Synthesis, characterization, and electrochemical study of a mononuclear Cu(II) complex with a 4-acyl pyrazolone ligand

2018 ◽  
Vol 73 (10) ◽  
pp. 713-718 ◽  
Author(s):  
Kiran Nakum ◽  
Rajendrasinh N. Jadeja
Keyword(s):  
Single Crystal ◽  
Thermo Gravimetric Analysis ◽  
Planar Geometry ◽  
Spectroscopic Techniques ◽  
Gravimetric Analysis ◽  
Thermo Gravimetric ◽  
X Ray ◽  
Square Planar ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Abstract1-(2-Chlorophenyl)-3-methyl-4-propionyl-1H-pyrazol-5(4H)-one was synthesized and characterized by Fourier transform infrared (FT-IR) spectroscopy, 1H nuclear magnetic resonance, and single-crystal X-ray analysis. Its Cu(II) complex was prepared and characterized by FT-IR, thermo gravimetric analysis-differential thermal analysis, ultraviolet-visible spectroscopy, cyclic voltammetry, and single-crystal X-ray structure determination. On the basis of analytical and spectroscopic techniques, a distorted square planar geometry of the complex has been found.

Trigonal dodecahedral sodium coordination in a trinuclear copper(II)-sodium complex incorporating a salen-type compartmental Schiff base

2017 ◽  
Vol 72 (2) ◽  
pp. 133-140 ◽  
Author(s):  
Madhusudan Nandy ◽  
Debnath Saha ◽  
Corrado Rizzoli ◽  
Shyamapada Shit
Keyword(s):  
Schiff Base ◽  
Sodium Ion ◽  
Planar Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Physicochemical Studies ◽  
Ft Ir ◽  
Good Agreement ◽  
Ft Ir Spectroscopy

AbstractA new trinuclear heterometallic complex, [(CuL)Na(CuL)]·ClO4 (1), has been prepared using a Schiff base, H2L (where H2L=N,N′-(1,2-phenylene)-bis(3-methoxysalicylideneimine) and characterized by elemental analysis, Fourier transform infra-red (FT-IR) spectroscopy, UV/Vis, magnetic, electrochemical, and single crystal X-ray diffraction methods. The structure analysis reveals that two metallo-ligand [(CuL)] units are connected to each other by a sodium ion resulting in the cationic unit [(CuL)Na(CuL)]+. Both the copper(II) ions display an almost square planar geometry while the sodium ion adopts a trigonal-dodecahedral coordination geometry. The spectroscopic and other physicochemical studies are in good agreement with the crystal structure of the complex.

Effect of Synthesis Temperature on Particles Size and Morphology of Zirconium Oxide Nanoparticle

2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola
Keyword(s):  
Electron Microscopy ◽  
Particle Size ◽  
Zirconium Oxide ◽  
Thermo Gravimetric Analysis ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Crystallite Sizes ◽  
Ft Ir

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.

Grafting of Chitosan: Structural, Thermal and Antimicrobial Properties

2019 ◽  
Vol 41 (2) ◽  
pp. 240-240
Author(s):  
Nevin Cankaya Nevin Cankaya
Keyword(s):  
Antimicrobial Activity ◽  
Graft Copolymers ◽  
Thermo Gravimetric Analysis ◽  
Antimicrobial Properties ◽  
Gravimetric Analysis ◽  
Analysis Method ◽  
Methacryloyl Chloride ◽  
Thermo Gravimetric ◽  
Thermal Stabilities ◽  
Ft Ir

In this study, some new chitosan materials were synthesized by the grafting of chitosan with the monomers such as 1-vinylimidazole (VIM), methacrylamide (MAm) and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS). First of all, chitosan methacrylate was prepared by esterification of primary -OH group with methacryloyl chloride a 25.13% yield by mole. The monomers were grafted into chitosan methacrylate via free radical polymerization using 2,2and#39;-Azobisisobutyronitrile as an initiator in N,N-dimethylformamide. The graft copolymers were characterized by FT-IR spectra and elemental analysis. Thermal stabilities of the graft copolymers were determined by TGA (thermo gravimetric analysis) method. The synthesized chitosan methacrylate and its graft copolymers were tested for their antimicrobial activity against bacteria and yeast.

Functionalization of α-ZrP by 1,2-Epoxypropane for Further Modification

2017 ◽  
Vol 898 ◽  
pp. 2347-2353
Author(s):  
Ahmed Hossamaldin ◽  
Ping Liu ◽  
Ya Du ◽  
Xiao Ze Jiang ◽  
Bin Sun ◽  
...  
Keyword(s):  
Epoxy Group ◽  
Thermo Gravimetric Analysis ◽  
Mas Nmr ◽  
Interlayer Distance ◽  
Gravimetric Analysis ◽  
Thermo Gravimetric ◽  
Grafting Ratio ◽  
Internal Surfaces ◽  
Carbon Mass ◽  
Ft Ir

To prepare alpha zirconium phosphate (α-ZrP) with high interlayer distance, grafting ratio and thermal stability, 1,2-epoxypropane was used to modify α-ZrP as the epoxy group reacting with P-OH on the external and internal surfaces of α-ZrP to form P-O-C bonds after small amines pre-intercalation. Different characterization techniques were used, including X-ray Powder Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR), Thermo-Gravimetric Analysis (TGA) and Carbon Mass Nuclear Magnetic Resonance (13C MAS NMR). The results of XRD confirmed the pre-intercalation of amino-propane and the intercalation of 1,2-epoxypropane, as the interlayer distance increased from 7.5 Å to 16.9 Å and 15.3 Å, respectively. FT-IR and 13C MAS NMR results confirmed the formation of P-O-C bonds between 1,2-epoxypropane and α-ZrP. TGA analysis showed that the grafting ratio of 1,2-epoxypropane was 19.44%.

Biosynthesis and Characterization of Copper Nanoparticles Using a Bioflocculant Extracted from Alcaligenis faecalis HCB2

2019 ◽  
Vol 11 (11) ◽  
pp. 1064-1070 ◽  
Author(s):  
Nkosinathi G. Dlamini ◽  
Albertus K. Basson ◽  
V. S. R. Rajasekhar Pullabhotla
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Copper Nanoparticles ◽  
Average Particle Size ◽  
Thermo Gravimetric Analysis ◽  
Average Particle ◽  
Gravimetric Analysis ◽  
X Ray ◽  
Transmission Electron ◽  
Ft Ir

Bioflocculant from Alcaligenis faecalis HCB2 was used in the eco-friendly synthesis of the copper nanoparticles. Nanoparticles were characterized using a scanning electron microscope (SEM), transmission electron microscopy (TEM), UV-visible spectroscopy, thermo gravimetric analysis (TGA) and Fourier Transform Infrared Spectroscopy (FT-IR). The transmission electron microscopy images showed close to spherical shapes with an average particle size of ∼53 nm. Energy-dispersive X-ray spectroscopy analysis confirmed the presence of the Cu nanopartilces and also the other elements such as O, C, P, Ca, Cl, Na, K, Mg, and S originated from the bioflocculant. FT-IR results showed the presence of the –OH and –NH2 groups, aliphatic bonds, amide and Cu–O bonds. Powder X-ray diffraction peaks confirmed the presence of (111) and (220) planes of fcc structure at 2 of 33° and 47° respectively with no other impurity peaks.

scholarly journals Synthesis of a novel magnetic polyacrylamide coagulant and its application in wastewater purification

2016 ◽  
Vol 75 (3) ◽  
pp. 581-586 ◽  
Author(s):  
Zheng Zhou ◽  
Aiqin Shan ◽  
Yuxia Zhao
Keyword(s):  
Suspended Solids ◽  
Removal Rate ◽  
Thermo Gravimetric Analysis ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Wastewater Purification ◽  
Thermo Gravimetric ◽  
Turbidity Removal ◽  
X Ray ◽  
Magnetite Fe3o4

In this study, a novel magnetic polyacrylamide (PAM) coagulant based on the core of magnetite (Fe3O4), with oleic acid serving as modifier and acrylamide as monomer, was synthesized to remove suspended solids in kaolin-suspended water. The composites were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, thermo gravimetric analysis and scanning electron microscopy. The results demonstrated that 82.8% of turbidity removal rate was obtained in 5 min of static settling in simulated kaolin-suspended water. This proved to be superior to that of PAM and poly aluminum chloride. Also confirmed in this study was the fact that zeta potential was significantly correlated with turbidity removal.

1,3,5-Tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane

2016 ◽  
Vol 71 (1) ◽  
pp. 81-84 ◽  
Author(s):  
Eugen Weisheim ◽  
Hans-Georg Stammler ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

AbstractThe reaction of 1,3,5-triethynyl-1,3,5-trimethyl- 1,3,5-trisilacyclohexane with (dimethylamino)trimethylstannane afforded 1,3,5-tris[(trimethylstannyl)ethynyl]- 1,3,5-trimethyl-1,3,5-trisilacyclohexane with tin-functionalised ethynyl groups. The compound was characterized by single-crystal X-ray diffraction, elemental analysis, mass spectrometry, NMR and FT-IR spectroscopy.

scholarly journals In vitro Complexation of Olmesartan Medoxomil with Dapagliflozin, Vildagliptin and Metformin

2019 ◽  
Vol 18 (2) ◽  
pp. 271-280 ◽  
Author(s):  
Fahima Aktar ◽  
Md Zakir Sultan ◽  
Mohammad A Rashid
Keyword(s):  
Drug Interactions ◽  
Thermo Gravimetric Analysis ◽  
Olmesartan Medoxomil ◽  
Therapeutic Agents ◽  
Gravimetric Analysis ◽  
Thermochemical Properties ◽  
Scanning Calorimetry ◽  
Thermo Gravimetric ◽  
Ft Ir

Drug-drug interactions have been a serious concern for pharmacokinetics, pharmacodynamics and pharmacological profiles of therapeutic agents. The aim of this study was to carry out interactions of olmesartan medoxomil with dapagliflozin, vildagliptin and metformin, which were confirmed by TLC, HPLC and FT-IR. The newly formed complexes showed characteristic thermochemical properties in differential scanning calorimetry (DSC) and thermo gravimetric analysis (TGA). In TLC, three spots from the three complexes were found to be different from their precursor drugs. In HPLC chromatograms, the Rt (retention time) of the pure olmesartan medoxomil, dapagliflozin, vildagliptin and metformin were found to be different from their respective complexes. The FT-IR spectra obtained for drug-drug interactions were seen to demonstrate new pattern of peaks compared to pure drugs. The DSC and TGA thermograms of olmesartan medoxomil, dapagliflozin, vildagliptin and metformin were also found to be different from their complexes. All these variations from parent compounds indicated the formation of new complexes. Dhaka Univ. J. Pharm. Sci. 18(2): 271-180, 2019 (December)

Darstellung von 1,3,5-Trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinanen; Einkristall-Röntgenstrukturanalyse eines Platin(II)-Komplexes/Preparation of 1,3,5-Trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinanes; Single Crystal X-Ray Diffraction Study of a Platinum(II)-Complex

1992 ◽  
Vol 47 (4) ◽  
pp. 517-525 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crown Ether ◽  
Single Crystal ◽  
Diffraction Study ◽  
Planar Geometry ◽  
Boat Conformation ◽  
Staudinger Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Synthesis ◽  
Square Planar

A new synthesis for 2-chloro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (1) is described. Chlorine-fluorine exchange in 1 by means of sodium fluoride in acetonitrile in the presence of catalytic amounts of a crown ether furnished 2-fluoro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (2). The synthesis of the bromine and iodine analogues, 3 and 4, by metathesis of 1 with the appropriate trimethylsilyl halides, Me3SiBr and Me3SiI, respectively, is also described. The syntheses of an iron(0)tetracarbonyl complex (5) and of a dichloroplatinum( II) complex (6) are reported. A single crystal X-ray diffraction study was conducted on 6. [P21/c, a = 1161.3(3), b = 1423.2(3), c = 1247.7(3) pm, β = 109.42(2)°, R = 0.028], There are deviations from ideal square planar geometry at platinum. The heterocycles display a flattened boat conformation. A Staudinger reaction of 1 with Me3SiN3 led to the formation of a substituted cyclotriphosphazene.

The mixed-valent 10-manganese(III/IV)-containing 36-tungsto-4-arsenate(V), [MnIII 6MnIV 4O4(OH)12(H2O)12(A-β-AsW9O34)4]22−

2018 ◽  
Vol 74 (11) ◽  
pp. 1390-1394 ◽  
Author(s):  
Rami Al-Oweini ◽  
Bassem S. Bassil ◽  
Marwa Itani ◽  
Dilara Börte Emiroğlu ◽  
Ulrich Kortz
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Sodium Salt ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Potassium Sodium ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

Interaction of the mixed-valent 12-manganese coordination complex [MnIII 8MnIV 4O12(CH3COO)16(H2O)4] with the lacunary 9-tungstoarsenate(V) [A-α-AsW9O34]9− resulted in the 10-manganese(III/IV)-containing 36-tungsto-4-arsenate(V), [MnIII 6MnIV 4O4(OH)12(H2O)12(A-β-AsW9O34)4]22− (1). Polyanion 1 was isolated as a hydrated mixed potassium–sodium salt, K14Na8[MnIII 6MnIV 4O4(OH)12(H2O)12(A-β-AsW9O34)4]·104H2O, which crystallizes in the orthorhombic space group Pbcn and was characterized by FT–IR spectroscopy and single-crystal X-ray diffraction, as well as elemental and thermogravimetric analyses. The title polyanion contains a unique [MnIII 6MnIV 4O4(OH)12(H2O)12]14+ core stabilized within the 36-tungsto-4-arsenate(V) framework.

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