سحر عقيل حسين الاعسم

Extraction experiments for Zn+2 ion from aqueous phase by new laboratory prepared Azo derivation as complexation agent 2- [(4- Benzyloxy phenyl)azo]- 5- nitro-4-phenyl imidazole (BANI) shows the optimum conditions for this extraction method was (pH= 9) (10 minutes) shaking time and 100μg (1.5x10-4M) concentration of Zn+2 ion in aqueous phase. Organic solvents effect study shows there is not any linear relation between distribution ratio (D) for extraction of Zn+2 ion and dielectric constant (ε)for organic solvents used but there is un effect for organic solvent structure on the extraction of Zn+2 ion and distribution ratio (D) values. Stoichiometric studies demonstrated the more probable structure ion pair complex extracted for Zn+2 was 1:1.

A new Schiff base derivative ligand (LI) have been produced by condensed isatin and 2,3-diaminobutane (2:1) molar ratio. The (LI) ligand has been separated and distinguished by 1H,13C-NMR, (CHN) elemental analysis, UV-visible, mass spectroscopy and Fourier Transform infrared (FTIR) methods. The metal ions, cobalt(II), nickel(II) and copper(II) complexes were synthesized with the ligand. The complexes were typified by, UV-Visible, FTIR, atomic absorption, molar conductance, magnetic susceptibility and elemental analysis (CHN) techniques. Octahedral geometry are suggested for the metal complexes based on the results of physico-chemical and spectral techniques. The TLC for (LI) ligand and complexes demonstrated single spot for each, signifying their compounds purity. All these compounds were determined aligned with two classes of human pathogenic; bacteria Gram positive and Gram negative.

Three organic reagents were synthesized 2-[4-bromo-3,5-diethyl phenyl azo]-4,5diphenylimidazole(BDPI) , 2-[(4-Benzyloxy phenyl)azo]-5-nitro-4- phenyl imidazol (BANI) , 4-[N-(5-methylisoxazol-3-yl)benzene sulfonamide azo] -1- Naphthol (AMBN) ,which are utilized for separation , extraction and spectrophotometric determination Zinc(II) ,Lanthanum(III) and Cerium(III) as cations according to liquid-liquid extraction method , depending on the measurement of absorption of ion pair complex extracted at maximum wavelength (max )and calculation distribution ratio (D). This study involves limitation of optimum conditions for complex formation as well extraction as pH. as well the experiment showes optimum pH for extraction Zn(II) with [(BDPI), (BANI),(AMBN)] (pH=8,9,9) respectively but for La(III) was (pH=11,10,10) with [(BANI) ,(BDPI), (AMBN)] respectively as well (pH=9,9,8) for Ce(III) with [(AMBN) (BDPI) (BANI)] . The study about metal ions concentration effect on extraction methods illustrates 50μg/5mL Zn2+ appropriate concentration obtaining higher absorbance for ion pair complex extracted to organic solution as well higher distribution ratio (D) with all organic reagents , and for La3+ was 80μg/5mL with all organic reagents also 100μg/5mL Ce3+ all organic reagents. Kinetic energy has significant role in extraction. method according to liquid - liquid extraction , as well the study show effect of shaking time of two layers on qualify of extracted and explains 10 min which were appropriate shaking time for Zn(II), La(III) and Ce(III) with all organic reagents to give higher distribution ratio (D) as well higher absorbance of ion pair complex extracted to organic phase.

Extraction experiments for Ce+3 ion from aqueous phase by new laboratory prepared Azo derivation as complexation agent 4- [N-(5-methyl isoxazol-3-yl)benezen sulfonamide azo]-1- Naphthol (AMBN) shows the optimum conditions for this extraction method was (pH= 9) (10 minutes) shaking time and 100μg (1.5x10-4M) concentration of Ce+3 ion in aqueous phase. Organic solvents effect study shows there is not any linear relation between distribution ratio (D) for extraction of Ce+3 ion and dielectric constant (ε)for organic solvents used but there is un effect for organic solvent structure on the extraction of Ce+3 ion and distribution ratio (D) values. Stoichiometric studies demonstrated the more probable structure ion pair complex extracted for Ce+3 was 1:1 .

Abstract: Extraction experiments for Zn(II) ions from aqueous phase by new laboratory prepared Azo derivation as complex agent 2- [4-bromo-2,6-diethyl phenylazo] -4,5-diphenylimidazole(BDPI)shows the optimum conditions for this extraction method was (pH= 8) (10 minutes) shaking time and 50μg concentration of Zn(II)ions in aqueous phase. Organic solvents effect study shows there is not any linear relation between distribution ratio (D) for extraction of Zn+2 ions and dielectric constant (ε)for organic solvents used but there is in effect for organic solvent structure on the extraction of Zn+2 ions and distribution ratio (D) values. Stoichiometric studies demonstrated the more probable structure ion pair complex extracted for Zn+2 was 1:1.

The new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu 2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pH ex =9), optimum concentration was 40μg/5mLCu 2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu 2+ : BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and distribution ration (D). Thermodynamically found the reaction was Endothermic reaction, with ΔH ex = 0.0131 KJ.mole-1 ,ΔG ex =-54.20 KJ.mole-1 ,ΔS ex = 167.84 J.mole-1 .Beer's law was obeyed over the concentration 1-30μg/5mL, and ε=922.90 Lmol-1 .cm-1 ,with detection limit 1.7×10-5 and Sandell's sensitivity 6.8× 10-7 gcm-2 .

Abstract: This study includes the preparation of chelate complexes of Pt(II),Pd(II)andPb(II) by reacting these ions with the ligand 2-(Benzothiozolyl azo-4- benzyl phenol ,The preparation of the complexes was conducted after fixing the optimum conditions such as pH and concentration .UV- visible spectra of these complex solutions were studied for a range of pH and concentration which obey Lampert-Beers Law .The structures of complexes are deduced according to mole ratio method which were obtained from the spectroscopic studies of the complex solutions .The ratios of metal: ligand obtained were (1:2) for all complexes. Identification of the ligand by using UV-Vis. Spectral, IR-Spectral, H1-NMR, elemental analysis. The conductivity measurements. Results show that the ligand was tridentated. Also the proposed geometrical structures of the complexes of Pt (II), Pd (II), Pb (II) ions are octahedral.

The New ligand of 5-((2,4-dichlorophenyl)azo)-2,2-dimethyl-1,3-dioxane-4,6-dione (DPOD) have been prepared . Three chelate complexes Have also been prepared by reacting this ligand with the metal ions Co (II),Ni(II) and Cd(II). The preparation has been conducted after fixing the optimum conditions of concentration U.V- visible spectra of these complexes solutions have been studied for a range of pH and concentrations which obey Lampert-Beers Law .The structures of complexes are deduced according to mole ratio method which were obtained from the spectroscopic studies of the complex solutions .The ratios of metal: ligand obtained are (1:2) for all complexes ions .(UV-Vis) absorption spectra of ethanolic solution of complexes showed bathchromic shift , as compared with that of free ligand .The infrared spectra of the chelating complexes have been studied ,this may indicate that coordination between the metal ions and the prepered ligand takes place .The conductivity measurements ,the percentage of metal ions of the complexes were determined ,depending on these results , in addition to, the proposed geometrical structures of the complexes of Co (II), Ni(II), Cd(II) ions are octahedral .

xtraction experiments forions from aqueous phase by new laboratory prepared Azo derivation as complex agent shows the optimum conditions for this extraction method (10 minutes) shaking time . Organic solvents effect study shows there is not any linear relation between distribution ratio (D) ions and dielectric constant (ε)for organic solvents used but there is in effect for organic solvent structure on the extraction and distribution ratio (D) values. Stoichiometric studies demonstrated the more probable structure ion pair complex extracted for was 1:1.

Extraction procedures for Ag+ from aqueous solutions by 2-[(4-Chloro-2-Methoxy phenyl) azo]-4,5-diphenyl imidazole (4-ClMePADPI) shows aqueous solutions must be at (pH=10) and concentration of Ag+ ions is (40μg)(7.36×10-5 M), with shaking time (11minutes), organic solvents effect on extraction method demonstrate there is not any linear relation between dielectric constant (ε) for organic solvents used and distribution ratio values (D), but there is effect for structure of organic solvent. Stoichiometry studies shows more probable structure of ion pair complex extracted was (1:1) (Metal:Ligand) [Ag(4-ClMePADPI)]+NO3-, temperature effect shows from thermodynamic viewpoint the reaction between Ag+ ions and ligand (4-ClMePADPI) was endothermic reaction, synergism studies appear there is one molecules of TBP participate in ion pair complex extracted [Ag(4-ClMePADPI)(TBP)]+NO3-.

In this work we have prepared three complexes by reacting the ligand of azo imidazole 2[(4-Benzyloxy phenyl)azo]-4,5- diphenyl imidazole (P-BOPAI) with the following metal ions Cr(III) ,Mn(II), and Ag(I) . The preparation has been conducted after fixing the optimum conditions of concentration and (PH). U.V- visible spectra of the complex solutions of the above metal ions with the ligand (P-BOP AI) have been studied for a range of (PH) and concentration which obey lampert-Beers rule. The structures of complexes are deduced according to mole ratio method which were obtained from the spectroscopic studies of the complex solutions .The ratios of metal: ligand obtained are (1 :2) to the complexes of Cr(III), Mn(II), ions and (1: 1) to the complexe of Ag(II) ion . The stability of complexes in solution were also studied at the optimum conditions. All our complexes mentioned above have been identified as follows: (UV -Vis) absorption spectra of ethanolic solution of complexes showed bath chromic shift, as compared with that of free ligand. The infrared spectra of the chelating complexes have been studied ,they were also compared with the ligand spectrum, they showed obvious changes in the band positions .Some of them has been disappear while others are shifted,this may indicate that acoordination between the metal ions and our ligand takes place. The conductivity measurements of our complexes have shown that non- ionic characters appear in ethanol solution to Mn(II),Ag(I)ions and ionic characters to Cr(III)ion .Elemental analysis for all complexes were determined , good agreement was obtained between the found and calculated values. Depending on these results , in addition to the measurements of magnetic susceptibility of our complexes it seems that some of these complexes are paramagnetic, while others are diamagnetic . We can conclude that the proposed geometrical structures of the complexes of Cr(III), Mn(II), ions are octahedral , while the complexe of Ag(I) ion is tetrahedral geometry .

The New ligand of azo naphthol 1-[(4-Antipyril)azo]-2- naphthol (4-AAP-2-N) have been prepared . Three chelate complexes Have also been prepared by reacting this ligand with the metal ions Co (II),Ni(II) and Cu(II). The preparation has been conducted after fixing the optimum conditions of concentration.U.V- visible spectra of these complexes solutions have been studied for a range of pH and concentrations which obey Lampert-Beers Law .The structures of complexes are deduced according to mole ratio method which were obtained from the spectroscopic studies of the complex solutions .The ratios of metal: ligand obtained are (1:2) for all complexes ions .(UV-Vis) absorption spectra of ethanolic solution of complexes showed bathchromic shift , as compared with that of free ligand .The infrared spectra of the chelating complexes have been studied ,this may indicate that coordination between the metal ions and the prepered ligand takes place .The conductivity measurements , Elemental analysis ,the percentage of metal ions and the measurements of magnetic susceptibility of the complexes were determined ,depending on these results , in addition to, the proposed geometrical structures of the complexes of Co (II), Ni(II), Cu(II) ions are octahedral . finally the study of the biological activity of some of these prepared compounds towards two kinds of disease bacteria, which is a positive bacteria for Gram pigment: 1- Staphylococcus aureus Second classification for negative bacteria including: 2- pseudomonas aeruginosa The results showed that some of the prepared compounds had inhibition activity toword some types of bacteria.