scholarly journals Hierarchization of Zeolites A and X Using Bacterial Cellulose as Macroporous Support

Author(s):  
Raquel Bessa ◽  
André Luís Pereira ◽  
Morsyleide Rosa ◽  
Michael Anderson ◽  
Adonay Loiola

In this work, we studied the formation of hierarchical porous cartridges by means of bacterial cellulose impregnation with the zeolites A and X. Cellulose was successfully produced by Komagataeibacter genus and the zeolites were obtained by hydrothermal route. The composites were formed using both oxidized and non-oxidized cellulose. Different characterization techniques were used to analyze the resulting materials like powder X-ray diffraction, spectroscopic techniques (infrared vibrational spectroscopy and nuclear magnetic resonance), electron microscopy, thermal analyses, as well as ionic exchange experiments. The results show that the composites present layers with large voids among them, formed by cellulose nanofibrils tangling the particles in the oxidized samples, and shiftings in the bands referent to the carboxilyc groups and hydrogen bondings. The oxidation step for the cellulose seems to be important for the hierarchization and a positive effect on the cartridges is found for Ca2+ ionic exchange tests. Thus, these components can be successfully mixed to form cartridges with potential use at gas and liquid adsorption technologies.

2018 ◽  
Vol 21 (7) ◽  
pp. 495-500 ◽  
Author(s):  
Hassan A. Almarshad ◽  
Sayed M. Badawy ◽  
Abdalkarem F. Alsharari

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.


1999 ◽  
Vol 23 (7) ◽  
pp. 418-419
Author(s):  
Simon J. Coles ◽  
Paul Faulds ◽  
Michael B. Hursthouse ◽  
David G. Kelly ◽  
Georgia C. Ranger ◽  
...  

Nickel(II) phosphine complexes are prepared with a series of diphenylalkenylphosphine ligands and characterised by single crystal X-ray diffraction and spectroscopic techniques.


Biomolecules ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 862
Author(s):  
Iryna Stepanenko ◽  
Maria V Babak ◽  
Gabriella Spengler ◽  
Marta Hammerstad ◽  
Ana Popovic-Bijelic ◽  
...  

A series of thiosemicarbazone-coumarin hybrids (HL1-HL3 and H2L4) has been synthesised in 12 steps and used for the preparation of mono- and dinuclear copper(II) complexes, namely Cu(HL1)Cl2 (1), Cu(HL2)Cl2 (2), Cu(HL3)Cl2 (3) and Cu2(H2L4)Cl4 (4), isolated in hydrated or solvated forms. Both the organic hybrids and their copper(II) and dicopper(II) complexes were comprehensively characterised by analytical and spectroscopic techniques, i.e., elemental analysis, ESI mass spectrometry, 1D and 2D NMR, IR and UV–vis spectroscopies, cyclic voltammetry (CV) and spectroelectrochemistry (SEC). Re-crystallisation of 1 from methanol afforded single crystals of copper(II) complex with monoanionic ligand Cu(L1)Cl, which could be studied by single crystal X-ray diffraction (SC-XRD). The prepared copper(II) complexes and their metal-free ligands revealed antiproliferative activity against highly resistant cancer cell lines, including triple negative breast cancer cells MDA-MB-231, sensitive COLO-205 and multidrug resistant COLO-320 colorectal adenocarcinoma cell lines, as well as in healthy human lung fibroblasts MRC-5 and compared to those for triapine and doxorubicin. In addition, their ability to reduce the tyrosyl radical in mouse R2 protein of ribonucleotide reductase has been ascertained by EPR spectroscopy and the results were compared with those for triapine.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Loreana C. Gallo ◽  
Noelia L. Gonzalez Vidal ◽  
Fabio F. Ferreira ◽  
María V. Ramírez-Rigo

Abstract Background Sulbactam pivoxil is an irreversible β-lactamase inhibitor that can be used with β-lactam antibiotics to improve antibacterial therapy by the oral route. Relevant properties of this drug for pharmaceutical manufacturing are not available in the open literature. In this work, a solid-state characterization of sulbactam pivoxil at the molecular, particle, and bulk levels was performed. Results Particles exhibited a mean diameter of about 350 μm, irregular shape crystals, and good flow properties. This work presents for the first time the crystal structure of this β-lactamase inhibitor obtained by X-ray diffraction analysis. Fourier-transform infrared results showed the characteristic bands of aliphatic hydrocarbons and ester groups. The differential scanning calorimetry curve exhibited a sharp endothermic peak at 109 °C corresponding to sulbactam pivoxil melting. The thermogravimetric curve revealed a mass loss at 184 °C associated with a decomposition process. This powder showed a moisture content of 0.34% and a water activity of 0.463. Potential interactions between sulbactam pivoxil and common pharmaceutical excipients were evaluated by thermal analysis. The endothermic peak and the enthalpies of melting were preserved in almost all the analyzed mixtures. Conclusion The powder was constituted by micro-sized crystals of sulbactam pivoxil that had suitable physicochemical properties for processing in controlled humidity environments. Thermal analyses suggested that sulbactam pivoxil is compatible with most of the evaluated excipients. The information obtained in the present study is relevant for the development, manufacturing, and storage of formulations that include sulbactam pivoxil.


Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4331
Author(s):  
David B. Hobart ◽  
Michael A. G. Berg ◽  
Hannah M. Rogers ◽  
Joseph S. Merola

The reaction of palladium(II) acetate with acyclic amino acids in acetone/water yields square planar bis-chelated palladium amino acid complexes that exhibit interesting non-covalent interactions. In all cases, complexes were examined by multiple spectroscopic techniques, especially HRMS (high resolution mass spectrometry), IR (infrared spectroscopy), and 1H NMR (nuclear magnetic resonance) spectroscopy. In some cases, suitable crystals for single crystal X-ray diffraction were able to be grown and the molecular structure was obtained. The molecular geometries of the products are discussed. Except for the alanine complex, all complexes incorporate water molecules into the extended lattice and exhibit N-H···O and/or O···(HOH)···O hydrogen bonding interactions. The non-covalent interactions are discussed in terms of the extended lattice structures exhibited by the structures.


2011 ◽  
Vol 1292 ◽  
Author(s):  
Dengrong Cai ◽  
Jianmin Li ◽  
Shundong Bu ◽  
Shengwen Yu ◽  
Dengren Jin ◽  
...  

ABSTRACTA facile hydrothermal route assisted by polyethylene glycol (PEG) 400 was utilized to synthesize single-phase Bi2Fe4O9 crystallites. X-ray diffraction results showed the products with PEG 400 of 30 g/L exhibited a preferred growth along the (001) plane. Transmission electron microscopy indicated that the morphology of the as-prepared Bi2Fe4O9 crystallites with PEG 400 were plake-like and rod-like. Strong absorption in visible-light region of the products was characterized by UV-vis diffuse reflectance spectrum (UV-DRS). The photocatalytic activity of Bi2Fe4O9 crystallites was evaluated on degradation of methyl orange (MO) under visible light irradiation. For 3 h irradiation, the degradation ratio was increased to 93% with the aid of a small amount of H2O2. The analysis of FT-IR spectra proved that the Bi2Fe4O9 catalysts were remained stable after the photocalytic reactions.


2014 ◽  
Vol 28 (06) ◽  
pp. 1450045 ◽  
Author(s):  
Arbab Mohammad Toufiq ◽  
Fengping Wang ◽  
Qurat-ul-Ain Javed ◽  
Yan Li

In this paper, single crystalline 1D tetragonal MnO 2 pen-type nanorods were synthesized by varying the dwell time through a facile hydrothermal route at a reaction temperature of 250°C. X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies showed that the diameter of MnO 2 nanorods decreases from 460 nm to 250 nm with the increase in hydrothermal reaction time from 5 h to 15 h. Field-emission scanning electron microscopy (FESEM) and TEM studies revealed the evolution of improved surface morphology of MnO 2 nanorods that are prepared with longer hydrothermal reaction time. The magnetic properties of the products were evaluated using vibrating sample magnetometer (VSM) at room temperature, which showed that the as-prepared samples exhibit weak ferromagnetic behavior. The effect of diameter on the magnetization values was observed and discussed in detail.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Hernane S. Barud ◽  
Thaís Regiani ◽  
Rodrigo F. C. Marques ◽  
Wilton R. Lustri ◽  
Younes Messaddeq ◽  
...  

Antimicrobial bacterial cellulose-silver nanoparticles composite membranes have been obtained by“in situ”preparation of Ag nanoparticles from hydrolytic decomposition of silver nitrate solution using triethanolamine as reducing and complexing agent. The formation of silver nanoparticles was evidenced by the X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and absorption in the UV-Visible (350 nm to 600 nm). Thermal and mechanical properties together with swelling behavior for water were considered. TEA concentration was observed to be important in order to obtain only Ag particles and not a mixture of silver oxides. It was also observed to control particle size and amount of silver contents in bacterial cellulose. The composite membranes exhibited strong antimicrobial activity against Gram-negative and Gram-positive bacteria.


Plants ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 6
Author(s):  
Asma Tabasum ◽  
Mousa Alghuthaymi ◽  
Umair Yaqub Qazi ◽  
Imran Shahid ◽  
Qamar Abbas ◽  
...  

Pesticides are one of the main organic pollutants as they are highly toxic and extensively used worldwide. The reclamation of wastewater containing pesticides is of utmost importance. For this purpose, GO-doped metal ferrites (GO-Fe3O4 and GO-CoFe2O4) were prepared and characterized using scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopic techniques. Photocatalytic potentials of catalysts were investigated against acetamiprid’s degradation. A detailed review of the parametric study revealed that efficiency of overall Fenton’s process relies on the combined effects of contributing factors, i.e., pH, initial oxidant concentration, catalyst dose, contact time, and acetamiprid load. ~97 and ~90% degradation of the acetamiprid was achieved by GO-CoFe2O4 and GO-Fe3O4, respectively during the first hour under UV radiations at optimized reaction conditions. At optimized conditions (i.e., pH:3, [H2O2]: 14.5 mM (for Fe3O4, GO-Fe3O4, and GO-CoFe2O4) and 21.75 mM (for CoFe2O4), catalysts: 100 mgL−1, time: 60min) the catalysts exhibited excellent performance, with high degradation rate, magnetic power, easy recovery at the end, and efficient reusability (up to 5 cycles without any considerable loss in catalytic activity). A high magnetic character offers its easy separation from aqueous systems using an external magnet. Moreover, the combined effects of experimental variables were assessed simultaneously and justified using response surface methodology (RSM).


2020 ◽  
Vol 18 (1) ◽  
pp. 453-462
Author(s):  
Jerry O. Adeyemi ◽  
Damian C. Onwudiwe ◽  
Nirasha Nundkumar ◽  
Moganavelli Singh

AbstractAmmonium benzyldithiocarbamate, represented as NH4L, was prepared and used in the complexation reaction involving three organotin(iv) salts, represented as R2SnCl2 (R = CH3, C4H9, and C6H5). The structures of the synthesized complexes [(CH3)2SnL2] (1), [(C4H9)2SnL2] (2), and [(C6H5)2SnL2] (3) were established using various spectroscopic techniques (Fourier transform infrared spectroscopy, 1H NMR, 13C NMR, and 119Sn NMR) and elemental analysis. Thermal decomposition of the complexes using thermogravimetric analysis under nitrogen showed no definite pathway in the pattern of the complexes even though they are structurally related. X-ray diffraction studies of the final residue showed a common diffraction pattern for the complexes and confirmed SnS as the product of the thermal treatment. Cytotoxicity studies of these complexes against the human tumor cell lines (HeLa and MCF-7) compared favorably with the used standard 5-fluorouracil drug, with complexes 2 and 3 showing very good activity toward the used cell lines.


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