A simple, rapid and sensitive spectrophotometric method has been proposed for the determination of La (III) using 3-hydroxy -4-(2-hydroxy-phenyl azo) naphthalene -1- sulfonic acid as a chromogenic reagent. This method is based on the formation of a red-pink colored complex, upon the reaction of La(III) with the reagent in an alkaline medium (pH= 9.50), having a maximum absorbance at 459 nm. Beer's law is valid in the concentration range 0.512 µg.ml-1 with a Sandell's sensitivity value of 0.0188 µg.cm-2 and molar absorptivity of 7376.12 L.mol-1.cm-1. The stoichiometric composition of the chelate is 1:3. The effect of the presence of different cations as interferants in the determination of La(III) under the given optimum conditions were investigated.
The present study combines UV-Vis spectrophotometry and dispersive liquid-liquid microextraction (DLLME) for the preconcentration and determination of trace level clidinium bromide (Clid) in pharmaceutical preparation and real samples. The method is based on ion-pair formation between Clid and bromocresol green in aqueous solution using citrate buffer (pH = 3). The colored product was first extracted using a mixture of 800 µL acetonitrile and 300 µL chloroform solvents. Then, a spectrophotometric measurement of sediment phase was performed at λ = 420 nm. The important parameters affecting the efficiency of DLLME were optimized. Under the optimum conditions, the calibration graphs of standard -1 (Std.), drug, urine and serum were ranged
... Show MoreSimple and sensitive kinetic methods are developed for the determination of Paracetamol in pure form and in pharmaceutical preparations. The methods are based on direct reaction (oxidative-coupling reaction) of Paracetamol with o-cresol in the presence of sodium periodate in alkaline medium, to form an intense blue-water-soluble dye that is stable at room temperature, and was followed spectrophotometriclly at λmax= 612 nm. The reaction was studied kinetically by Initial rate and fixed time (at 25 minutes) methods, and the optimization of conditions were fixed. The calibration graphs for drug determination were linear in the concentration ranges (1-7 μg.ml-1) for the initial rate and (1-10 μg.ml-1) for the fixed time methods at 25 min.
... Show MoreThe aim of the work is synthesis and characterization of bidentate ligand [dipotassium sodium7-((E)-2-(2-((Z)-1-carboxylatoethylideneamino)thiazol-4-yl)-2 (carboxylatemethoxyimino) acet amido)-8-oxo-3-vinyl-5- thia-1-azabicyclo[4.2.0] oct-2- ene-2- carboxylate] [Nak2L], from the reaction of cefixime with sodium pyruvet to produce the ligand [Nak2L], the reaction was carried out in methanol as a solvent under reflux. The prepared ligand [Nak2L] which was characterized by FT-IR, UV-Vis spectroscopy, 1H, 13C-NMR spectra, Mass spectra, (C.H.N) and melting point. The mixed ligand complexes were prepared from ligand [Nak2L] was used as a primary ligand while 8-hydroxy quinoline [Q] was used as a secondary ligand with metal ion M(?).Where M(?) =
... Show MoreThe aim of the work is synthesis and characterization of bidentate ligand [dipotassium sodium7-((E)-2-(2-((Z)-1-carboxylatoethylideneamino)thiazol-4-yl)-2 (carboxylatemethoxyimino) acet amido)-8-oxo-3-vinyl-5- thia-1-azabicyclo[4.2.0] oct-2- ene-2- carboxylate] [Nak2L], from the reaction of cefixime with sodium pyruvet to produce the ligand [Nak2L], the reaction was carried out in methanol as a solvent under reflux. The prepared ligand [Nak2L] which was characterized by FT-IR, UV-Vis spectroscopy, 1H, 13C-NMR spectra, Mass spectra, (C.H.N) and melting point. The mixed ligand complexes were prepared from ligand [Nak2L] was used as a primary ligand while 8-hydroxy quinoline [Q] was used as a secondary ligand with metal ion M(Π).Where
... Show MoreNew series of metal ions complexes have been prepared from the new ligand [2,2′‐(5,5‐dimethylcyclohexane‐1,3‐diylidene)bis(azan‐1‐yl‐1‐ylidene)dibenzoic acid] derived from 5,5‐dimethylcyclohexane‐1,3‐dione and 2‐aminobenzoic acid. Accordingly, mono‐nuclear Ni(II), Pd(II), Re (II), and Pt(IV) complexes were prepared by the reaction of previous ligand with NiCl2.6H2O, PdCl2, ReCl5, and H2PtCl6.6H2O, respectively. The compounds have been characterized by Fourier‐transform infrared (FTIR), ultraviolet–visible (UV–vis), mass, H
The inhibitive action of Phenyl Thiourea (PTU) on the corrosion of mild steel in strong Hydrochloric acid, HCl, has been investigated by weight loss and potentiostatic polarization. The effect of PTU concentration, HCl concentration, and temperature on corrosion rate of mild steel were verified using 2 levels factorial design and surface response analysis through weight loss approach, while the electrochemical measurements were used to study the behavior of mild steel in 5-7N HCl at temperatures 30, 40 and 50 °C, in absence and presence of PTU. It was verified that all variables and their interaction were statistically significant. The adsorption of (PTU) is found to obey the Langmuir adsorption isotherm. The effect of temperature on th
... Show MoreA new spectrophotometric method for the determination of allopurinol drug was investigated. The proposed method was based on the reaction of the intended drug with catechol and Fe(II) to form a blue soluble complex which was measured at λmax 580 nm. A graph of absorbance versus concentration shown that Beer’s law was obeyed over the concentration range of 2–10 μg ml–1 with molar absorptivity of 9.4 x 103 l mol–1 cm–1 and Sandell sensitivity of 1.4 x 10–2 μg cm–2. A recovery percentage of 100% with RSD of 1.0%–1.3% was obtained. The proposed method was applied successfully for the determination of allopurinol drug in tablets with a good accuracy and
The new azo dye was synthesized via the reaction of the diazonium salt form of 3-aminophenol with 2-hydroxyquinoline. This dye was then used to access a series of complexes with the chlorides of manganese, iron, zinc, cadmium, and vanadium sulfate. The prepared ligand and its complexes were characterized by FT-IR spectroscopy, UV-visible spectroscopy, mass spectrometry, thermogravimetric analysis, differential scanning calorimeter, and microelemental analysis. Conductivity, magnetic susceptibility, metal content, and chlorine content of the complexes were also measured. The ligand and cadmium complex were identified using1H NMR and 13C NMR spectroscopy. The results showed that the shape of the ligand is a trigonal planner, and the c
... Show MoreNew Schiff bases derivatives [IV]a-e is prepared via condensation of Derythroascorbic acid with p-substituted aldehydes in dry benzene. To obtain these derivatives, the 5,6-O-isopropylidene-L-ascorbic acid[I] was chosen as starting material, compound prepared from the reaction of L-ascorbic acid as starting material. Compound[I] was prepared from the reaction of L-ascorbic acid with dry acetone in the presence of hydrogen chloride. The esterification of hydroxyl groups at C-2 and C-3 positions with excess ofethyl α –chloroacetate in the presence of sodium acetate produce acorresebonding ester [II] , which was condensed with hydrazine hydrate to give new hydrazide [III] . The new Schiff bases [IV]a-e were synthesized by reaction of acid h
... Show MoreMixed ligands reaction of [2-[(3-hydroxyphenyl)diazinyl]-1,2-benzothiazol-3(2H)-one-1,1-dioxide] (H2L, primary ligand) and bipyridyl (secondary ligand) with salts of Cr(III), Mn(II), Fe(III), Co(II) and Ni(II) was performed. A series of air-stable complexes with distinctive octahedral moieties was created by equal molar ratio (1:1:1). The formation of these compounds was verified using detecting analysis techniques incorporating mass spectra, which validated the achieved geometries. Fourier transform infrared (FTIR) analysis demonstrated how the ligands (H2L and bipyridyl) are chelated as tridentate (ONO) and bidentate (NN) groups, respectively and the coordination with the metal ions. Thermal decomposition studies using pyrolysis (
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