) and acrylamide (AAm) in different stoichiometric ratios, using tetrabutylphosphonium persulfate (TBPPS) as a radical initiator and N,N′-methylenebisacrylamide (BIS) as cross-linking agent. The structural, morphological, and textural characteristics of clays, copolymers, and nanocomposites were determined through different analytical and instrumental techniques, i.e., X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). Adsorption kinetics experiments of ATZ were determined with the modified and synthesized materials, and the effect of the ratio between 4VP and AAm moieties on the removal capacities of the obtained nanocomposites was evaluated. Finally, from these sets of experiments, it was demonstrated that the synthesized nanocomposites with higher molar fractions of 4VP obtained the highest removal percentages of ATZ.


Polymers ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 53
Author(s):  
Adrian Szewczyk ◽  
Adrianna Skwira ◽  
Marta Ginter ◽  
Donata Tajer ◽  
Magdalena Prokopowicz

Herein, the microwave-assisted wet precipitation method was used to obtain materials consisting of mesoporous silica (SBA-15) and calcium orthophosphates (CaP). Composites were prepared through immersion of mesoporous silica in different calcification coating solutions and then exposed to microwave radiation. The composites were characterized in terms of molecular structure, crystallinity, morphology, chemical composition, and mineralization potential by Fourier-transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD), and scanning electron microscopy equipped with energy-dispersive X-ray spectroscopy (SEM-EDX). The application of microwave irradiation resulted in the formation of different types of calcium orthophosphates such as calcium deficient hydroxyapatite (CDHA), octacalcium phosphate (OCP), and amorphous calcium phosphate (ACP) on the SBA-15 surface, depending on the type of coating solution. The composites for which the progressive formation of hydroxyapatite during incubation in simulated body fluid was observed were further used in the production of final pharmaceutical forms: membranes, granules, and pellets. All of the obtained pharmaceutical forms preserved mineralization properties.


Author(s):  
Peng Liu ◽  
Hongbin Zhang ◽  
Sinong Wang ◽  
Hui Yu ◽  
Bingjie Lu ◽  
...  

AbstractThe crystallinity indices (CrI) of Chinese handmade papers were investigated using the X-ray diffraction (XRD) method. Four Chinese handmade papers, Yingchun, Zhuma, Yuanshu and Longxucao papers were used as model substrates of mulberry bark, ramie, bamboo and Eulaliopsis binata papers, respectively. Two forms of the paper samples, paper sheets and their comminuted powders, were used in this study. The results showed that their XRD patterns belong to the cellulose-I type and Iβ dominates the cellulose microstructure of these paper samples. Moreover, it was found that the microstructures and CrIs of cellulose of these papers were changed by the grinding treatment. This work suggested that the sheet form of the handmade papers is suitable to determine CrI by XRD, despite the contribution of non-cellulosic components in the papers. The order of CrIs for these paper sheet samples was Yingchun, Zhuma, Longxucao and Yuanshu papers. Besides CrIs, differences in cross-sectional areas of the crystalline zone of cellulose can be used for comparing different types of handmade papers. It was also found that the CrIs and crystallite size of paper cellulose varied between the sheet samples and the powder samples, illustrating that the pulverisation has a negative influence on the microstructure of the handmade papers.


Symmetry ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 732
Author(s):  
Alexander A. Bredikhin ◽  
Aidar T. Gubaidullin ◽  
Zemfira A. Bredikhina ◽  
Robert R. Fayzullin ◽  
Olga A. Lodochnikova

Chiral recognition plays an important role in the self-assembly of soft materials, in particular supramolecular organogels formed by low molecular weight gelators (LMWGs). Out of 14 pairs of the studied racemic and enantiopure samples of alkyl-substituted phenyl ethers of glycerol, only eight enantiopure diols form the stable gels in nonane. The formation of gels from solutions was studied by polarimetry, and their degradation with the formation of xerogels was studied by the PXRD method. The revealed crystalline characteristics of all studied xerogels corresponded to those for crystalline samples of the parent gelators. In addition to those previously investigated, crystalline samples of enantiopure para-n-alkylphenyl glycerol ethers [alkyl = pentyl (5), hexyl (6), heptyl (7), octyl (8), nonyl (9)] and racemic 3-(3,5-dimethylphenoxy)propane-1,2-diol (rac-14) have been examined by single crystal X-ray diffraction analysis. Among 22 samples of compounds 1-14 studied by SC-XRD, seven different types of supramolecular motifs are identified, of which only two are realized in crystals of supramolecular gelators. An attempt was made to relate the ability to gel formation with the characteristics of the supramolecular motif of a potential gelling agent, and the frequency of formation of the motif, required for gelation, with the chiral characteristics of the sample.


2018 ◽  
Vol 74 (12) ◽  
pp. 1684-1691
Author(s):  
Marek L. Główka ◽  
Sylwia Kałużyńska ◽  
Malwina Krause ◽  
Katarzyna Gobis ◽  
Henryk Foks ◽  
...  

Tuberculosis still remains a very important problem, especially its multidrug resistant varieties (MDR-TB). Among the potential tuberculostatics, there are two benzimidazole derivatives, namely 5,6-dimethyl-2-phenylethylbenzo[d]imidazole (1) and (E)-5,6-dimethyl-2-styryl-1H-benzo[d]imidazole (2) which showed significant tuberculostatic activities, better than those of Pyrazinamide and Isoniazyd. Also, the cytotoxicity of 1 appeared promising. The compounds were studied (with the use of X-ray diffraction) in the form of the hemihydrate of 1, C17H18N2·0.5H2O (1a), the methanol hemisolvate of 2, C17H16N2·0.5CH3OH (2a), and the acid oxalate salt of 2, namely (E)-5,6-dimethyl-2-styryl-1H-benzo[d]imidazolium hydrogen oxalate, C17H17N2 +·C2HO4 − (2b). All three structures reveal a similar extended conformation, despite the flexible linker between the two aromatic systems and the different types of strong intermolecular hydrogen bonds. The molecules of 2a are practically planar due to the double bond in the linker, which enables conjugation along the whole molecule, while the molecules of 1a exhibit the possibility of parallel orientations of their aromatic systems, despite the aliphatic (ethyl) linker.


Clay Minerals ◽  
2017 ◽  
Vol 52 (4) ◽  
pp. 453-468 ◽  
Author(s):  
A. Aras ◽  
S. Kiliç

AbstractThe present study focused on the mineralogical and chemical characterization and firing behaviour of clays from the Lake Van region and compared them with the same characteristics established for two ancient pot sherds. Four pottery clays collected from Kutki and Kuşluk in the Kesan Valley to the south, from Kavakbaşı to the southwest and from Bardakçı village on the east coast of Lake Van were analysed by X-ray diffraction to identify mineralogical composition (bulk clays and <2 μm fractions after heating at 300–500°C and ethylene glycol solvation). Further analyses were conducted to determine the size distribution, chemical composition and physical properties of test bodies derived from these clays. The in situ weathered schist forming the primary micaceous red clays which are suitable for local pottery production are characterized by large muscovite-sericite-illite and small calcite contents. In contrast, the Bardakçı clays are dominated by large smectite contents and are only used sparingly in mixtures of local pottery production because they undergo firing shrinkage and present drying and firing flaws in the fired bodies. Firing ranges of ~800–900°C were inferred from the mineralogy and colours of the two ancient sherds from Kutki. As a result of mineralogical analysis of fired and unfired test bodies of these pottery clays and pot sherds, two different types of pastes were determined for pottery production in the Lake Van region: metamorphic and volcanic paste, the former characterized by a calcite-poor and mica-sericite-rich matrix and the latter by large smectite and small calcite contents.


2014 ◽  
Vol 70 (a1) ◽  
pp. C554-C554 ◽  
Author(s):  
Purnendu Nandy ◽  
V. Pedireddi

Molecular adducts of 5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin (1) with aza-donors like 4,4'-bipyridine (a), 1,2-bis(4-pyridyl)ethane (b), trans-1,2-bis(4-pyridyl)ethylene (c), 4,4'-trimethylene-dipyridine (d), phenazine (e), 1,10-phenanthroline (f), 1,7-phenanthroline (g) and 4,7-phenanthroline (h) have been prepared. All the molecular complexes are crystallized along with the solvent of crystallization, except in the complex with the aza-donor b. Detailed structural analysis of the obtained complexes has been carried out by single crystal X-ray diffraction. The three dimensional structures of the molecular adducts are facilitated by directional hydrogen bonding features of hydroxyl groups with aza donors as well as solvent molecules, leading to the formation of different types of supramolecular architectures like sheets, tapes, host-guest assembly etc. For example, in the complex of 1 and aza donor a, which crystallizes as a hydrate, the porphyrin molecules interact with water and 4,4'-bipyridine through O-H...O and O-H...N hydrogen bonds, which leads to the formation of molecular sheets in two dimensional arrangement. An important noteworthy observation is that the molecular complexes are crystalline even after removal of the solvents by heating, as characterized by thermogravimetric analysis (TGA) and powder X-ray diffraction (PXRD). Further, all the complexes are found to be fluorescence sensitive, perhaps due to the porphyrin molecules.


2013 ◽  
Vol 1617 ◽  
pp. 43-48
Author(s):  
R. Cisneros Tamayo ◽  
I.J. Gerrero Moreno ◽  
A. Vivas Hernandez ◽  
J.L. Casas Espinola ◽  
L. Shcherbyna

ABSTRACTThe photoluminescence (PL), its temperature dependence and X-ray diffraction (XRD) have been studied in MBE grown GaAs/AlGaAs/InGaAs/AlGaAs /GaAs quantum wells (QWs) with InAs quantum dots embedded in the center of InGaAs layer in the freshly prepared states and after the thermal treatments during 2 hours at 640 or 710 °C. The structures contained two buffer (Al0.3Ga0.7As/In0.15Ga0.85As) and two capping (In0.15Ga0.85As / Al0.3Ga0.7As) layers. The temperature dependences of PL peak positions have been analyzed in the temperature range 10-500K with the aim to investigate the QD composition and its variation at thermal annealing. The experimental parameters of the temperature variation of PL peak position in the InAs QDs have been compared with the known one for the bulk InAs crystals and the QD composition variation due to Ga/Al/In inter diffusion at thermal treatments has been detected. XRD have been studied with the aim to estimate the capping/buffer layer compositions in the different QW layers in freshly prepared state and after the thermal annealing. The obtained emission and XRD data and their dependences on the thermal treatment have been analyzed and discussed.


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