scholarly journals Synthesis, Composition and Structure of Complexes of Dialyzed Collagen With CuSO4

2021 ◽  
Author(s):  
Adham Rafikov ◽  
Dildora Sadikova ◽  
Oybek Tursunkulov ◽  
Malika Zubaydullaeva
Keyword(s):  
Phase Analysis ◽  
Salt Content ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Textile Materials ◽  
Composition And Structure ◽  
Ft Ir ◽  
Almost All ◽  
Synthesis Composition ◽  
Ft Ir Spectroscopy

Abstract Coordination complexes of collagen with copper (II) sulfate were synthesized at different ratios of the starting materials. For the synthesis, a collagen solution was used, isolated from the skin of cattle, and then freed from electrolytes by dialysis. With an increase in the salt content, the yield of the reaction product increases. The composition and structure of the complex were determined by FT-IR spectroscopy, SEM, X-ray phase analysis, and differential scanning calorimetry. The complex is formed due to the coordination interaction of with the nitrogen and oxygen atom of collagen and water. An inadequate change in the composition of the complexes with a change in the initial ratio of the components was found. With an excess of collagen, some of it does not bind into a complex and precipitates. With an excess of salt, almost all of the collagen is bound into a complex and a rhombic single crystal is formed. The composition of the complex changes not due to a change in the coordination number , but due to an increase in the amount of these ions. An X-ray phase analysis of the starting materials and complexes has been carried out. The correspondence of the parameters of the crystal structure in the X-ray spectra of the complexes was found for a wide ratio of the starting materials. The synthesized complexes have been successfully used for dyeing textile materials.

scholarly journals Inclusion of the Phytoalexin trans-Resveratrol in Native Cyclodextrins: A Thermal, Spectroscopic, and X-Ray Structural Study

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 998 ◽  
Author(s):  
Laura Catenacci ◽  
Milena Sorrenti ◽  
Maria Cristina Bonferoni ◽  
Lee Hunt ◽  
Mino R. Caira
Keyword(s):  
Inclusion Complexation ◽  
Exothermic Effect ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Physical Mixing ◽  
Ft Ir ◽  
Co Precipitation ◽  
Ft Ir Spectroscopy ◽  
Severe Disorder

The aim of the study was to determine the feasibility of complexation between the antioxidant trans-resveratrol (RSV) and underivatized cyclodextrins (CDs) using a variety of preparative methods, including physical mixing, kneading, microwave irradiation, co-evaporation, and co-precipitation techniques. Products were characterized using differential scanning calorimetry (DSC), simultaneous thermogravimetric/DSC analysis (TGA/DSC), Fourier transform infrared (FT-IR) spectroscopy, and powder X-ray diffraction (PXRD). With α-CD and RSV, sample amorphization was revealed by PXRD and FT-IR, but no definitive inclusion complexation was evident. Similar results were obtained in attempts to complex RSV with β-CD. However, complex formation between γ-CD and RSV was evident from observation of an endo-/exothermic effect appearing in the DSC trace of the product from kneading and was further corroborated by FT-IR and PXRD methods. The latter technique indicated complexation unequivocally as the diffraction peak profile for the product matched that for known isostructural γ-CD complexes. Single crystal X-ray analysis followed, confirming the predicted complex between γ-CD and RSV. A combination of 1H NMR and TGA data yielded the complex formula (γ-CD)3·(RSV)4·(H2O)62. However, severe disorder of the RSV molecules prevented their modeling. In contrast, our previous studies of the inclusion of RSV in methylated CDs yielded crystals with only minor guest disorder.

Mechanochemical synthesis insights and solid-state characterization of quininium aspirinate, a glass-forming drug–drug salt

2021 ◽  
Vol 77 (9) ◽  
Author(s):  
Nehemiah Harris ◽  
Jubilee Benedict ◽  
Diane A. Dickie ◽  
Silvina Pagola
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Ir Spectroscopy ◽  
Mechanochemical Synthesis ◽  
Mechanochemical Reaction ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Quinine (an antimalarial) and aspirin (a nonsteroidal anti-inflammatory drug) were combined into a new drug–drug salt, quininium aspirinate, C20H25N2O2 +·C9H7O4 −, by liquid-assisted grinding using stoichiometric amounts of the reactants in a 1:1 molar ratio, and water, EtOH, toluene, or heptane as additives. A tetrahydrofuran (THF) solution of the mechanochemical product prepared using EtOH as additive led to a single crystal of the same material obtained by mechanochemistry, which was used for crystal structure determination at 100 K. Powder X-ray diffraction ruled out crystallographic phase transitions in the 100–295 K interval. Neat mechanical treatment (in a mortar and pestle, or in a ball mill at 20 or 30 Hz milling frequencies) gave rise to an amorphous phase, as shown by powder X-ray diffraction; however, FT–IR spectroscopy unambiguously indicates that a mechanochemical reaction has occurred. Neat milling the reactants at 10 and 15 Hz led to incomplete reactions. Thermogravimetry and differential scanning calorimetry indicate that the amorphous and crystalline mechanochemical products form glasses/supercooled liquids before melting, and do not recrystallize upon cooling. However, the amorphous material obtained by neat grinding crystallizes upon storage into the salt reported. The mechanochemical synthesis, crystal structure analysis, Hirshfeld surfaces, powder X-ray diffraction, thermogravimetry, differential scanning calorimetry, FT–IR spectroscopy, and aqueous solubility of quininium aspirinate are herein reported.

scholarly journals Nematic Phase Induced from Symmetrical Supramolecular H-Bonded Systems Based on Flexible Acid Core

Crystals ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 801 ◽  
Author(s):  
Hoda A. Ahmed ◽  
Muna S. Khushaim
Keyword(s):  
Uv Spectroscopy ◽  
X Ray Diffraction ◽  
Terminal Complex ◽  
Scanning Calorimetry ◽  
Xrd Pattern ◽  
X Ray ◽  
Smectic A ◽  
Ft Ir ◽  
Nematic Phases ◽  
Ft Ir Spectroscopy

New symmetrical 1:2 supramolecular H-bonded liquid crystals (SMHBLCs) interactions, A/2Bn, were formed between adipic acid and 4-(4′–pyridylazophenyl) 4″-alkoxybenzoates. Optical and mesomorphic behaviors of the prepared SMHBLC complexes were investigated using differential scanning calorimetry (DSC), polarizing optical microscopy (POM) and X-ray diffraction (XRD). FT-IR spectroscopy was carried out to confirm the H-bond interactions of the prepared complexes via Fermi bands formation. Their photo-physical properties were investigated by UV-spectroscopy and the observed absorbance values were found to be mainly dependent on the length of the terminal alkoxy chain. Mesomorphic behaviour for all A/2Bn complexes revealed that all complexes are dimorphic-exhibiting enantiotropic mesophases with induced nematic phases, except for the long chain terminal complex which exhibits only a monomorphic smectic A phase. In order to investigate the effect of mesogenic core geometry on the mesophase properties, a comparison was established between the mesomeric behaviors of the present complexes and previously reported rigid core acid complexes. Finally, the XRD pattern confirmed the POM and DSC results.

scholarly journals Preparation and Characterization of Cetyl Trimethylammonium Intercalated Sericite

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Hao Ding ◽  
Yuebo Wang ◽  
Yu Liang ◽  
Faxiang Qin
Keyword(s):  
Ion Exchange ◽  
Interlayer Space ◽  
Xrd Analysis ◽  
Acid Activation ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Intercalated sericite was prepared by intercalation of cetyl trimethylammonium bromide (CTAB) into activated sericite through ion exchange with the following two steps: the activation of sericite by thermal modification, acid activation and sodium modification; the ion exchange intercalation of CTA+into activated sericite. Effects of reaction time, reaction temperature, CTAB quantity, kinds of medium, and aqueous pH on the intercalation of activated sericite were examined by X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). The results indicated that the CTA+entered sericite interlayers and anchored in the aluminosilicate interlayers through strong electrostatic attraction. The arrangement of CTA+in sericite interlayers was that alkyl chain of CTA+mainly tilted at an angle about 60° (paraffin-type bilayer) and 38° (paraffin-type monolayer) with aluminosilicate layers. The largest interlayer space was enlarged from 0.9 nm to 5.2 nm. The intercalated sericite could be used as an excellent layer silicate to prepare clay-polymer nanocomposites.

scholarly journals Nematogenic Laterally Substituted Supramolecular H-Bonded Complexes Based on Flexible Core

Crystals ◽  
2020 ◽  
Vol 10 (10) ◽  
pp. 878 ◽  
Author(s):  
H.A. Ahmed ◽  
Muna S. Khushaim
Keyword(s):  
Uv Spectroscopy ◽  
Supramolecular Complexes ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Xrd Pattern ◽  
X Ray ◽  
Ft Ir ◽  
Chain Lengths ◽  
Flexible Core ◽  
Ft Ir Spectroscopy

New laterally CH3-substituted series of 1:2 hydrogen-bonded supramolecular complexes (HBSMCs) based on flexible acid core were prepared and mesomorphically investigated. Mixtures were formed through H-bonded interactions between adipic acid (A) and 4-(2-(pyridin-4-yl)diazenyl-(3-methylphenyl) 4-alkoxybenzoate (Bn). Mesomorphic and optical properties were investigated by differential scanning calorimetry (DSC), polarized optical microscopy (POM), X-ray diffraction (XRD), and UV-spectroscopy. HBSMCs formed from 1:2 mol mixture of A:2Bn, where the base component (B) bearing different alkoxy chain lengths from n = 8 to 14. The new HBSMCs (A/2B) interactions were confirmed by Fermi-bands formation via FT-IR spectroscopy measurements. Results revealed that all prepared HBSMCs are enantiotropic, exhibiting induced nematic (N) phase. The XRD pattern confirmed the POM texture results. Moreover, a comparison was made between the new laterally HBSMC series based on flexible core and the previously analyzed laterally neat complexes.

Thermal Behaviour of Candesartan Active substance and in pharmaceutical compounds

2017 ◽  
Vol 68 (8) ◽  
pp. 1895-1902
Author(s):  
Ioana Cristina Tita ◽  
Eleonora Marian ◽  
Bogdan Tita ◽  
Claudia Crina Toma ◽  
Laura Vicas
Keyword(s):  
Thermal Behaviour ◽  
Active Substance ◽  
Pharmaceutical Research ◽  
Pharmaceutical Product ◽  
Nitrogen Atmosphere ◽  
Pure Substance ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ft Ir

Thermal analysis is one of the most frequently used instrumental techniques in the pharmaceutical research, for the thermal characterization of different materials from solids to semi-solids, which are of pharmaceutical relevance. In this paper, simultaneous thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) were used for characterization of the thermal behaviour of candesartan cilexetil � active substance (C-AS) under dynamic nitrogen atmosphere and nonisothermal conditions, in comparison with pharmaceutical product containing the corresponding active substance. It was observed that the commercial samples showed a different thermal profile than the standard sample, caused by the presence of excipients in the pharmaceutical product and to possible interaction of these with the active substance. The Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) were used as complementary techniques adequately implement and assist in interpretation of the thermal results. The main conclusion of this comparative study was that the TG/DTG and DSC curves, together with the FT-IR spectra, respectively X-ray difractograms constitute believe data for the discrimination between the pure substance and pharmaceutical forms.

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.

scholarly journals Incorporation of silver stearate nanoparticles in methacrylate polymeric monoliths for hemeprotein isolation

2020 ◽  
Vol 18 (1) ◽  
pp. 399-411
Author(s):  
Eman Alzahrani
Keyword(s):  
Noble Metals ◽  
Extraction Process ◽  
Sem Analysis ◽  
X Ray ◽  
Polymeric Scaffold ◽  
Extended Surface ◽  
Unique Method ◽  
Unique Approach ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

AbstractA unique method was used to synthesize extremely stable silver stearate nanoparticles (AgStNPs) incorporated in an organic-based monolith. The facile strategy was then used to selectively isolate hemeproteins, myoglobin (Myo) and hemoglobin (Hb). Ethyl alcohol, silver nitrate, and stearic acid were, respectively, utilized as reducing agents, silver precursors, and capping agents. The color changed to cloudy from transparent, indicating that AgStNPs had been formed. AgStNP nanostructures were then distinctly integrated into the natural polymeric scaffold. To characterize the AgStNP–methacrylate polymeric monolith and the silver nanoparticles, energy-dispersive X-ray (EDX), scanning electron microscopy (SEM), and Fourier-transform infrared (FT-IR) spectroscopy were used. The results of the SEM analysis indicated that the AgStNP–methacrylate polymeric monolith’s texture was so rough in comparison with that of the methacrylate polymeric monolith, indicating that the extraction process of the monolith materials would be more efficient because of the extended surface area of the absorbent. The comparison between the FT-IR spectra of AgStNPs, the bare organic monolith, and AgStNP–methacrylate polymeric monolith confirms that the AgStNPs were immobilized on the surface of the organic monolith. The EDX profile of the built materials indicated an advanced peak of the Ag sequence which represented an Ag atom of 3.27%. The results therefore established that the AgStNPs had been successfully integrated into the monolithic materials. Extraction efficiencies of 92% and 97% were used to, respectively, recover preconcentrated Myo and Hb. An uncomplicated method is a unique approach of both fabrication and utilization of the nanosorbent to selectively isolate hemeproteins. The process can further be implemented by using other noble metals.

Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi
Keyword(s):  
Liquid Crystalline ◽  
Spectroscopic Method ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
Scanning Calorimetry ◽  
Polar Solvents ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.

Synthesis and Properties of Thermotropic Liquid Crystalline Polyesters with Flexible Polymethylene Spacer

2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao
Keyword(s):  
Optical Microscopy ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Structure Morphology ◽  
Temperature Ranges ◽  
Ft Ir ◽  
Diffraction Peaks ◽  
Ubbelohde Viscometer

Polymethylene bis(p-hydroxybenzoates) were prepared from methyl p-hydroxybenzoate and different diols by melted transesterification reaction. Three liquid crystalline polyesters were synthesized from terephthaloyl dichloride and polymethylene bis(p-hydroxybenzoates). Its structure, morphology and properties were characterized by Ubbelohde viscometer, Fourier transform infrared spectroscopy (FT-IR), Differential scanning calorimetry (DSC), polarized optical microscopy (POM) with a hot stage, and wide-angle X-ray diffraction (WAXD). Results indicated that the intrinsic viscosities were between 0.088 and 0.210 dL/g. Optical microscopy showed that the TLCP has a highly threaded liquid crystalline texture and a high birefringent schlieren texture character of nematic phase and has wider mesophase temperature ranges for all polyesters. DSC analysis were found that the melting point (Tm), isotropic temperature (Ti) of TLCPs decreased and the temperature range of the liquid crystalline phase became wider with increased number of methylene spacers in the polyester. The WAXD results showed that TLCPs owned two strong diffraction peaks at 2θ near 19° and 23°.

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