crystallization procedure
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Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1355
Author(s):  
Giuseppe Cirillo ◽  
Elvira Pantuso ◽  
Manuela Curcio ◽  
Orazio Vittorio ◽  
Antonella Leggio ◽  
...  

In this work, we combined electrically-conductive graphene oxide and a sodium alginate-caffeic acid conjugate, acting as a functional element, in an acrylate hydrogel network to obtain multifunctional materials designed to perform multiple tasks in biomedical research. The hybrid material was found to be well tolerated by human fibroblast lung cells (MRC-5) (viability higher than 94%) and able to modify its swelling properties upon application of an external electric field. Release experiments performed using lysozyme as the model drug, showed a pH and electro-responsive behavior, with higher release amounts and rated in physiological vs. acidic pH. Finally, the retainment of the antioxidant properties of caffeic acid upon conjugation and polymerization processes (Trolox equivalent antioxidant capacity values of 1.77 and 1.48, respectively) was used to quench the effect of hydrogen peroxide in a hydrogel-assisted lysozyme crystallization procedure.


2020 ◽  
Vol 33 (1) ◽  
Author(s):  
Yu Luo ◽  
Yidong Jiang ◽  
Pei Zhang ◽  
Xin Wang ◽  
Haibo Ke ◽  
...  

Abstract Zr-based Bulk metallic glasses exhibit incredible corrosion resistance and glass forming ability, however, these properties need further enhancement to meet the practical use. In this study, Zr63Fe2.5Cu23Al11.5, a new type of Zr-based bulk metallic glass was fabricated. Potentiodynamic polarization techniques were used to measure the corrosion resistance of this alloy. Furthermore, crystallization behavior and kinetics of Zr63Fe2.5Cu23Al11.5 bulk metallic glass were investigated by using differential scanning calorimetry of non-isothermal model. Kissinger and Ozawa methods were used for calculating activation energies of crystallization and the mechanism of crystallization was analyzed by Johnson-Mehl-Avrami-Kolmogorow methods. The results suggest that this specified metallic glass system possesses a relatively high thermal stability and glass forming ability. Moreover, the crystallization procedure is mainly dominated by nucleation with an increasing rate. The study demonstrates that the slight composition adjustment of Zr–Fe–Cu–Al system bulk metallic glass can make a considerable contribution to higher glass forming and thermal stability as well as corrosion resistance.


Pharmaceutics ◽  
2020 ◽  
Vol 12 (7) ◽  
pp. 648
Author(s):  
Patrycja Garbacz ◽  
Dominik Paukszta ◽  
Artur Sikorski ◽  
Marek Wesolowski

The low water solubility of benzodiazepines seriously affects their bioavailability and, in consequence, their biological activity. Since co-crystallization has been found to be a promising way to modify undesirable properties in active pharmaceutical ingredients, the objective of this study was to prepare co-crystals of two benzodiazepines, chlordiazepoxide and lorazepam. Using different co-crystallization procedures, slurry evaporation and liquid-assisted grinding, co-crystals of chlordiazepoxide with p-aminobenzoic acid and lorazepam with nicotinamide were prepared for the first time. Confirmation that co-crystals were obtained was achieved through a comparison of the data acquired for both co-crystals using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier-transform infrared (FTIR) and Raman spectroscopy, with comparisons acquired for the physical mixtures of both benzodiazepines and coformers. The compatibility of PXRD patterns of both benzodiazepines co-crystals with those contained in the base Powder Diffraction File (PDF-4+) suggests that new crystal structures were indeed created under the co-crystallization procedure. Single-crystal X-ray diffraction revealed that a chlordiazepoxide co-crystal with p-aminobenzoic acid and a lorazepam co-crystal with nicotinamide crystallized in the monoclinic P21/n and P21/c space group, respectively, with one molecule of benzodiazepine and one of coformer in the asymmetric unit. FTIR and Raman spectroscopy corroborated that benzodiazepine and coformer are linked by a hydrogen bond without proton exchange. Furthermore, a DSC study revealed that single endothermic DSC peaks assigned to the melting of co-crystals differ slightly depending on the co-crystallization procedures and solvent used, as well as differing from those of starting components.


Materials ◽  
2020 ◽  
Vol 13 (7) ◽  
pp. 1640 ◽  
Author(s):  
Jun Du ◽  
Yan Wang ◽  
Yan Wang ◽  
Ruifeng Li

Hierarchically porous ZSM-5 was prepared by utilizing a two-step crystallization procedure with carbon–silica composites as precursors. The hierarchically porous zeolites obtained a regular mesoporous structure with aluminum incorporated into the carbon–silica composite frameworks. The carbon–silica composite zeolites were characterized by XRD, TEM, SEM, and nitrogen adsorption/desorption. As-prepared hierarchical zeolites were used in the 1,3,5-triisopropylbenzene (TIPB) cracking reaction and exhibited significantly high TIPB conversion, while the accessibility factors were also determined.


Crystals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 201 ◽  
Author(s):  
Alexander A. Bredikhin ◽  
Dmitry V. Zakharychev ◽  
Zemfira A. Bredikhina ◽  
Alexey V. Kurenkov ◽  
Aida I. Samigullina ◽  
...  

Spontaneous resolution of Pasteur’s salt was historically the first way to obtain pure enantiomers from the racemate. The current increase in interest in the direct racemates resolution during crystallization is largely due to the opened prospects for the industrial application of this approach. The chiral 3-(3,4-dimethylphenoxy) propane-1,2-diol 1 is a synthetic precursor of practically useful amino alcohols, the enantiomers of which exhibit different biological effects. In this work, it was first discovered that racemic diol 1 is prone to spontaneous resolution. However, the crystallization process is complicated by the existence, along with the conglomerate, of two other crystalline forms. Using the differential scanning calorimetry (DSC) approach, methods have been developed to obtain individual metastable phases, and all identified modifications ((R)-1, (R+S)-1, α-rac-1, β-rac-1) were ranked by energy. The IR spectroscopy and powder X-ray diffraction (PXRD) methods demonstrated the identity of the first two forms and their proximity to the third, while β-rac-1 is significantly different from the rest. The crystal structure of the forms (R)-1 and α-rac-1 was established by the single crystal X-ray diffraction (SC-XRD) method. Preliminary information on the structure of β-rac-1 phase was obtained by the PXRD approach. Based on the information received, the experimental conditions for a successful direct resolution of racemic 1 into individual enantiomers by a preferential crystallization procedure were selected.


2020 ◽  
Vol 44 (4) ◽  
Author(s):  
G. V. Douniama‐Lönn ◽  
A. C. Ngakegni‐Limbili ◽  
R. Valentin ◽  
H. Nsamoto ◽  
M. Cerny ◽  
...  

RSC Advances ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 7301-7312 ◽  
Author(s):  
Afanasy V. Lunin ◽  
Ilya L. Sokolov ◽  
Ivan V. Zelepukin ◽  
Ilya V. Zubarev ◽  
Maria N. Yakovtseva ◽  
...  

Novel MRI active spindle-like nanoparticles prepared by a facile procedure display cytotoxicity due to synergistic combination of shape and europium content.


Nanomaterials ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 915 ◽  
Author(s):  
Lei Shi ◽  
Huiying Hao ◽  
Jingjing Dong ◽  
Tingting Zhong ◽  
Chen Zhang ◽  
...  

Intermediate phase is considered an important aspect to deeply understand the crystallization procedure in the growth of high-quality perovskite layers by an anti-solvent technique. However, the moisture influence on the intermediate phase formation is not clear in air conditions as yet. In this work, pure (FA0.2MA1.8)Pb3X8(DMSO·DMF) intermediate phase was obtained in as-prepared perovskite film by spin-coating the precursor of co-solvent (DMSO and DMF) in an ambient air (RH20–30%). Moreover, the appropriate quantity of ethyl acetate (C4H8O2, EA) also controls the formation of pure intermediate phase. The uniform and homogeneous perovskite film was obtained after annealing this intermediate film. Therefore, the best power conversion efficiency (PCE) of perovskite solar cells (PSCs) is 16.24% with an average PCE of 15.53%, of which almost 86% of its initial PCE was preserved after 30 days in air conditions. Besides, the steady-state output efficiency ups to 15.38% under continuous illumination. In addition, the PCE of large area device (100 mm2) reaches 11.11% with a little hysteresis effect. This work would give an orientation for PSCs production at the commercial level, which could lower the cost of fabricating the high efficiency PSCs.


2018 ◽  
Vol 74 (10) ◽  
pp. 1486-1490
Author(s):  
Igor Elkin ◽  
Thierry Maris ◽  
Patrice Hildgen ◽  
Christopher J. Barrett

cis-4,4′-(Diazenediyl)bis(2,3,5,6-tetrafluorobenzoic acid), C14H2F8N2O4, and its ethanol disolvate, C14H2F8N2O4·2C2H5OH, represent new examples of self-stabilized cis-configured azobenzenes obtained by a common crystallization procedure at room temperature under normal laboratory lighting conditions. The target structure constitutes of two 2,3,5,6-tetrafluorobenzoic acid residues linked to each other by a cis-configured azo group and was confirmed for two isolated specimens extracted from the same sample, corresponding to a solvent-free form and an ethanol disolvate. In the solvent-free form, the molecule is characterized by rotational symmetry around a twofold rotation axis bisecting its central N=N bond while this symmetry is not present in the solvated form. The values of the inclination angles of the terminal carboxyl groups towards the corresponding benzene rings vary from 5.2 (4) to 45.7 (2)°, depending on the crystal composition. In the unsolvated form, the molecules are linked through identical hydrogen bonds with a classical R 2 2(8) graph-set ring motif of carboxylic acids, by generating supramolecular chains running approximately parallel to [101]. The presence of ethanol in the solvated form also leads to changes in the short-contact pattern to produce both the R 4 4(12) ring and open-chain motifs with alternating alcohol and dicarboxylic acid molecules.


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