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استخدام تقنية كروماتوغرافيا الغاز باستعمال اطوار سائلة ثابتة لدراسة كفاءة فصل بعض مركبات الازو المشتقة من الباراكريزول == Use Gas - Chromatography Technique By Using Stationary Liquid Phases For Study of Separation Efficiency For Some Azo Compounds Derivative From P - Cresol
Author name:
وداد ابراهيم يحيى خزاعل
Supervisor name:
قاسم كاظم الاسدي
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
University of Kufa - College Of Education For Girls - Chemistry Department
Language:
Arabic
University location:
Najaf
First pages:
25T1452 - p.pdf
Abstract:
حضر كاشفين عضويين جديدين هما2 - [3 - Acyl methyl phenyl )azo] - 4,5 - diphenyl imidazol (3 - AMePADPI) 1 - [(2 - Pyridyl azo)] - 2 - naphthol (PAN) وقد استخدما في فصل واستخلاص والتقدير الطيفي لعناصر النحاس(II)، النيكل(II)والبلاديوم(II) على هيئة ايونات موج | Synthesized two organic reagent was 2 - [(3 - Acyl methyl phenyl)azo] - 4,5 diphenyl imidazole (3 - AMePADPI) and 1 - [(2 - pyridyl azo)] - 2 - naphthol (PAN), which is used for separation , extraction and spectrophotometric determination Copper(II) ,Nickel(II) and Palladium(II) as Cations according to solvent extraction method ,dependence on measurement absorbance of ion pair complex extracted at ?max as well Calculation distribution ratio (D). This Study include limitation of optimum conditions for Complex formation and extraction such as pHex. and the experimental shows optimum pH for extraction Copper(II) with (3 - AMePADP) (pHex=8) and (pHex=9) with (PAN) but for Nickel was(pHex=11) with both organic reagent as well (pHex=9) for palladium (II) with both organic reagents. The study about metal ions concentration effect on extraction methods demonstrate 40µg Cu2+ suitable concentration giving higher absorbance for ion pair complex extracted to organic phase and higher distribution ratio (D) with both organic reagent , also for Nickel(II) was 80µg Ni2+ with (3 - AMePADP) and 50µg Ni2+ with (PAN) , but for palladium(II) was 20µg Pd2+ with(3 - AMePADPI) and 15µg Pd2+ with (PAN). Kinetic energy has important role in extraction. method according to Solvent extraction , and this study show effect shaking time of two immiscible phase on qualification `of extracted and illustrate 15 min was suitable shaking time for Copper(II) and Nickel(II) with both organic reagent and 5 min for palladium(II) with both organic reagent to obtaining higher absorbance of ion pair complex extracted to organic phase and distribution ratio (D). Organic solvent effect study appear there is not any linear relation between dielectric constant (?) of organic solvents and distribution ratio (D) that’s is mean there is not any effect for polity of organic solvent on extraction method but there is an effect for organic solvent structure which is participate in the structure of ion pair complex extracted by formation ,Tight ion pair or loose ion pair as well experiment result illustrate dichloro methane organic solvent (DCM) was the best organic solvent in extraction Copper(II) ,Nickel(II) and Palladium(II) by organic reagent (3 - AMePADPI) and PAN. Study about determination more probable structure of ion pair complex extracted (stoichiometry ) by performance four spectrophotometric method for extraction Cu2+ , Ni2+ and Pd2+ by (3 - AMePADPI) and PAN under optimum conditions and all experiment show the structure of ion pair complex extracted was (1 : 1) (metal : ligad) [Cu(3 - AMePADPI)]2+SO42 - . , [Cu(PAN)]+HSO4 - .[Ni(PAN)]+Cl - . [Ni(3 - AMePADPI)]2+2Cl - . [Pd(3 - AMePADPI)]2+2Cl - . , [Pd(PAN)]+Cl - . Declination of distribution ratio (D) frequently by reason of the organic reagent not gratify the coordination shell of metal ion and in this case water molecule participate to saturate the coordination shell and increase partition the complex to aqueous phase and increase dissociation of complex and decrease distribution ratio(D) as well probable to formation ion pair complex in structure of [M(L)]n+(OH) where M=Cu2+ , Ni2+ and Pd2+ and L = (3 - AMePADPI) or PAN this complex favorite partition to aqueous phase and decrease distribution ratio. Thermodynamic study include Temperature effect on extraction efficiency the experimental results demonstrate the reaction was exothermic for Copper(II) with both organic reagent (3 - AMePADPI) and PAN but the Complextion reaction of Nickel(II) and Palladium(II) with organic reagent (3 - AMePADPI) and PAN endothermic reaction , after calculation thermodynamic data ?Hex , ?Gex , ?Sex show entropy values was high that is mean complexation reaction is entropic in region. The study about Interferences effect on extraction method of Cu2+ , Ni2+ and Pd2+ by (3 - AMePADPI) and PAN to clarify metal cations of first group in periodic table Li+ , Na+ and K+ giving enhancement in distribution ratio in arranging Li+ >Na+>K+ by reason of high affinity of these ions to water and the thickness hydration shell increase with diameter decrease , this properties these ions being to contribute to destroy hydration shell of Cu2+ , Ni2+ and Pd2+ and increase chances of association with organic reagent and increase distribution ratio (D) , but metal cations of second group in periodic table Mg2+ , Ca2+ has more charge density than metal cation of first group and has less thickness in hydration shell and the effective behavior on extraction method was less , but anions able to participate in electrostatic combination with cation complex and giving different effects by differ in molar volume , stereo structure and charge density. The study about synergism by used tributyl phosphate (TBP) and Methyl iso butyl Ketone (MBK) in the extraction the experimental results shows TBP and MIBK giving enhancement in distribution ratio (D) by participate molecular of these solvents in the structure of ion pair complex extracted install f water molecular in coordination shell of metal cation as well as the results show there is one molecular of TBP or MIBK participate in ion pair complex extraction [Cu(MIBK)(PAN)]+HSO - 4 , [Cu(MIBK)(3 - AMePADPI)]2+SO42 - [Cu(TBP)(PAN)]+HSO - 4 , [Cu(TBP)(3 - AMePADPI)]2+SO42 - [ Ni (MIBK)(PAN) ]+Cl - , [ Ni (TBP)(3 - AMePADPI)]2+ 2Cl - [ Ni (MIBK)(PAN) ]+Cl - , [ Ni (TBP)(3 - AMePADPI)]2+ 2Cl - [Pd(MIBK)(PAN)]+Cl - , [ Pd(MIBK)(3 - AMePADPI)]2+2Cl - [Pd(TBP)(PAN)]+Cl - , [ Pd(TBP)(3 - AMePADPI)]2+2Cl - The study about of effect of ethanol in aqueous solution on extraction method of metal in aqueous solution on extraction method of metal cation Cu2+ , Ni2+ and Pd2+ by (3AMePADPI) and PAN the results show foundation of ethanol in aqueous solution with metal cations giving increase in distribution ratio and this increasing continue until reached optimum concentration of ethanol after this value distribution ratio (D) decrease. This study include used organic reagent (3AMePADPI) and PAN for spectrophotometric determination of Copper(II) ,Nickel(II) and Palladium(II) in different environmental and vital samples.
