A sensitive and selective method have been developed for the determination of palladium (II)and platinum (II) . A new reagent and two complexes have been prepared in ethanolic solutions .The method is based on the chelation of metal ions with 4-(4?- pyrazolon azo) resorcinol (APAR) to form intense color soluble products, that are stable and have a maximum absorption at 595 nm and at 463 nm and ?max of 1.11×10 4 and.1.35 ×104 Lmole-1cm-1 for Pd(II) Pt(II) respectively. A linear correlation of (1.4 – 0.2) and (3.2 -0.4 ) ppm for pd(II) pt(II) respectively .The stability constants , relative errors , a relative standard deviations for Pd(II) and Pt(II) were 0.40×105 , 0.4×104 L mol-1 ,0.34 - 0.21% and 2.4 – 0.91% respectively. The conductivity measurements for complexes are consistent with those expected for an electrolyte. The proposed method was successfully applied to the analysis of dust and synthetic mixtures without any preliminary concentration or sparation.
Simple and sensitive batch and Flow-injection spectrophotometric methods for the determination of Procaine HCl in pure form and in injections were proposed. These methods were based on a diazotization reaction of procaine HCl with sodium nitrite and hydrochloric acid to form diazonium salt, which is coupled with chromatropic acid in alkaline medium to form an intense pink water-soluble dye that is stable and has a maximum absorption at 508 nm. A graphs of absorbance versus concentration show that Beer’s law is obeyed over the concentration range of 1-40 and 5-400 µg.ml-1 of Procaine HCl, with detection limits of 0.874 and 3.75 µg.ml-1 of Procaine HCl for batch and FIA methods respectively. The FIA average sample throughput was 70 h-1. A
... Show MoreThis work is based on the synthesis of Cobalt(II) and Cadmium(II) mixed-ligands compounds obtained from the reaction of N'-(4-methylsulfanyl-benzoyl)-hydrazine carbodithioic acid methyl ester as a ligand and using ethylendiamine (en), 2,2'-bipyridine (bipy) or 1,10-phenanthroline (phen) as a co-ligand. The synthesis of ligand (HL) was based on multi-steps synthetic procedure. The reaction of 4-methylsulfanyl-benzoyl chloride with hydrazine gave 4-methylsulfanyl-benzoic acid hydrazide. This compound was reacted with carbon disulfide and potassium hydroxide in methanol to yield N'-(4-methylsulfanylbenzoyl)-hydrazine potassium thiocarbamate, which upon reaction with methyl iodide resulted in the formation of the ligand. A range of physico-chem
... Show MoreThis work is based on the synthesis of Cobalt(II) and Cadmium(II) mixed-ligands compounds obtained from the reaction of N'-(4-methylsulfanyl-benzoyl)-hydrazine carbodithioic acid methyl ester as a ligand and using ethylendiamine (en), 2,2'-bipyridine (bipy) or 1,10-phenanthroline (phen) as a co-ligand. The synthesis of ligand (HL) was based on multi-steps synthetic procedure. The reaction of 4-methylsulfanyl-benzoyl chloride with hydrazine gave 4-methylsulfanyl-benzoic acid hydrazide. This compound was reacted with carbon disulfide and potassium hydroxide in methanol to yield N'-(4-methylsulfanylbenzoyl)-hydrazine potassium thiocarbamate, which upon reaction with methyl iodide resulted in the formation of the ligand. A range of physico-c
... Show MoreA newly developed analytical method characterized by its speed and sensitivity for the determination of metformin-HCl via the formation of complex for metformin-HCl-OH--copper(II) ion from the gel bead system by continuous flow injection analysis. The method is based on the imbedded copper(II) ion in the gel bead structure can be used in the reaction for the formation of red –magneta colour complex(λmax. =530nm) formed by direct reaction of the drug with the released copper (II) ion from the gel bead in alkaline medium. Linear dynamic range for the absorbance versus metformin concentration was 0.001-1 mmol.L-1 while C.O.D was (r2% =95.33%) . The L.O.Q was 0.868mmol.L-1.L.O.D (S/N=3)=0.5μmol.L-1 from the step wise dilution for the min
... Show MoreIn this study, a new, rapid and sensitive batch and flow injection-merging zones spectrophotometric methods for the determination of hydroquinone in a pure material and in pharmaceutical preparation were proposed. These methods were based on the oxidative-coupling reaction of HQ with 2,4-dinitrophenylhydazine (DNPH) in the presence of sodium periodate and sodium hydroxide to form a dark brown water slouble dye that is stable and has maximum absorption at 530 nm, graphs of absorbance versus concentration show that Beer's low is obeyed over the concentration rang of 1-40 and 3-300 μg.ml-1 of hydroquinone, with detection limits of 0.162 and 0.510 μg.ml-1 of hydroquinone for batch and FIA methods, respectively. The optimized FIA system is
... Show MoreNew metal complexes of the ligands 2-benzamido benzothiazole(B1), and 2-actamido benzothiazole(B2) with metal ions Ni(II),and Co(II) were prepared in alcoholic medium. The prepared complexes were characterized by FT-IR and electronic spectroscopy, Magnetic susceptibility, Flame Atomic Absorption technique as well as elemental analysis and conductivity measurement. From the spectral studies, an octahedral monomer structure proposed for Ni(II) complexes, and a tetrahedral monomer structure for Co(II)complexes.Semi-empirical methods (PM3,and ZINDO/1)were carried out to evaluate the heat formation( ?H?f)binding energy(?Eb) and dipole moment(µ)for all metal complexes. Also vibration frequencies, Electrostatic potential, HOMO and LUMO
... Show MoreA simple, precise and accurate spectrophotometric method has been developed for simultaneous estimation of sulfanilamide and furosemide in their mixture by using first and second order derivative method in the ultraviolet region. The method depends on first and second derivative spectrophotometry, with zero-crossing and peak to base line and peak area measurements. The first derivative amplitudes at 214, 238 and 266 nm were selected for the assay of sulfanilamide and 240, 260, 284, 314 and 352 nm for furosemide. Peak area at 201222, 222-251 and 251-281 nm selected for estimation of sulfanilamide and at 229-249, 249270, 270-294, 294-333 and 333-382 nm for furosemide. The second derivative amplitudes at 220, 252 and 274 nm for sulfanilamid
... Show MoreDirect FIA methods for estimation of Naringenin (NG) in different samples were proposed. These methods are based on diazotization coupling reactions of two reagents: method (A) p-chloroaniline (PCA) and method (B) procaine hydrochloride (PRH) with NG in basic medium. Yellow dyes with maximum absorption at 416 and 415 nm were formed respectively. Calibration curves were constructed over different NG concentrations, linearity was from 1- 70 and 1- 40 µgmL-1 with detection limits of 0.55 and 0.24 µgmL-1 for (A) and (B) respectively. All analytical variables involved in the FIA procedure were evaluated and optimized. The established methods were successfully applied for the determination of NG in its supplements and u
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