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1.
Environ Technol ; : 1-23, 2023 Nov 12.
Article in English | MEDLINE | ID: mdl-37953534

ABSTRACT

ABSTRACTResearch efforts are focusing on investigating cost-effective and ecologically friendly ways to create nanoparticles as a result of promising developments in green technology (NPs). This experiment focused on the effectiveness of using biochar (TWB) made from coffee waste to extract levofloxacin (LEV) from water. The conclusive results of the trials showed that TWB is an effective adsorbent for removing LEV from liquid solutions. The TWB produced through biological processes underwent comprehensive analysis using techniques such as X-ray diffractometry (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller surface area measurement (BET), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. The bioengineered TWB's exceptional crystalline properties, which closely resemble the monoclinic structure of bulk TWB, were confirmed by the XRD analysis. Based on the scanning electron microscopy (SEM) data, the synthesis of TWB Nanoparticles resulted in the formation of spherical particles with an approximate diameter of 40 nm, accompanied by a substantial surface area of 285.55 m²/g. The Pseudo-Second-Order model, which best captured Levofloxacin's adsorption characteristics, was evaluated on the TWB, and the results showed that external mass transfer was the main determinant of response rate. It was also found that the adsorption process was endothermic and spontaneous. The system was optimized using the Box-Behnken design (BBD) methodology. The achieved removal capacity of 1119.19 mg/g utilizing the tested adsorbent was determined to be reasonable when compared to the performance of other previously used adsorbents when evaluating the effectiveness of eliminating LEV. The process of LEV adsorption onto TWB involves a number of different mechanisms, such as ion exchange, π-π interactions, electrostatic pore filling, and hydrogen bonding. Following extensive testing in connection with a real-world sample, the adsorbent demonstrated remarkable efficacy, and it maintained good performance even after undergoing three further regeneration cycles. By adjusting the annealing temperature, we controlled the synthesis of TWB nanoparticles across a range of sizes in order to maximize their antibacterial capabilities. This research utilized a pair of Gram-positive bacteria (Staphylococcus aureus and Bacillus subtilis) and a pair of Gram-negative bacteria (Pseudomonas aeruginosa and Escherichia coli) to evaluate the antibacterial efficacy of TWB.


Green synthesis of biochar via using tea waste.Adsorption studies of harmful pesticides Levofloxacin (LEV).The adsorbents exhibited good reusability for four adsorption/desorption cycles.Adsorption fit with pseudo second order kinetics and Langmuir isotherm model.The adsorption fitted to pseudo-second-order kinetically.This system will provide helpful guidance for coloured effluent treatment.Optimized the results by using Box-Behnken design.

2.
Environ Technol ; : 1-20, 2023 Jun 01.
Article in English | MEDLINE | ID: mdl-37248830

ABSTRACT

In the current investigation, we have reported on the preparation of Na-Mordenite (MOR) modified by tryptophan (MOR-NH2) nanocomposite was synthesized and characterized using FT-IR, XRD, SEM, XPS, and BET that represented that the MOR-NH2 has high surface area 288 m2/g and pore volume 0.38 cm3/g. This composite represented high efficiency in removal of food dye Azorubine (E122) was 1043 mg/g. Study all the factors that affected on the adsorption such as pH, dose, salinity, E122 dye concentration as well as study the adsorption isotherm models that represented that was fitted to Langmuir. Moreover, study the effect of time according to it the adsorption process was fitted to Pseudo-second-order, and the effect of temperature that approved that the reaction was endothermic, spontaneous, and chemisorption process. The MOR-NH2 nanocomposite was tested and proven to effectively inhibit the growth of Escherichia coli ATCC® 25922™ and Staphylococcus aureus ATCC® 25923™ at low concentrations. To the best of our knowledge, this work is the first to report the usage of MOR-NH2 adsorbents for the removal of E122 dye in wastewater samples. The mechanism of interaction between MOR-NH2 and E122 dye was determining as it could be through Hydrogen bonding, pore filling, or through π-π interaction. This research offers a promising solution for purifying water sources that are contaminated with a variety of chemicals, microorganisms, and other contaminants.

3.
Environ Technol ; : 1-17, 2023 Feb 20.
Article in English | MEDLINE | ID: mdl-36749794

ABSTRACT

The indirect emission had a negative influence on the ecosystem of enormous amounts of harmful dyes into water. Fe3O4@Ag-MOF was successfully fabricated to capture Gentine violet (GV)) as a model example of cationic dye from their aqueous solutions was evaluated in this search as a method to eliminate dyes from water contaminants. FTIR, XPS, BET, TGA, SEM, TEM, and XRD have all been used to study this adsorbent in order to determine its structural and chemical characteristics as well as to interpret its binding mechanisms. According to the results of the characterization, the synthesized composite had a size about 45 nm, a surface area of 856.06 m2/g, and considerable magnetic characteristics (66.2 emug-1). Consequently, we created mesoporous surfaces that had a strong ability to interface and absorb GV dye. It is possible to use the pseudo-second order rate equation to characterize the kinetic profile., while the Langmuir equation fits isotherm models. At pH 9, maximum sorption capacities can reach 1.68 mmol.g-1. Additionally, the investigations of temperature profiles indicated the endothermic process and Thermodynamic parameters were discovered as, ΔG°, ΔH° and ΔS° The synthesized adsorbent had an interestingly high reusability of > 92 percent up to the sixth cycle. These findings revealed that a mixture of electrostatic interactions, π-π stacking, hydrogen bonds, and pore filling were involved in the GV adsorption mechanism. Fe3O4@Ag-MOF was successful in demonstrating its effectiveness as a point-of-use colour collection candidate from actual dyeing effluents.

4.
Article in English | MEDLINE | ID: mdl-36537029

ABSTRACT

The purpose of this research was to investigate the doxorubicin (DOX) adsorption behavior on Fe3O4@Ag-Metal Organic Framework (Fe3O4@Ag-MOF). This adsorbent was effectively prepared using a simple synthetic process. Many instruments, including FTIR, XRD, SEM, TEM, and XPS, were used to characterized the new Fe3O4@Ag-MOF. Additionally, the presented Fe3O4@Ag-surface MOF's area was shown to be 586.06 m2/g with a size of around 43 nm. The composite that was made has magnetic properties that were quite strong (63.3 emu/g). The produced Fe3O4@Ag-MOF was discovered to have a fantastic ability to adsorb the anti-cancer drug DOX, with a 1.72 mmol/g (934.85 mg/g) adsorption capacity. On the basis of changes in temperature, pH, and DOX concentration, the DOX adsorption behavior mechanism was investigated. The adsorption capacity of Fe3O4@Ag-MOF for DOX was greater at pH 7.0, according to experimental data. The adsorption equilibrium also demonstrated that the Langmuir adsorption was regulated the best fit to the extracted data compared with the other models. Additionally, the activation energy of adsorption for DOX onto Fe3O4@Ag-MOF was determined, indicating the chemisorption process. The adsorption kinetics was shown in the well-known kinetic model of the pseudo-second-order. The adsorption thermodynamic measurements were documented according to according to the enthalpy (ΔH°), entropy(ΔS°), and Gibbs free energy (ΔG°) parameters demonstrated that the reaction was endothermic and spontaneous thermodynamic. The adsorption of DOX onto Fe3O4@Ag-MOF from real water samples (tap water, effluent wastewater, and influence wastewater) were investigated. It's interesting that the synthetic adsorbent had great recyclability 72.6 percent in the fifth cycle indicating that it was highly recyclable. After adsorption, the typical Fe3O4@Ag-MOF XRD peak intensities and locations were mostly unchanged throughout adsorption indicates the crystalline phase remained steady. The results indicated that Fe3O4@Ag-MOF were a good candidate for adsorbing the DOX and treating wastewater.


Subject(s)
Nanocomposites , Water Pollutants, Chemical , Adsorption , Wastewater , Doxorubicin , Water/chemistry , Water Pollutants, Chemical/chemistry , Kinetics
5.
RSC Adv ; 12(44): 28364-28375, 2022 Oct 04.
Article in English | MEDLINE | ID: mdl-36320495

ABSTRACT

We present the effective synthesis and structural characterization of three novel imidazolium-thiohydantoin ligands (IMTHs, 5a-c) and their Mn(iii) complexes (Mn(iii)IMTHs, 6a-c) in this study. The findings of elemental analyses, spectral analyses and magnetic measurements will be used to infer the stoichiometry, coordination styles, and geometrical aspects of Mn(iii)IMTHs. The new compounds were evaluated for their chemotherapeutic potential against ESKAPE pathogens and liver cancer (HepG2). According to the MIC and MBC values, the bactericidal and bacteriostatic activities of IMTHs have been significantly improved following coordination with the Mn(iii) ion. The MTT assay results showed that all Mn(iii)IMTHs had the potential to reduce the viability of liver carcinoma (HepG2) cells in a dose-dependent manner, with the BF4-supported complex (6b) outperforming its counterparts (6a and 6c) as well as a clinical anticancer drug (VBL). Additionally, Mn-IMTH2 (6b) showed the highest level of selectivity (SI = 32.05) for targeting malignant cells (HepG2) over healthy cells (HL7702).

6.
J Water Health ; 13(4): 970-84, 2015 Dec.
Article in English | MEDLINE | ID: mdl-26608759

ABSTRACT

Most drinking water industries are closely examining options to maintain a certain level of disinfectant residual through the entire distribution system. Chlorine dioxide is one of the promising disinfectants that is usually used as a secondary disinfectant, whereas the selection of the proper monitoring analytical technique to ensure disinfection and regulatory compliance has been debated within the industry. This research endeavored to objectively compare the performance of commercially available analytical techniques used for chlorine dioxide measurements (namely, chronoamperometry, DPD (N,N-diethyl-p-phenylenediamine), Lissamine Green B (LGB WET) and amperometric titration), to determine the superior technique. The commonly available commercial analytical techniques were evaluated over a wide range of chlorine dioxide concentrations. In reference to pre-defined criteria, the superior analytical technique was determined. To discern the effectiveness of such superior technique, various factors, such as sample temperature, high ionic strength, and other interferences that might influence the performance were examined. Among the four techniques, chronoamperometry technique indicates a significant level of accuracy and precision. Furthermore, the various influencing factors studied did not diminish the technique's performance where it was fairly adequate in all matrices. This study is a step towards proper disinfection monitoring and it confidently assists engineers with chlorine dioxide disinfection system planning and management.


Subject(s)
Chlorine Compounds/analysis , Disinfectants/analysis , Drinking Water/analysis , Oxides/analysis , Water Purification/methods , Environmental Monitoring
7.
Article in English | MEDLINE | ID: mdl-26067934

ABSTRACT

The coordination behavior of a series of transition metal ions named Cr(III), Fe(III), Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with a mono negative tridentate guaifenesin ligand (GFS) (OOO donation sites) and 1,10-phenanthroline (Phen) is reported. The metal complexes are characterized based on elemental analyses, IR, (1)H NMR, solid reflectance, magnetic moment, molar conductance, UV-vis spectral studies, mass spectroscopy, ESR, XRD and thermal analysis (TG and DTG). The ternary metal complexes were found to have the formulae of [M(GFS)(Phen)Cl]Cl·nH2O (M=Cr(III) (n=1) and Fe(III) (n=0)), [M(GFS)(Phen)Cl]·nH2O (M=Mn(II) (n=0), Zn(II) (n=0) and Cu(II) (n=3)) and [M(GFS)(Phen)(H2O)]Cl·nH2O (M=Co(II) (n=0), Ni(II) (n=0) and Cd(II) (n=4)). All the chelates are found to have octahedral geometrical structures. The ligand and its ternary chelates are subjected to thermal analyses (TG and DTG). The GFS ligand, in comparison to its ternary metal complexes also was screened for their antibacterial activity on gram positive bacteria (Bacillus subtilis and Staphylococcus aureus), gram negative bacteria (Escherichia coli and Neisseria gonorrhoeae) and for in vitro antifungal activity against (Candida albicans). The activity data show that the metal complexes have antibacterial and antifungal activity more than the parent GFS ligand. The complexes were also screened for its in vitro anticancer activity against the Breast cell line (MFC7) and the results obtained show that they exhibit a considerable anticancer activity.


Subject(s)
Antineoplastic Agents , Coordination Complexes , Guaifenesin/chemistry , Transition Elements/chemistry , Anti-Bacterial Agents/chemical synthesis , Anti-Bacterial Agents/chemistry , Anti-Bacterial Agents/pharmacology , Antineoplastic Agents/chemical synthesis , Antineoplastic Agents/chemistry , Antineoplastic Agents/pharmacology , Coordination Complexes/chemical synthesis , Coordination Complexes/chemistry , Coordination Complexes/pharmacology , Drug Screening Assays, Antitumor , Guaifenesin/chemical synthesis , Guaifenesin/pharmacology , Humans , MCF-7 Cells , Magnetic Resonance Spectroscopy , Mass Spectrometry , Microbial Sensitivity Tests , Molecular Structure , Spectrophotometry, Infrared , Thermodynamics , Transition Elements/pharmacology
8.
Spectrochim Acta A Mol Biomol Spectrosc ; 147: 200-11, 2015 Aug 05.
Article in English | MEDLINE | ID: mdl-25841152

ABSTRACT

5-(2,3-Dimethyl-1-phenylpyrazol-5-one azo)-2-thioxo-4-thiazolidinone (HL) and its metal complexes with copper(II) (1), cobalt(II) (2) and nickel(II) (3) are synthesized and characterized by physico-chemical techniques. The thermal properties of the ligand (HL) and its metal complexes (1-3) are discussed. The thermal activation energies of decomposition (Ea) of HL and its metal complexes with Cu(II), Co(II) and Ni(II) are found to be 48.76, 36.83, 30.59 and 40.45 kJ/mol, respectively. The frequency and temperature dependence of ac conductivity, dielectric constants for HL and its complexes (1-3) are investigated in the temperature range 300-356 K and frequency range 0.1-100 kHz. Both of the ac conductivity and the values of the thermal activation energy for conduction, as well as the dielectric properties of the complexes of HL are found to depend on the nature of the metallic ions. The values of the thermal activation energies of electrical conductivity decrease with increasing the value of test frequency. The small polarons tunneling (SPT) is the dominant conduction mechanism for the ligand (HL), while for complex (2) the overlapping large tunneling model (OLPT) is the dominant conduction mechanism. The correlated barrier hopping (CBH) is the dominant conduction mechanism for both of the complexes (1) and (3).

9.
Spectrochim Acta A Mol Biomol Spectrosc ; 143: 200-12, 2015 May 15.
Article in English | MEDLINE | ID: mdl-25727297

ABSTRACT

A novel series of (5-(4'-derivatives phenyl azo)-8-hydroxy-7-quinolinecarboxaldehyde) (AQLn) (n=1, p-OCH3; n=2, R=H; and n=3; p-NO2) and their complexes [Cu(AQLn)2]·5H2O are synthesized and investigated. The optimized bond lengths, bond angles and the calculated quantum chemical parameters for AQLn are investigated. HOMO-LUMO energy gap, absolute electronegativities, chemical potentials, and absolute hardness are also calculated. The thermal properties, dielectric properties, alternating current conductivity (σac) and conduction mechanism are investigated in the frequency range 0.1-100kHz and temperature range 293-568K for AQL1-3 and 318-693K for [Cu(AQL1-3)2]·5H2O complexes. The thermal properties are of ligands (AQLn) and their Cu(II) complexes investigated by thermogravimetric analysis (TGA). The temperature and frequency dependence of the real and the imaginary part of the dielectric constant are studied. The values of the thermal activation energy of conduction mechanism for AQLn and their complexes [Cu(AQLn)2]·5H2O under investigation are calculated at different test frequencies. The values of thermal activation energies ΔE1 and ΔE2 for AQLn and [Cu(AQLn)2]·5H2O decrease with increasing the values of frequency. The ac conductivity is found to be depending on the chemical structure of the compounds. Different conduction mechanisms have been proposed to explain the obtained experimental data. The small polaron tunneling (SPT) is the dominant conduction mechanism for AQL1 and its complex [Cu(AQL1)2]·5H2O. The quantum mechanical tunneling (QMT) is the dominant conduction mechanism for AQL2 and its complex [Cu(AQL2)2]·5H2O. The correlated barrier hopping (CBH) is the dominant conduction mechanism for AQL3 and its complex [Cu(AQL3)2]·5H2O, and the values of the maximum barrier height (Wm) are calculated.


Subject(s)
Azo Compounds/chemistry , Chelating Agents/chemistry , Coordination Complexes/chemistry , Copper/chemistry , Quinolines/chemistry , Azo Compounds/chemical synthesis , Chelating Agents/chemical synthesis , Coordination Complexes/chemical synthesis , Electric Conductivity , Models, Molecular , Quantum Theory , Quinolines/chemical synthesis , Thermodynamics , Thermogravimetry
10.
Spectrochim Acta A Mol Biomol Spectrosc ; 140: 111-31, 2015 Apr 05.
Article in English | MEDLINE | ID: mdl-25589393

ABSTRACT

A number of novel polymer complexes of various anions of copper(II), cobalt(II), nickel(II) and uranyl(II) with N(4-(acrylamido)-2-hydroxy benzoic acid) (ABH) have been synthesized and characterized by elemental analysis, IR, 1H NMR, magnetic susceptibility measurements, electronic spin resonance, vibrational spectra and thermal analysis. The molecular structures of the ligand are optimized theoretically and the quantum chemical parameters are calculated. Tentative structures for the polymeric metal complexes due to their potential application are also suggested. The IR data exhibit the coordination of ONO2/OAc/SO4 with the metal ions in the polymeric metal complex. Vibrational spectra indicate coordination of carboxylate oxygen and phenolic OH of the ligand giving a MO4 square planar chromophore. Ligand field ESR spectra support square planar geometry around Cu(II). The thermal decomposition of the polymer complexes were discussed in relation to structure, and the thermodynamic parameters of the decomposition stages were evaluated applying Coast-Redfern and Horowitz-Metzger methods.


Subject(s)
Acrylamides/chemistry , Salicylic Acid/chemistry , Acrylamides/chemical synthesis , Electron Spin Resonance Spectroscopy , Magnetic Resonance Spectroscopy , Models, Molecular , Salicylic Acid/chemical synthesis , Thermodynamics , Thermogravimetry
11.
Spectrochim Acta A Mol Biomol Spectrosc ; 137: 1039-49, 2015 Feb 25.
Article in English | MEDLINE | ID: mdl-25286116

ABSTRACT

N-acryloyl-4-aminosalicylic acid (4-AMSA), monomer (HL) and 5-(4'-alkyl phenylazo)-N-acryloyl-4-aminosalicylic acid (HLn) are synthesized and characterized with various physico-chemical techniques. Thin films of 5-(4'-alkyl phenylazo)-N-acryloyl-4-aminosalicylic acid (HLn) are prepared by spin coating technique. The X-ray diffraction (XRD) patterns of 4-aminosalicylic acid (4-ASA) and its derivatives are investigated in powder and thin film forms. Thermal properties of the compounds are investigated by thermogravemetric analysis (TGA). The optical energy gap and the type of optical transition are investigated in the wavelength range (200-2500 nm) for 4-ASA, HL and HLn. The values of fundamental energy gap (Eg) are in the range 3.60-3.69 eV for all compounds and the type of optical transition is found to be indirect allowed. The onset energy gap Eg(∗) appeared only for azodye compounds is found to be in the range 0.95-1.55 eV depending on the substituent function groups. The refractive index, n, shows a normal dispersion in the wavelength range 650-2500 nm, while shows anomalous dispersion in the wavelength rang 200-650 nm. The dispersion parameters ε∞, εL, Ed, Eo and N/m(∗) are calculated. The photoluminescence phenomena (PL) appear for thin films of 4-ASA and its derivatives show three main emission transitions.


Subject(s)
Azo Compounds/chemistry , Membranes, Artificial , Salicylates/chemistry , X-Ray Diffraction
12.
Spectrochim Acta A Mol Biomol Spectrosc ; 135: 774-91, 2015 Jan 25.
Article in English | MEDLINE | ID: mdl-25150428

ABSTRACT

An interesting azodye heterocyclic ligand of copper(II), cobalt(II), nickel(II) and uranyl(II) complexes have been synthesized by the reaction of metal salts with 5-(2,3-dimethyl-1-phenylpyrazol-5-one azo)-2-thioxo-4-thiazolidinone (HL) yields 1:1 and 1:2 (M:L) complexes depending on the reaction conditions. The elemental analysis, magnetic moments, spectral (UV-Vis, IR, (1)H and (13)C NMR and ESR) and thermal studies were used to characterize the isolated complexes. The molecular structures of the ligand tautomers are optimized theoretically and the quantum chemical parameters are calculated. The IR spectra showed that the ligand (HL) act as monobasic tridentate/neutral bidentate through the (-N=N), enolic (C-O)(-) and/or oxygen keto moiety groups forming a five/six-membered structures. According to intramolecular hydrogen bond leads to increasing of the complexes stability. The molar conductivities show that all the complexes are non-electrolytes. The ESR spectra indicate that the free electron is in dxy orbital. The calculated bonding parameter indicates that in-plane σ-bonding is more covalent than in-plane π-bonding. The coordination geometry is five/six-coordinated trigonal bipyramidal for complex (1) and octahedral for complexes (2-6). The value of covalency factor ß1(2) and orbital reduction factor K accounts for the covalent nature of the complexes. The activation thermodynamic parameters are calculated using Coats-Redfern and Horowitz-Metzger methods. The synthesized ligand (HL) and its Cu(II) complexes (1, 2 and 4) are screened for their biological activity against bacterial and fungal species. The ligand (HL) showed antimicrobial activities against Escherichia coli. The ligand (HL) and its Cu(II) complexes (2 and 4) have very high antifungal activity against Penicillium italicum. The inhibitive action of ligand (HL), against the corrosion of C-steel in 2M HCl solution has been investigated using potentiodynamic polarization and electrochemical impedance spectroscopy (EIS).


Subject(s)
Azo Compounds/chemistry , Coloring Agents/chemistry , Metals/chemistry , Temperature , Azo Compounds/pharmacology , Bacteria/drug effects , Carbon-13 Magnetic Resonance Spectroscopy , Coloring Agents/pharmacology , Dielectric Spectroscopy , Electron Spin Resonance Spectroscopy , Electrons , Fungi/drug effects , Ions , Kinetics , Ligands , Magnetic Phenomena , Microbial Sensitivity Tests , Molecular Conformation , Proton Magnetic Resonance Spectroscopy , Pyrazoles/chemistry , Quantum Theory , Spectrophotometry, Infrared , Spin Labels , Stereoisomerism , Thermogravimetry , X-Ray Diffraction
13.
Article in English | MEDLINE | ID: mdl-24840490

ABSTRACT

The synthesis and characterization of ruthenium mononuclear complexes containing NO bidentate ligands are reported. The complexes cis-[Ru(II)(bpy)2L](PF6)n (1a-c), [Ru(III)Cl(L)2(H2O)] (2a-b) and [Ru(III)Cl2(L)2]Cl (2c) were prepared by the reaction of cis-[Ru(II)Cl2(bpy)2]·2H2O (bpy=2,2'-bipyridine) and/or RuCl3·nH2O with the Ligands: 2-aminophenol (2-aph), 8-hydroxyquinoline (8-hq) and 4-aminoantipyrine (4-apy). These complexes were characterized by elemental analysis, spectroscopic (IR, UV-Vis, (1)H NMR, ESR) and magnetic susceptibility measurements. The ligand field parameters, Δo (splitting parameter), B (Racah parameter of interelectronic repulsion), and ß (nephelauxetic ratio) were calculated. The redox properties were also investigated electrochemically by cyclic voltammetry. The complexes cis-[Ru(II)(bpy)2(8-hq)](PF6)2 (1b) and [Ru(III)Cl(8-hq)2(H2O)] (2b) have been investigated in conjunction with N-methylmorpholine-N-oxide (NMO) as co-oxidant for the catalytic dehydrogenation of benzyl amine, p-methyl benzylamine and p-nitrobenzylamine to their respective nitriles.


Subject(s)
Coordination Complexes/chemistry , Nitric Oxide/chemistry , Ruthenium/chemistry , Benzylamines/chemistry , Catalysis , Coordination Complexes/chemical synthesis , Electrochemical Techniques , Hydrogenation , Ligands , Nitric Oxide/chemical synthesis , Nitriles/chemistry , Oxidation-Reduction , Spectrum Analysis
14.
Spectrochim Acta A Mol Biomol Spectrosc ; 127: 310-28, 2014 Jun 05.
Article in English | MEDLINE | ID: mdl-24632240

ABSTRACT

A series of heterocyclic ligand of copper(II) complexes have been synthesized by the reaction of copper(II) acetate with 5-(4'-derivatives phenylazo)-2-thioxothiazolidin-4-one (HLn) yields 1:1 and 1:2 (M:L) complexes depending on the reaction conditions. The elemental analysis, spectral (IR and ESR), conductance, magnetic measurements, and thermogravimetric analysis (TGA) are used to characterize the isolated complexes. It is found that the change of substituent affects the thermal properties of azodye rhodanine derivatives and their Cu(II) complexes. The molecular and electronic structures of the investigated compounds (HLn) were also studied using quantum chemical calculations. According to intramolecular hydrogen bond leads to increasing of the complexes stability. The data revealed that the coordination geometry around Cu(II) in all complexes (1-4) exhibit a trans square planar by NO monobasic bidentate and the two monobasic bidentate in octahedral complexes (5-7). Electronic, magnetic data and ESR spectra proposed the square planar structure for all complexes (1-4) under investigation. The value of covalency factor [Formula: see text] and orbital reduction factor K accounts for the covalent nature of the complexes. The activation thermodynamic parameters, such as activation energy (Ea), enthalpy (ΔH(*)), entropy (ΔS(*)), and Gibbs free energy change of the decomposition (ΔG(*)) are calculated using Coats-Redfern and Horowitz-Metzger methods.


Subject(s)
Copper/chemistry , Heterocyclic Compounds, 2-Ring/chemistry , Molecular Structure , Thermodynamics
15.
Article in English | MEDLINE | ID: mdl-23973590

ABSTRACT

A series of novel bidentate azodye quinoline ligands were synthesized with various p-aromatic amines like p-(OCH3, CH3, H, Cl and NO2). All ligands and their complexes have been characterized on the basis of elemental analysis, IR, (1)H and (13)C NMR data and spectroscopic studies. IR and (1)H NMR studies reveal that the ligands (HLn) exists in the tautomeric azo/hydrazo form in both states with intramolecular hydrogen bonding. The ligands obtained contain NN and phenolic functional groups in different positions with respect to the quinoline group. IR spectra show that the azo compounds (HLn) act as monobasic bidentate ligand by coordinating via the azodye (NN) and oxygen atom of the phenolic group. The ESR (g|| and g ) and bonding α(2) parameters of the copper ion were greatly affected by substituting several groups position of ring of quinoline and p-aromatic ring. The ESR spectra of copper complexes in powder form show a broad signal with values in order g|| >g > ge > 2.0023. The value of covalency factor ß and orbital reduction factor K accounts for the covalent nature of the complexes. All complexes possessed an octahedral and square planar geometry. The thermal properties of the complexes were investigated using TGA and DSC. It is found that the change of substituent affects the thermal properties of complexes.


Subject(s)
Azo Compounds/chemistry , Coloring Agents/chemistry , Copper/chemistry , Quinolines/chemistry , Electron Spin Resonance Spectroscopy , Hydrogen Bonding , Ligands , Spectrophotometry, Infrared
16.
Article in English | MEDLINE | ID: mdl-23268204

ABSTRACT

A novel series of copper(II) and palladium(II) with 4-derivatives benzaldehyde pyrazolone (L(n)) were synthesized. The mixed ligand complexes were prepared by using 1,10-phenanthroline (Phen) as second ligand. The structure of these complexes was identified and confirm by elemental analysis, molar conductivity, UV-Vis, IR and (1)H NMR spectroscopy and magnetic moment measurements as well as thermal analysis. The ligand behaves as a neutral bidentate ligand through ON donor sites. ESR spectra show the simultaneous presence of a planar trans and a nearly planar cis isomers in the 1:2 ratio for all N,O complexes [Cu(L(n))(2)]Cl(2)⋅2H(2)O. Schiff bases (L(n)) were tested against bacterial species; namely two Gram positive bacteria (Staphylococcus aureus and Bacillus cereus) and two Gram negative bacteria (Escherichia coli and Klebsiella pneumoniae) and fungal species (Aspergillus niger, Fusarium oxysporium, Penicillium italicum and Alternaria alternata). The tested compounds have antibacterial activity against S. aureus, B. cereus and K. pneumoniae.


Subject(s)
Anti-Infective Agents/pharmacology , Ampyrone/chemistry , Ampyrone/pharmacology , Anti-Bacterial Agents/pharmacology , Anti-Infective Agents/chemical synthesis , Anti-Infective Agents/chemistry , Antifungal Agents/pharmacology , Bacteria/drug effects , Coordination Complexes/chemistry , Coordination Complexes/pharmacology , Copper/chemistry , Copper/pharmacology , Electron Spin Resonance Spectroscopy , Electrons , Fungi/drug effects , Ligands , Magnetic Phenomena , Magnetic Resonance Spectroscopy , Microbial Sensitivity Tests , Palladium/chemistry , Schiff Bases/chemical synthesis , Schiff Bases/chemistry , Schiff Bases/pharmacology , Spectrophotometry, Infrared , Thermogravimetry , X-Ray Diffraction
17.
Article in English | MEDLINE | ID: mdl-23064551

ABSTRACT

A novel series of platinum(II) and palladium(II) complexes have been synthesized by template condensation of 4-methoxybenzaldehyde, benzaldehyde, 4-chlorobenzaldehyde and 4-nitrobenzaldehyde, with appropriate 4-aminoantipyrine (4-AAP) in the presence of K(2)PtCl(4)/PdCl(2) to form complexes of the type [M(L(n))Cl(2)](where M=Pt(II) or Pd(II)). The corresponding Schiff base complexes mixed ligand were prepared by condensation of [M(L(n))Cl(2)] with ethanolamine (LH). The complexes have been characterized with the help of elemental analysis, IR, (1)H and (13)C NMR, electronic spectra, conductance measurements, magnetic susceptibilities and thermal analysis. On the basis of these studies, it is clear that ligands coordinated to metal atom in a mononuclear (NO) in (1-6), Schiff base complexes (NN(*)) in (7-9) and monobasic tridentate Schiff base complexes (NN(*)O) in (10-12). Thus, suitable square planar geometry for tetradentated state has been suggested for the metal complexes. Various ligand and nephelouxetic parameter have been calculated for the complexes. The thermal decomposition for complexes was studied.


Subject(s)
Ampyrone/chemistry , Benzaldehydes/chemistry , Coordination Complexes/chemistry , Organoplatinum Compounds/chemistry , Palladium/chemistry , Ampyrone/chemical synthesis , Benzaldehydes/chemical synthesis , Coordination Complexes/chemical synthesis , Ligands , Magnetic Resonance Spectroscopy , Molecular Conformation , Organoplatinum Compounds/chemical synthesis , Schiff Bases/chemical synthesis , Schiff Bases/chemistry , Spectrophotometry, Infrared , Thermogravimetry
18.
Article in English | MEDLINE | ID: mdl-22137746

ABSTRACT

The amidation of aliphatic amine with acryloyl chloride in dry benzene as a solvent has been performed. Moreover, the polymer complexes have been prepared and structurally characterized by analyses, molar conductance measurements, magnetic susceptibility measurements, spectral techniques like IR, UV, NMR, ESR and thermal methods. Acryloyl hydrazine (AH) has been shown to behave as a bidentate ligand via its nitrogen (NH(2) of hydrazine group) and C-O/C=O (acryloyl group) in polymer complexes, all of which exhibit supramolecular architectures assembled through weak interaction including hydrogen bonding and π-π stacking .The magnetic and spectral data indicate a square planar geometry for Cu(2+) complexes and an octahedral geometry for Co(II) and UO(2)(II). The ESR spectral data of the Cu(II) complexes showed that the metal-ligand bonds have considerable covalent character. The thermal stability was investigated using thermogravimetric analysis. The results showed that the polymer complexes are more stable than the homopolymer.


Subject(s)
Macromolecular Substances/chemistry , Models, Chemical , Polymers/chemistry , Coordination Complexes/chemistry , Differential Thermal Analysis , Electric Conductivity , Electron Spin Resonance Spectroscopy , Electrons , Hydrazines/chemistry , Hydrogen Bonding , Ligands , Magnetic Resonance Spectroscopy , Magnetics , Spectrophotometry, Infrared , Stereoisomerism , Temperature , Thermogravimetry , Vibration
19.
Article in English | MEDLINE | ID: mdl-21962380

ABSTRACT

The synthetic methods of novel Cu(II) and adduct complexes, with selective azodyes containing nitrogen and oxygen donor ligands have been developed, characterized and presented. The prepared complexes fall into the stoichiometric formulae of [Cu(L(n))(2)](A) and [Cu(L(n))(2)(Py)(2)](B), where two types of complexes were expected and described. In type [(A) (1:2)] the chelate rings are six-membered/four coordinate, whereas in type [(B) (1:2:2)] they are six-membered/six coordinate. The important bands in the IR spectra and main (1)H NMR signals are tentatively assigned and discussed in relation to the predicted assembly of the molecular structure. The IR data of the azodye ligands suggested the existing of a bidentate binding involving azodye nitrogen and C-O oxygen atom of enolic group. They also showed the presence of Py coordinating with the metal ion. The coordination geometries and electronic structures are determined from the framework of the proposed modeling of the formed novel complexes. The complexes (1-5) exist in trans-isomeric [N,O] solid form, while adduct complexes (6-10) exist in trans isomeric (Py) form. The square planar/octahedral coordination geometry of Cu(II)/adduct is made up of an N-atom of azodye, the deprotonated enolic O-atom and two Py. The azo group was involved in chelation for all the prepared complexes. ESR spectra show the simultaneous presence of a planar trans and a nearly planar cis isomers in the 1:2 ratio for all N,O complexes [Cu(L(n))(2)]. The ligands in the dimmer are stacked over one another. In the solid state of azo-rhodanine, the dimmers have inter- and intramolecular hydrogen bonds. Interactions between the ligands and Cu(II) are also discussed.


Subject(s)
Azo Compounds/chemistry , Coloring Agents/chemistry , Coordination Complexes/chemistry , Copper/chemistry , Electron Spin Resonance Spectroscopy , Hydrogen Bonding , Magnetic Resonance Spectroscopy
20.
Spectrochim Acta A Mol Biomol Spectrosc ; 61(8): 1847-51, 2005 Jun.
Article in English | MEDLINE | ID: mdl-15863056

ABSTRACT

Several dioxouranium(VI) heterochelates with tetradentate monobasic hydrazone compounds (HL(n)) have been synthesized. The heterochelates of the type [(UO2)2(HL(n))(L(n))2(OAc)2(OH2)2]n have been characterized on the basis of elemental analyses, IR and electronic spectra, conductance and magnetic susceptibility measurements. The complexes are polymeric, non-electrolytes, diamagnetic and eight-coordinated. Wilson, G.F. matrix method, Badger's formula, Jones and El-Sonbati equations were used to determine the stretching and interaction force constants from which the U-O bond distances were calculated. The bond distances of these complexes were also investigated.


Subject(s)
Hydrazones/chemistry , Nitrogen/chemistry , Spectrophotometry, Infrared/methods , Electrolytes/chemistry , Electrons , Heterocyclic Compounds , Ions , Macrocyclic Compounds , Magnetic Resonance Spectroscopy , Magnetics , Models, Chemical , Molecular Conformation , Polymers/chemistry , Spectrophotometry , Uranium/chemistry
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