scholarly journals SYNTHESIS OF COCRYSTALS OF BETULIN WITH SUBERIC ACID AND STUDY OF THEIR PROPERTIES

2021 ◽  
pp. 183-192
Author(s):  
Anastasiya Vital'yevna Mikhailovskaya ◽  
Svetlana Anatol'yevna Myz ◽  
Konstantin Borisovich Gerasimov ◽  
Svetlana Alekseyevna Kuznetsova ◽  
Tat'yana Petrovna Shakhtshneider
Keyword(s):  
Aqueous Media ◽  
Aliphatic Acid ◽  
Suberic Acid ◽  
X Ray Diffraction ◽  
Lupane Triterpenoids ◽  
Pharmaceutical Ingredients ◽  
Grinding Method ◽  
Rate Of Dissolution ◽  
Wide Range ◽  
Acid Melts

Lupane triterpenoids, betulin and its derivatives, are attracting great interest due to their wide range of biological and pharmacological activities. However, the poor solubility of betulin and its derivatives in aqueous media significantly reduces their bioavailability. Obtaining cocrystals, that is, multicomponent crystal systems containing active pharmaceutical ingredients and non-toxic partner molecules in their structure, is used in pharmacy to change the physicochemical properties of drugs, including the rate of dissolution and solubility. In this study, cocrystals of betulin with suberic acid were obtained by liquid-assisted grinding method using organic solvents of different polarity: ethanol, acetone, ethyl acetate, chloroform, toluene, dioxane. The formation of cocrystals was confirmed by X-ray diffraction analysis, IR spectroscopy, and thermal analysis. It has been shown that cocrystals of betulin with suberic acid contain water molecules in their structure; anhydrous cocrystals can be obtained by heating a physical mixture of reagents until the acid melts. The results of experiments on the dissolution of cocrystals of betulin with suberic acid in comparison with the data for cocrystals of betulin with adipic acid showed that an increase in the length of the aliphatic acid chain leads to a decrease in the rate of betulin release into solution.

scholarly journals Charge Compensation in Europium-Doped Hafnia Nanoparticles: Solvothermal Synthesis and Colloidal Dispersion

Crystals ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1042
Author(s):  
Xavier H. Guichard ◽  
Francesco Bernasconi ◽  
Alessandro Lauria
Keyword(s):  
Low Temperature ◽  
Hafnium Oxide ◽  
Aqueous Media ◽  
Charge Compensation ◽  
Colloidal Dispersion ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Direct Formation ◽  
Enhanced Luminescence

Effective charge compensation of europium in hafnium oxide nanoparticles was achieved at low temperature, allowing high doping incorporation (up to 6 at.%) and enhanced luminescence. The efficiency of the incorporation and charge compensation was confirmed by scanning electron microscope energy dispersive X-ray spectroscopy and powder X-ray diffraction measurements. Despite the known polymorphism of hafnium oxide, when doped to a concentration above 3 at.%, only the pure monoclinic phase was observed up to 6 at.% of europium. Furthermore, the low-temperature solvothermal route allowed the direct formation of stable dispersions of the synthesized material over a wide range of concentrations in aqueous media. The dispersions were studied by diffuse light scattering (DLS) to evaluate their quality and by photoluminescence to investigate the incorporation of the dopants into the lattice.

scholarly journals Сocrystals of betulin with suberic acid: mechanochemical synthesis and thermal behavior

2021 ◽  
Vol 340 ◽  
pp. 01019
Author(s):  
Anastasiya Mikhailovskaya ◽  
Svetlana Myz ◽  
Konstantin Gerasimov ◽  
Svetlana Kuznetsova ◽  
Tatyana Shakhtshneider
Keyword(s):  
Thermal Analysis ◽  
Ir Spectroscopy ◽  
Thermal Behavior ◽  
Structural Transformation ◽  
Mechanochemical Synthesis ◽  
Water Removal ◽  
Suberic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grinding Method

In this work, the cocrystals of betulin with suberic acid were prepared by liquid-assisted grinding method using solvents of different polarity. The formation of cocrystals was confirmed by means of powder X-ray diffraction, IR spectroscopy and thermal analysis. It was shown that under heating, a structural transformation occurred after water removal, followed by cocrystal dissociation.

scholarly journals Removal of Zinc Ions Using Hydroxyapatite and Study of Ultrasound Behavior of Aqueous Media

Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1350 ◽  
Author(s):  
Simona Iconaru ◽  
Mikael Motelica-Heino ◽  
Régis Guegan ◽  
Mihai Predoi ◽  
Alina Prodan ◽  
...  
Keyword(s):  
Aqueous Solutions ◽  
Aqueous Media ◽  
Zinc Ions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Wide Range ◽  
Ultrasonic Measurements ◽  
Ultrasonic Conditions ◽  
Langmuir And Freundlich Models

The present study demonstrates the effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions. The synthesized hydroxyapatites before (HAp) and after the adsorption of zinc (at a concentration of 50 mg/L) in solution (HApD) were characterized using X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM, respectively). The effectiveness of hydroxyapatite nanopowders in the adsorption of zinc in aqueous solutions was stressed out through ultrasonic measurements. Both Langmuir and Freundlich models properly fitted on a wide range of concentration the equilibrium adsorption isotherms, allowing us to precisely quantify the affinity of zinc to hydroxyapatite nanopowders and to probe the efficacy of hydroxyapatite in removal of zinc ions from aqueous solutions in ultrasonic conditions.

Self-Recognizing π-π Stacking Interactions Designed for the Generation of Ultrastable Mesoporous Hydrogen-Bonded Organic Frameworks

2019 ◽  
Author(s):  
KAIKAI MA ◽  
Peng Li ◽  
John Xin ◽  
Yongwei Chen ◽  
Zhijie Chen ◽  
...  
Keyword(s):  
Pore Size ◽  
Fiber Composite ◽  
Aqueous Media ◽  
Stacking Interactions ◽  
Mustard Gas ◽  
X Ray Diffraction ◽  
X Ray ◽  
Expansion Strategy ◽  
Π Stacking ◽  
Hydrogen Bonded

Creating crystalline porous materials with large pores is typically challenging due to undesired interpen-etration, staggered stacking, or weakened framework stability. Here, we report a pore size expansion strategy by self-recognizing π-π stacking interactions in a series of two-dimensional (2D) hydrogen–bonded organic frameworks (HOFs), HOF-10x (x=0,1,2), self-assembled from pyrene-based tectons with systematic elongation of π-conjugated molecular arms. This strategy successfully avoids interpene-tration or staggered stacking and expands the pore size of HOF materials to access mesoporous HOF-102, which features a surface area of ~ 2,500 m2/g and the largest pore volume (1.3 cm3/g) to date among all reported HOFs. More importantly, HOF-102 shows significantly enhanced thermal and chemical stability as evidenced by powder x-ray diffraction and N2 isotherms after treatments in chal-lenging conditions. Such stability enables the adsorption of dyes and cytochrome c from aqueous media by HOF-102 and affords a processible HOF-102/fiber composite for the efficient photochemical detox-ification of a mustard gas simulant.

Evaluation of the accuracy indicators in determination of the coating thickness by crater grinding method

2020 ◽  
Vol 86 (7) ◽  
pp. 39-44
Author(s):  
K. V. Gogolinsky ◽  
A. E. Ivkin ◽  
V. V. Alekhnovich ◽  
A. Yu. Vasiliev ◽  
A. E. Tyurnina ◽  
...  
Keyword(s):  
Coating Thickness ◽  
Functional Dependence ◽  
Measurement Procedure ◽  
Metrological Certification ◽  
Measuring Instruments ◽  
Properties Of Coatings ◽  
Special Equipment ◽  
Grinding Method ◽  
Accuracy Of Measurements ◽  
Wide Range

Thickness is one of the key indicators characterizing the quality and functional properties of coatings. Various indirect methods (electromagnetic, radiation, optical) most often used in practice to measure thickness are based on the functional dependence of a particular physical parameter of the system «base – coating» on the coating thickness. The sensitivity of these procedures to the certain properties of coatings imposes the main restriction to the accuracy of measurements. Therefore, the development and implementation of the approaches based on direct measurements of geometric parameters of the coating appears expedient. These methods often belong to the class of «destructive» and, in addition to measuring instruments, require the use of special equipment. To ensure the uniformity of measurements in the laboratory or technological control, these methods are isolated as a separate procedure (method) and must undergo metrological certification in accordance with GOST R 8.563–2009. We present implementation, metrological certification and practical application of the method for measuring thickness of coatings by crater-grinding method. The principles of technical implementation of test equipment, measurement procedure and calculation formulas are described. The results of evaluating the accuracy indicators of the proposed procedure by calculation and experimental methods are presented. In both cases, the relative error did not exceed 6%. The applicability of the developed technique is shown for a wide range of coating materials (from soft metals to superhard ceramics) of different thickness (with from units to hundreds of micrometers). Apart from the goals of process control and outgoing inspection, the method can be recommended as a reference measurement procedure for calibration of measures and adjusting samples for various types of thickness gauges.

scholarly journals Relationship between the Stereocomplex Crystallization Behavior and Mechanical Properties of PLLA/PDLA Blends

Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1851
Author(s):  
Hye-Seon Park ◽  
Chang-Kook Hong
Keyword(s):  
Mechanical Properties ◽  
Lactic Acid ◽  
Crystallization Behavior ◽  
Mechanical Analysis ◽  
X Ray Diffraction ◽  
Nucleation Agent ◽  
Scanning Calorimetry ◽  
Nucleation Sites ◽  
Wide Range ◽  
Degree Of Crystallization

Poly (l-lactic acid) (PLLA) is a promising biomedical polymer material with a wide range of applications. The diverse enantiomeric forms of PLLA provide great opportunities for thermal and mechanical enhancement through stereocomplex formation. The addition of poly (d-lactic acid) (PDLA) as a nucleation agent and the formation of stereocomplex crystallization (SC) have been proven to be an effective method to improve the crystallization and mechanical properties of the PLLA. In this study, PLLA was blended with different amounts of PDLA through a melt blending process and their properties were calculated. The effect of the PDLA on the crystallization behavior, thermal, and mechanical properties of PLLA were investigated systematically by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), polarized optical microscopy (POM), dynamic mechanical analysis (DMA), and tensile test. Based on our findings, SC formed easily when PDLA content was increased, and acts as nucleation sites. Both SC and homo crystals (HC) were observed in the PLLA/PDLA blends. As the content of PDLA increased, the degree of crystallization increased, and the mechanical strength also increased.

scholarly journals Multidimensional Ln-Aminophthalate Photoluminescent Coordination Polymers

Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1786
Author(s):  
Carla Queirós ◽  
Chen Sun ◽  
Ana M. G. Silva ◽  
Baltazar de Castro ◽  
Juan Cabanillas-Gonzalez ◽  
...  
Keyword(s):  
Water Content ◽  
Coordination Polymers ◽  
Metal Ion ◽  
Low Cost ◽  
Microwave Assisted Synthesis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

The development of straightforward reproducible methods for the preparation of new photoluminescent coordination polymers (CPs) is an important goal in luminescence and chemical sensing fields. Isophthalic acid derivatives have been reported for a wide range of applications, and in addition to their relatively low cost, have encouraged its use in the preparation of novel lanthanide-based coordination polymers (LnCPs). Considering that the photoluminescent properties of these CPs are highly dependent on the existence of water molecules in the crystal structure, our research efforts are now focused on the preparation of CP with the lowest water content possible, while considering a green chemistry approach. One- and two-dimensional (1D and 2D) LnCPs were prepared from 5-aminoisophthalic acid and Sm3+/Tb3+ using hydrothermal and/or microwave-assisted synthesis. The unprecedented LnCPs were characterized by single-crystal X-ray diffraction (SCRXD), powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM), and their photoluminescence (PL) properties were studied in the solid state, at room temperature, using the CPs as powders and encapsulated in poly(methyl methacrylate (PMMA) films, envisaging the potential preparation of devices for sensing. The materials revealed interesting PL properties that depend on the dimensionality, metal ion, co-ligand used and water content.

Synthesis and Characterization of Lanthanide Metal-Organic Frameworks with Perfluorinated Linkers

2016 ◽  
Vol 98 ◽  
pp. 70-74
Author(s):  
Andrius Laurikėnas ◽  
Jurgis Barkauskas ◽  
Aivaras Kareiva
Keyword(s):  
Metal Organic Frameworks ◽  
Aqueous Media ◽  
Xrd Analysis ◽  
X Ray Diffraction ◽  
Lanthanide Elements ◽  
Diffusion Controlled ◽  
Benzenedicarboxylic Acid ◽  
Metal Organic ◽  
Lanthanide Metal

In this study, lanthanide elements (Ln3+) and 2,3,5,6-tetrafluoro-1,4-benzenedicarboxylic acid (TFBDC) based metal-organic frameworks (MOFs) were synthesized by precipitation and diffusion-controlled precipitation methods. Powders insoluble in aqueous media and polar solvents were obtained. The microstructure and properties of Ln3+ MOFs were evaluated and discussed. X-ray diffraction (XRD) analysis, infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and fluorescence spectroscopy (FLS) were carried out to characterize Ln3+ MOF's crystallinity, the microstructure, chemical composition and optical properties.

scholarly journals Ureido Functionalization through Amine-Urea Transamidation under Mild Reaction Conditions

Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1583
Author(s):  
Natalia Guerrero-Alburquerque ◽  
Shanyu Zhao ◽  
Daniel Rentsch ◽  
Matthias M. Koebel ◽  
Marco Lattuada ◽  
...  
Keyword(s):  
Aqueous Media ◽  
Reaction Times ◽  
Reaction Rates ◽  
Secondary Amines ◽  
Isocyanic Acid ◽  
Advantages And Disadvantages ◽  
Major Disadvantage ◽  
Wide Range ◽  
Potential Alternative ◽  
Full Conversion

Ureido-functionalized compounds play an indispensable role in important biochemical processes, as well as chemical synthesis and production. Isocyanates, and KOCN in particular, are the preferred reagents for the ureido functionalization of amine-bearing compounds. In this study, we evaluate the potential of urea as a reagent to graft ureido groups onto amines at relatively low temperatures (<100 °C) in aqueous media. Urea is an inexpensive, non-toxic and biocompatible potential alternative to KOCN for ureido functionalization. From as early as 1864, urea was the go-to reagent for polyurea polycondensation, before falling into disuse after the advent of isocyanate chemistry. We systematically re-investigate the advantages and disadvantages of urea for amine transamidation. High ureido-functionalization conversion was obtained for a wide range of substrates, including primary and secondary amines and amino acids. Reaction times are nearly independent of substrate and pH, but excess urea is required for practically feasible reaction rates. Near full conversion of amines into ureido can be achieved within 10 h at 90 °C and within 24 h at 80 °C, and much slower reaction rates were determined at lower temperatures. The importance of the urea/amine ratio and the temperature dependence of the reaction rates indicate that urea decomposition into an isocyanic acid or a carbamate intermediate is the rate-limiting step. The presence of water leads to a modest increase in reaction rates, but the full conversion of amino groups into ureido groups is also possible in the absence of water in neat alcohol, consistent with a reaction mechanism mediated by an isocyanic acid intermediate (where the water assists in the proton transfer). Hence, the reaction with urea avoids the use of toxic isocyanate reagents by in situ generation of the reactive isocyanate intermediate, but the requirement to separate the excess urea from the reaction product remains a major disadvantage.

2D X-ray diffraction and molecular modelling of the crystalline structure of polyesters under uniaxial stress

2021 ◽  
pp. 096739112199822
Author(s):  
Ahmed I Abou-Kandil ◽  
Gerhard Goldbeck
Keyword(s):  
Crystalline Structure ◽  
Molecular Modelling ◽  
Three Dimensional ◽  
Uniaxial Stress ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Modelling Techniques ◽  
Diffraction Patterns

Studying the crystalline structure of uniaxially and biaxially drawn polyesters is of great importance due to their wide range of applications. In this study, we shed some light on the behaviour of PET and PEN under uniaxial stress using experimental and molecular modelling techniques. Comparing experiment with modelling provides insights into polymer crystallisation with extended chains. Experimental x-ray diffraction patterns are reproduced by means of models of chains sliding along the c-axis leading to some loss of three-dimensional order, i.e. moving away from the condition of perfect register of the fully extended chains in triclinic crystals of both PET and PEN. This will help us understand the mechanism of polymer crystallisation under uniaxial stress and the appearance of mesophases in some cases as discussed herein.

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