scholarly journals Structural, spectral and thermal properties of 2,2’-iminodipyridinium(+) trihydrogen pyromellitate

2014 ◽  
Vol 79 (6) ◽  
pp. 637-648
Author(s):  
Dejan Poleti ◽  
Jelena Rogan ◽  
Lidija Radovanovic ◽  
Marko Rodic

The title compound, (Hdipya)(H3pyr), where Hdipya is protonated 2,2?-dipyridilamine and H3pyr is monoanion of pyromellytic acid (H4pyr), was obtained from the reaction mixture containing Zn(II) ions, dipya, Na4pyr (the molar ratio 2 : 2 : 1) and HNO3. The products (micro- and single-crystalline) were characterized by X-ray structure determination, FT-IR spectroscopy and TG/DSC analysis. The most striking structural feature of (Hdipya)(H3pyr) are short inter- and extremely short intramolecular hydrogen bonds. These bonds mutually connect cations and anions making thin layers parallel to the crystallographic (223) plane. Also, quite unusual, linear proton-bound polymeric {H(H2pyr)-}n anions were identified in the structure. The results of crystal structure determination are compared with FT-IR and TG/DSC data. The low position of nas(COO) vibration at 1660 cm-1 is in accordance with strong hydrogen bonding. This value can be used as a measure of C=O bond order, which is calculated to be 1.81.

2016 ◽  
Vol 35 (5) ◽  
pp. 457-462 ◽  
Author(s):  
Mehdi Bazarganipour ◽  
Mahnaz Sahebi-Harandi ◽  
Masoud Salavati-Niasari

AbstractPosnjakite nanoparticles, Cu4SO4(OH)6 · H2O, were synthesized by utilizing a new thio-Schiff base ligand as new capping agent via a microwave approach. The effects of molar ratio, surfactants, heating time and microwave power on morphology of the product were investigated. The as-synthesized posnjakite nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and energy dispersive X-ray analysis (EDAX). The effects of different parameters such as the molar ratio, surfactants, microwave power and irradiation time on the morphology of the products were investigated. Moreover, adsorption of methylene orange dye on posnjakite nanoparticles was considered and the uptake percent was determined to be >65% in 200 min.


2005 ◽  
Vol 38 (5) ◽  
pp. 768-771 ◽  
Author(s):  
G. Bhagavannarayana ◽  
R. V. Ananthamurthy ◽  
G. C. Budakoti ◽  
B. Kumar ◽  
K. S. Bartwal

The annealing effect on the structural perfection of Fe-doped LiNbO3single crystals has been studied by high-resolution X-ray diffractometry (HRXRD), X-ray topography (XRT) and Fourier transform infrared (FT–IR) spectroscopy. The single crystals, prepared by mixing Li2CO3and Nb2O5powders in the molar ratio 48.6:51.4 with 0.05 mol% of iron at 1415 (1) K, were grown by the Czochralski (CZ) method along the [001] direction in air and poled during crystal growth by the application of a DC field. Two low-angle (tilt angle ∼1 arc minute) structural grain boundaries were observed in as-grown specimens. FT–IR spectra revealed that these crystals contain OH−and CO32−ionic defects. Grain boundaries and CO32−ionic defects were successfully removed, while the concentration of OH−ions was considerably reduced by post-growth thermal annealing at elevated temperatures.


Crystals ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 40
Author(s):  
Basanta Saikia ◽  
Andreas Seidel-Morgenstern ◽  
Heike Lorenz

Here, we report the synthesis and experimental characterization of three drug-drug eutectic mixtures of drug aminoglutethimide (AMG) with caffeine (CAF), nicotinamide (NIC) and ethenzamide (ZMD). The eutectic mixtures i.e., AMG-CAF (1:0.4, molar ratio), AMG-NIC (1:1.9, molar ratio) and AMG-ZMD (1:1.4, molar ratio) demonstrate significant melting point depressions ranging from 99.2 to 127.2 °C compared to the melting point of the drug AMG (151 °C) and also show moderately higher aqueous solubilities than that of the AMG. The results presented include the determination of the binary melt phase diagrams and accompanying analytical characterization via X-ray powder diffraction, FT-IR spectroscopy and scanning electron microscopy.


Author(s):  
Marina Tašner ◽  
Draginja Mrvoš-Sermek ◽  
Emina Hajdarpašić ◽  
Dubravka Matković-Čalogović

A new dinuclear paddle-wheel copper(II) complex with caffeine was synthesized by the solvent-based and mechanochemical methods from copper(II) acetate and caffeine in a 1:1 molar ratio. Mechanochemical synthesis was found to be the fastest and easiest way to prepare the complex. The reaction proceeds with addition of small amounts of methanol or ethanol. The complex was characterized by FT-IR spectroscopy, elemental and thermoanalytical methods (TG and DSC) and X-ray diffraction methods. The molecular and crystal structure was determined by the single crystal X-ray diffraction method. The complex molecule consists of a centrosymmetric dinuclear unit, Cu2(-Ac)4(caf)2, with two copper(II) atoms bridged by four acetato groups, and N-coordinated caffeine (caf) molecules in the apical posi-tions.


MRS Advances ◽  
2021 ◽  
Author(s):  
Axel T. Neffe ◽  
Candy Löwenberg ◽  
Andreas Lendlein

AbstractFunctionalization of gelatin with glycidylmethacrylate (GMA-gelatin) enables network formation employing the double bond, so that the reaction is orthogonal to the inherent functional groups in the biomacromolecule. Here, network formation by crosslinking of GMA-gelatin with hexane 1,6-dithiol or nonane 1,9-dithiol to tailor properties and enable a shape-memory effect is shown by 1H NMR and FT-IR spectroscopy. Hydrogel swelling (460–1900 vol%) and mechanical properties (Young’s modulus E = 59–512 kPa, elongation at break εb = 44–127%) depended on the molecular composition of the networks and temperature. Increased crosslinker length, thiol:methacrylate molar ratio, and precursor concentrations led to denser networks. Change of properties with temperature suggested adoption of triple helices by gelatin chains, forming physical netpoints at lower temperatures (< 20 °C). However, the limited freedom of the gelatin chains to move allowed only a minimal extent of triple helices formation, as it became apparent from the related signal in wide-angle X-ray scattering and the thermal transition associated to triple helices in some networks by DSC. The presented strategy is likely transferable to other biomacromolecules, and the results suggest that too short crosslinkers may result in a significant amount of grafting rather than network formation. Graphic abstract


Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1786
Author(s):  
Carla Queirós ◽  
Chen Sun ◽  
Ana M. G. Silva ◽  
Baltazar de Castro ◽  
Juan Cabanillas-Gonzalez ◽  
...  

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.


2020 ◽  
Vol 18 (1) ◽  
pp. 399-411
Author(s):  
Eman Alzahrani

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.


2018 ◽  
Vol 74 (3) ◽  
pp. 366-371 ◽  
Author(s):  
Wen Cui ◽  
Ruyu Wang ◽  
Xi Shu ◽  
Yu Fan ◽  
Yang Liu ◽  
...  

The interaction between the uranyl cation, (UO2)2+, and organic species is of interest due to the potential applications of the resulting compounds with regard to nuclear waste disposal and nuclear fuel reprocessing. The hydrothermal reaction of various uranyl compounds with flexible zwitterionic 1,1′-[1,4-phenylenebis(methylene)]bis(pyridin-1-ium-4-carboxylate) dihydrochloride (Bpmb·2HCl) in deionized water containing drops of H2SO4resulted in the formation of a novel two-dimensional uranyl coordination polymer, namely poly[tetraoxido{μ2-1,1′-[1,4-phenylenebis(methylene)]bis(pyridin-1-ium-4-carboxylate)}di-μ3-sulfato-diuranium(VI)], [(UO2)2(SO4)2(C20H16N2O4)]n, (1). Single-crystal X-ray diffraction reveals that this coordination polymer exhibits a layered arrangement and the (UO2)2+centre is coordinated by five equatorial O atoms. The structure was further characterized by FT–IR spectroscopy, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The polymer shows high thermal stability up to 696 K. Furthermore, the photoluminescence properties of (1) has also been studied, showing it to exhibit a typical uranyl fluorescence.


2017 ◽  
Author(s):  
◽  
Sharista Raghunath

The presence of dyes in effluent poses various environmental as well as health hazards for many organisms. Although various remediation strategies have been implemented to reduce their effect, dyes still manage to infiltrate into the environment and hence new strategies are required to address some of the problems. This study investigated the innovation of two cationic water-soluble polymers viz., Proline-Epichlorohydrin-Ethylenediamine Polymer (PEP) and Thiazolidine-Epichlorohydrin-Ethylenediamine Polymer (TEP) that were used to remediate selected synthetic dyes from synthetic effluent by adsorption and dye reduction. Both polymers were synthesized using monomers of a secondary amine, epichlorohydrin and ethylenediamine and were subsequently characterized and modified and their remediation potential studied. In the first study, PEP was synthesized and characterized by 1H-NMR Spectroscopy, FT-IR Spectroscopy, dynamic light scattering, and thermogravimetric analysis (TGA). Thereafter PEP was modified with bentonite clay, by simple mixing of the reactants, to form a Proline-Epichlorohydrin-Ethylenediamine Polymer-bentonite composite (PRO-BEN); it was characterized by FT-IR Spectroscopy, scanning electron microscopy (SEM)/ energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Adsorption studies were then undertaken with a synthetic effluent containing three textile dyes, viz., Reactive Blue 222 (RB 222), Reactive Red 195 (RR 195) and Reactive Yellow (RY 145). Various conditions were investigated including pH of the solution, temperature, sodium chloride concentration, initial dye concentration and the dosage of adsorbent used. The experimental data for all dyes followed a Langmuir isotherm. The adsorption process was found to be pseudo-second order. According to the thermodynamic parameters, the adsorption of the dyes was classified as physisorption and the reaction was spontaneous and exothermic. The data were also compared using studies with alumina as an adsorbent. Results showed that PRO-BEN exhibited better absorptivity and desorption than alumina making its use a better recyclable remediation strategy for the removal of organic dyes in wastewater treatment plants. In the second study, TEP was synthesized and then characterized by FT-IR Spectroscopy, 1H-NMR Spectroscopy, TGA and DLS. Thereafter, TEP was used to prepare TEP capped gold nanoparticles (TEP-AuNPs). Herein, two methods were investigated: the Turkevich method and an adaptation of the Turkevich method using bagasse extract. The TEP-AuNPs was characterized by FT-IR Spectroscopy, SEM, EDX, DLS and TEM. Thereafter the reduction of each of Allura Red, Congo Red and Methylene Blue was investigated with the TEP-AuNPs for its catalytic activity toward dye reduction. This study showed that the batch of AuNPs prepared by the Turkevich method had higher rates of dye reduction compared with AuNPs prepared using bagasse extract. Also the quantity of TEP used as capping agent greatly influenced the size, shape and surface charge of the nanoparticles as well as their catalytic performance: the Vroman effect explained this behavior of the TEP-AuNPs. It was finally concluded that whilst PRO-BEN, in the first study, showed excellent dye remediation properties, the second study on TEP-AuNPs showed good catalytic activity for the reduction of selected dyes, however, it was more effective at lower polymer concentration. Finally, both materials displayed good potential for the clean-up of selected synthetic dyes from synthetic effluents.


2020 ◽  
Vol 1 (4) ◽  
pp. 22-25
Author(s):  
Azwan Morni

This study reports a green method for the synthesis of gold nanoparticles (AuNPs) using the aqueous extract of Salix aegyptiaca extract. The effects of gold salt concentration, extract concentration and extract quantity were investigated on nanoparticles synthesis. Novel methods of ideally synthesizing AuNPs are thus thought that are formed at ambient temperatures, neutral pH, low costs and environmentally friendly fashion. AuNPs were characterized with different techniques such as UV–vis spectroscopy, FT-IR spectroscopy, X-ray diffraction, and TEM. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary carbonyl group, -OH groups and other stabilizing functional groups. TEM experiments showed that these nanoparticles are formed with various shapes and X-ray diffraction pattern showed high purity and face centered cubic structure of AuNPs. For electrochemical properties of AuNPs, a modified glassy carbon electrode using AuNPs (AuNPs/GCE) was investigated. The results show that electronic transmission rate between the modified electrode and [Fe (CN)6]3-/4- increased.


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